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TurboMatrix Headspace Sampler and HS 40/110 Trap User's Guide

1. 2 Connect Adapter to the GC Injector Figure 18 Installing the Heated Transfer Line at the PerkinElmer GC Injector 70 Installation The threads on the adapter are sharp and can cause cuts to your fingers or hand Use the proper protection a paper towel or gloves before tightening the adapter WARNING 9 Loosen the threaded collar from the stainless steel adapter but do not remove the adapter carefully see warning above use the threads on the adapter to screw the adapter into the injector port and tighten 10 Replace the threaded collar of the transfer line onto the stainless steel adapter and tighten Leak test the system as outlined in the Leak Testing procedure later in this chapter Installing the Heated Transfer Line at the GC for Direct Connection Recommended for the HS 40 110 trap You can install the transfer line so that it bypasses the inlet split of the GC injector By installing the fused silica tubing in this manner the GC carrier gas is now supplied by the HS and the incoming headspace sample is not split or diluted in any way To install the heated transfer line at the GC for direct connection 1 Turn off the GC and allow the injector to cool 2 Inside the GC oven disconnect the GC column from the injector 3 Score and break the fused silica tubing extending out of the end of the HS transfer line Be sure to have plenty of transfer line to work with 20 t
2. Using circlip pliers or round nose pliers remove the circlip from the securing pin on the crimp lever Circlip _ Snap Ring t t n 4m u ae Figure 113 Removing the Circlip and Snap Ring 2 3 4 272 Pull out the pin Remove the lever Using the circlip pliers or round nose pliers remove the snap ring from the top of the crimper Press the four jaws together and pull out the stamper assembly Clamp the flange of the stamper in a vice at the position shown in Figure 114 Place a suitable metal rod or screwdriver through the hole on the plunger Screw the plunger up or down with enough force to break the seal When the crimper is new the stamper is sealed with a thread sealant to prevent inadvertent movement Routine Maintenance Rod a Plunger O Stamper Remove the i Fl Stamper BD 4 i Assembly e Replace the fo Stamper Assembly ao i gt and Adjust the 7 gi Plunger ay UL ess gt ES TE 10 11 12 13 14 15 16 t Jaws Figure 114 Stamper Assembly Carefully place the stamper assembly back into the crimper Press against the stamper from below using your thumb to keep it from rotating Screw the plunger up or down to obtain the required pressure Screwing the plunger up increases the crimping pressure Screwing the plunger down decr
3. Figure 10 Assembling the Fittings Ahead of the GLT Connector 11 12 13 14 Score and break the fused silica tubing to remove any graphite residue which may block the carrier gas flow Push the fused silica tubing into the GLT connector tubing until it reaches the needle Slide the ferrule and nut into position and tighten finger tight Mark the position on the fused silica at the end of the nut Withdraw the fused silica tubing 1 to 1 5 cm back from the needle Tighten the nut Plug the other end of the fused silica tubing by forcing an injector septa on it Leak test the system before you finish assembling the transfer line See the Leak Testing procedure later in this chapter for details on performing a leak test Slide the transfer tubing down so that the PTFE sleeve is within 1 2 mm of the sleeve nut and then tighten the mounting screws on the collar 63 Installation Stainless Steel Sleeve PTFE Sleeve Sleeve Nut P N 04961109 Glass Line Tube Adapter P N B0503956 Swagelok Nut P N 09904956 Retaining Collar Outer Silicone Sleeve Fused Silica Transfer Capillary T a Graphite Ferrule Vent P N 09903700 Vespel Ferrule A Needle P N 04972263 Needle Unit Connection Needle Purge Supply Figure 11 Installation of Transfer Line at the Needle Unit 15 Pull the sliding insulation tube from the transfer line all the way down so that it touc
4. Table 25 Replacement Parts 338 Appendices Set of Injection vials 1000 B0104236 Red PTFE coated Septa 200 B0104239 Silicon Schall Coated Kit B0104241 Silicon Septa Aluminium Coated Kit B0104243 Hand crimper N930785 Vial Pressure gauge B0501377 2 needle Seal Assembly B0500833 Butyl Rubber Septa 100 B0159356 Needle O rings 10 B0198110 Static Headspace Gas Chromatography Theory and N1011210 Practice by B Kolb and L S Ettre Table 26 Contents of Headspace Only Starter Kit Stainless Steel Jet Needle silica steel treated passivated N6700130 Cold trap empty M0413627 Needle seal assembly B0500833 Transfer line tubing ID 0 32mm L 5m N9301357 Transfer line f s tubing ID 0 25mm L 5m N9301356 Needle seal O rings B0198110 Glass sample vials 1000 B0104236 Caps septa star springs silicone PFTE septa kit B0104242 Air monitoring trap glass trap cartridge filled M0413628 Assembly trap desorb tubes N6700112 Alignment rod N6700122 Trap removal tool N6701077 Table 27 Contents of HS 40 110 Trap Spares Kit 339 Appendices Adapter Kits for Gas Chromatographs Description Part Number HS adapter kit for HP 5890 6890 6850 B0505977 HS adapter kit for HP 5890 6890 6850 B0507944 On Column HS adapter kit for VARIAN 3400 3800 packed B0505978 column HS adapter kit for VARIAN 3400 3800 cap
5. STANDBY 10 33 35 Stat Rotate Toos Figure 26 Failed Leak Test Run Status Log Leak Test Result Initial Final Pressure Pressure psi psi Tests GasLeak 34 94 STANDBY 09 55 42 Stet Rotate Tools z Figure 27 Passed Leak Test The HS sampling system is now a closed pressurized system The pressure displayed on the PPC tab must not drop by more than 1 psi over a period of 30 seconds 87 Installation 6 Ifa leak is detected check all of the connections with a helium Leak Hunter or concentrated ethanol and water solution a 50 ethanol and 50 water mix Once you have checked and no leaks are detected then run the leak test again 7 Reduce the carrier pressure to the original pressure 8 Unplug the fused silica tubing and ensure that there is no septum material blocking the fused silica tubing If you are leak testing the HS sampling system and it has failed the leak test you should check the following connections first e O rings in the upper and lower needle sealing elements e Carrier gas connection at the rear panel e Carrier gas connections from the regulator including all filters and unions e Transfer line connection to the needle unit e Column connection at the injector outlet headspace only e Leak check all nuts around the trap e Be sure the trap is not cracked or broken e Check complete flow path and all valve connections If you are testing the w
6. Figure 85 High Pressure Figure 86 High Pressure Sampling Withdrawal Setting the Withdrawal Time For High Pressure Sampling The high pressure augments to the column head pressure until the end of the withdrawal time The withdrawal time should be long enough to ensure that enough of the sample has moved onto the GC column before returning to normal pressure This reduction in pressure causes a temporary reverse in the gas flow at the column head This should only have an effect on the carrier gas not on the sample When working with wide bore capillary columns 0 53 mm i d or with short quartz capillaries 0 32 mm i d a short withdrawal time is recommended e g 0 1 min This avoids unfavorable GC conditions very fast chromatograms caused by the extreme flow rates due to the high pressure P2 If the withdrawal time is too short split peaks and loss of injection volume may result If the withdrawal time is too long the chromatographic separation may be unacceptable due to the extreme flow rate through the column 211 Method Development Water Trap In cryofocusing water is removed from the sample prior to enrichment using the water adsorption trap Water from the sample is removed by adsorption onto a hygroscopic salt The water adsorption trap is necessary to prevent the GC column from becoming blocked by the formation of ice Operating Modes Headspace Only Constant Mode Constant mode is the stan
7. To run this calibration the following conditions should be strictly met e A non leaking vial sealing and septum e The calibration sample should be identical to the ones to be analyzed e The correct sample volume must be used the same as the volume which will be used for samples to be run e Check that the calibration curve profile is good See the next figure for an example of a good decay profile Here a safe Decay Time would be set at 1 6 min 124 Operation Calibrate Decay Time Pressure psi 0 0 0 O04 086 12 16 2 Time min Calibration Vial 1 Time 2 0 Decay Time 1 0 min STANDBY Oct 24 Figure 43 Calibrate Decay Time For a given Vial Pressure the decay slope and time will depend mainly on the sample volume e Smaller sample volume larger headspace volume small slope gradient slow pressure decay e Larger sample volume smaller headspace volume large slope gradient fast pressure decay Next you should choose Monitor Vial Integrity in the SETUP tab of the Preferences screen Tools button gt Preferences screen gt Setup tab With this option enabled the system will monitor and check each vial run in the method and report in the Log tab any deviation from the calibration curve profile i e e Slow pressure decay e Fast pressure decay see the following figure 125 Operation If Stop Vial On Error is also enabled in the Setup tab the system will
8. Using this technique samples containing constituents which are unsuitable for injection with a syringe can be analyzed e g soil polymers highly viscous liquids Suitable fields of application are in the analysis of polymers certifying of the volatile components in drinks and foodstuffs blood alcohol levels water and environmental analysis 185 Method Development The HS Sampling Technique The HS employs a unique sampling technique a pneumatic pressure balanced system The headspace sample is introduced onto the column without resorting to a gas syringe thus avoiding fractionation due to pressure changes in the syringe Since the needle is sealed there are no losses of headspace gas during transfer The sample injection is executed in three steps Thermostatting Phase During the thermostatting phase Standby the sampling needle is in the upper position The carrier gas flows through solenoid valve V1 to the column at the same time the needle cylinder is purged by a small cross flow vented through solenoid valve V2 and needle valve V2 The cross flow prevents carry over between injections Pressurization Phase A fter completion of the thermostatting time the sampling needle moves to the lower position piercing the sample vial septum The carrier gas flows into the vial headspace pressurizing it to equal the sampling head pressure P1 ull V V Ke G T R
9. HS 110 43 cm 17 wide x 61 cm 24 high x 61 24 deep HS 40 110 43 cm 17 wide x 61 cm 24 high Trap x 61 24 deep 41 Installation Clarus 400 66 cm 26 wide x 40 cm 16 high 500 x 72 cm 28 5 deep Clarus 600 53 cm 21 wide x 99 cm 26 high x 82 cm 32 deep AutoSystem 66 cm 26 wide x 40 cm 16 high XL x 64 cm 25 deep Weight HS 16 32 kg 70 1b HS 40 33 kg 73 1b HS 110 35 kg 77 1b HS 40 110 35 kg 77 1b Trap AutoSystem 49 kg 108 Ib XL Clarus 400 49 kg 108 lb 500 Clarus 600 64 5 kg 142 1b Table 7 Space Requirements Allow a minimum of 15 cm 6 of clearance at the rear of the HS and 126 cm 4 1 ft of clearance at the top of the HS GC system for ventilation If this is not possible install the HS GC system on a bench that has wheels Allow at least 90 cm 36 on either side of the GC HS to accommodate additional equipment for example the computer The laboratory bench should be sturdy enough to support the full weight of the HS and GC as well as any additional support equipment i e computer data interface and printer Expect the total weight of the HS GC system and accessory equipment to weigh at least 136 kg 300 Ib The HS is typically positioned to the right of the GC to allow connection of the transfer line 42 Installation If the HS must be locate
10. Increase the GC oven temperature to the operating temperature for the GC analysis Check that the pressure required for the operation of the column as recorded above in step 5 has been reached at the injector Adjust the HS carrier gas pressure further until the required column pressure P2 3 psi has been reached Method Development Fused Silica Transfer Line Packed Column wa Injector Flow Controller Ji P Packed Column Figure 94 Sampling with Packed Columns MHE Theory and Calculations Headspace Only One way to do quantitative analysis using headspace is the Multiple Headspace Extraction MHE technique This technique requires multiple extractions from the sample vial The concentration of the volatile compound of interest is determined at each extraction step Following each extraction re equilibration occurs between the two phases liquid solid and gas in the sample vial and although the concentration of the particular compound in both phases will be smaller than it was originally their ratio partition coefficient remains the same In typical headspace analysis it is not practical or possible for extractions from a sample vial to continue until all of the volatile compound is removed Using the MHE technique however it is unnecessary to perform extractions until all the volatile compound is exhausted as the decrease in concentration of the compound in subsequent extr
11. The post cryofocusing time represents the time after the end of the injection during which the analytes which are still in the water trap and other void volumes are transferred to and focused on the headspace before the start of chromatography An adequate post cryofocusing time is required to ensure that the peaks are sharp and do not tail as a result of the above mentioned void volume effects etc 205 Method Development The post cryofocusing time should be longer than the withdrawal time plus vent time up to a maximum of 2 3 minutes Typically you should set the post cryofocusing time to approximately 1 minute Cryofocusing is started prior to sample injection The first 8 of the column are cooled to the cryofocusing set point before the injection is made It is therefore important to make sure that a pre cryofocusing time is selected so that it does not interfere with the chromatography of the previous run This is of particular importance when operating in Constant mode as this involves the simultaneous thermostatting of several samples In such cases the cycle time must be prolonged by an amount equal to the cryofocusing time In Progressive mode a prolonged cycle time is not necessary as only one sample is thermostatted Post cryofocusing enables particularly volatile components to be separated from the broader air peak which is necessary for example when you are using ECD detection Post cryofocusing time can
12. tab Run Status Log Carrier 0 2 psi Needle 65 JG Transfer a 65 C Track ET Oven ver 60 lec Set Point Actual TestL_Env5_2 Ey Ba Temp Timing Option yppe STANDBY 10 09 26 Start Rotate Tools x Figure 35 Temperature Tab Entering a value of zero for any temperature parameter disables the related heater For example if you enter zero for the transfer line temperature The transfer line heater will be turned off and the transfer line will be at ambient temperature To set the temperature 1 Press the Temp radio button to switch to the Temperature screen 109 Operation 2 Press the Set Point option The current temperature set points will be displayed 3 Press the Needle or Transfer entry box A highlighted option indicates that it is active 4 Press the or buttons to increase or decrease the temperature to the desired value 5 The HS will cool or heat the needle or transfer line to the desired temperature Allow some time for the instrument to reach the new value 6 To save your settings as a new method or to update the existing method press the Tools button and select Save As 7 To save the method under the existing name press OK To create a new method enter a new name for the method by pressing the method name An alphabetic keypad is displayed To enter numeric characters press the Num key Press Shift to obtain uppercase character
13. All instruments of the system should be connected to a common phase 44 Installation The line power supply should conform to local safety regulations and must include a correctly wired protective earth ground terminal It should be checked by a qualified electrician before you connect the instrument To avoid interference caused by ground loops always connect the HS and any accessory to the same phase of the line power supply and insure that they share a common earth ground Observe outlet power limits Refer to the individual accessory manuals for details on installing various accessories and their power requirements Electrical Surge The toroidal power transformer and the switched mode power supply unit SMPSU of the HS provide a compact high efficiency unit A feature of these components however is that they can draw high inrush current from the external electricity supply during power up In some circumstances the current can be sufficient to cause external excess current devices particularly magnetically operated circuit breakers to open Although the SMPSU incorporates thermistors to limit the inrush current these are only effective when they are close to room temperature During normal operation these components run at an elevated temperature and as a result of their reduced electrical resistance are unable to prevent the passage of high surge currents associated with brief interruptions of the e
14. NOTE This cable contains a resistor diode and transistor contained within the 9 pin connector shell 1 Connect the 9 pin connector on the cable P N N6100402 to the Remote Start Stop connector port 3 on the rear panel of the HP 6890 or 5890 NOTE You can use either port 3 or port 6 since they are wired in parallel with each other 2 Ifthe HP6890 or HP 5890 is prepared and ready to start arun placing a contact closure shorting across the white wire and either one of the black wires will start the run 3 The open collector output from the red wire to either one of the Black wires simulates the GC Ready Output relay s Normally Open position with respect to Common at the black wire Use the red wire as the Ready Output relay s Normally Open position and use the black wire as the Ready Output relay s Common position 4 When the HP6890 or HP 5890 is Ready to begin the next run the red wire will be effectively shorted to the black wire ground through the transistor s collector emitter junction The HP 6890 GC cannot accept BCD signals from any external samplers including PerkinElmer samplers There is no cable or procedure available to accomplish this 57 Installation 1 You must ensure that the HP 6890 GC or HP 5890 GC data file and the appropriate HS vial number correspond to each other 2 Locate the I O port on the rear panel of the HS 3 Connect the white wire of the cable assembly P N N610 0402
15. Pressurization Time Headspace only After equilibrium has been reached the vial is pressurized by the carrier gas to a pressure equal to the sampling head pressure P2 You can set the 112 Operation pressurization time to any value between 0 1 and 999 minutes The default value is 1 minute Injection Time Headspace only At the end of the pressurization time the carrier gas supply is interrupted by closing a valve in the carrier gas supply line and the pressurized gas in the vial expands onto the column resulting in a flow of the headspace gas from the vial to the column You can set the injection time to any value between 0 and 9 99 minutes The default value is 0 04 minutes Injection Volume Headspace only The injection volume mL is based on the column flow rate and the injection time If you have opted to display a volume rather than a time on the Options tab then you will enter an injection volume here and the corresponding injection time will be displayed You can set the injection volume to any value between 0 and 10 mL Based on the injection volume that you enter and the column flow rate an injection time is calculated The injection time corresponds to the flow rate measured at the end of the GC column under normal atmospheric pressure and temperature conditions NOTE The calculation of the injection time for the entered volume is based on the assumption that the vial pressure remains constant during the sa
16. The HS is finishing up a vial sequence or returning the last vial Leak Test Time The timer for the leak test Error Condition A fault condition is occurring See Status Messages on this table and pages 314 315 Economy Mode The instrument is in economy mode Dry Purge Time The trap is being purged with carrier gas to remove water Inject Standard The internal standard is being added to the tube 295 Troubleshooting Sampling The pressurized vial is being vented through the trap Trap The trap is being conditioned at top trap temperature Conditioning purged and vented Trap Test The gas is flowing from the trap to the GC column Analyzing An analysis is in progress Dry Purging The trap is being purged with helium out to vent Economy Mode Fatal Error The instrument is in the economy mode The heaters have been switched off and the carrier gas flow has been reduced to the minimum A fatal error is a malfunction from which the instrument cannot recover without user intervention The instrument may need to be switched off and then turned on again If the fatal error reoccurs you will need to contact your PerkinElmer Service Representative Inject Standard The internal standard is being added to the vial Out Split Adjust Adjust the outlet split flow SV2 is open Primary Desorb The tube oven is moved into position and the sample vial is hea
17. load another vial rotate sample tray etc Run Status Log Log Report Oven Status Tray Rotation ee ountd own 1 min 9 sec f Lastvial loaded 1 Tray Rotation cou Available positions 2 20 i P 4D 1 min 9 se W The tray will rotate back when i Last vial loaded countdown reaches zero or T Available positions when the OK button is pressed Ba Rotate _ The tray will rotate ba countdown reaches z 152 Control Function Operation Description Last vial loaded Displays the last vial loaded Available positions This feature informs you as to which posi tions are available for loading new samples Some of the positions may appear to be empty because the samples are loaded into the Headspace This will help the user avoid the in use position The vials displayed will be from the next vial position to the upper range of a program step i e program step 1 to 10 next vial to be analyzed is 6 load in available positions from 6 to 10 OK The tray also rotates back when you press on the OK button However when Available positions parameter has a indicating that no vials remain scheduled for sampling pressing OK will not rotate the tray back to its original position Note To stop the entire sequence you must close the modal Countdown dialog first before the Stop button can be enabled Rotate The tray rotates 90 counterclockwise each time it is pr
18. An alphabetic keypad is displayed Enter the desired sequence name To enter numeric characters press the 189 Method Development Num key Press Alpha to return to the alphabetic keypad Press OK to enter the new name for your method and then press Save to save your new method Press Done to complete the selection and return to the Run tab To edit an existing method 190 1 Press the Tools button and then select Method Editor from the drop down box Select one of the methods from the list and press the Edit button The Edit Method tab opens The Edit Method tab is almost the same as the Status tab It contains four tabs that will allow you to set up various analysis parameters The parameters for the existing method are displayed Edit the parameters required for the updated method Press the Options tab and enable any options that are required to complete your method Select the desired operating mode If you are using MHE mode you must set certain parameters accordingly See MHE Theory and Calculations Headspace Only on page 229 for details Press Save to save your updated method Select another method to edit or press Done to complete the selection and return to the Run tab Method Development Temperature Tab Headspace and HS 40 110 Trap Needle and Transfer Line Temperatures The needle temperature should be set high enough to prevent condensation but not so high that the septum is burned with a ne
19. Cleaning the Trap 4 s4s cccaseseceascacarsecuaisaecascers 282 Trap Festen a E N 284 System Maintenance cece ceseceeceseeeseeeseceseeeseeees 288 Troubleshooting ccctesseesstessnteneseeees 293 Status Messages nnee ieee seid ie SEA 295 TurboMatrix Headspace and the HS 40 110 Trap Instrument Fault Conditions 2 0 0 0 eee essences 297 ATTENTION Carrier Gas Shut Off eee 306 Troubleshooting Procedures 307 Peak Broadening or Splitting 0 0 eee eeeseereeereeee 309 Contents System Contamination for the Headspace and HS 40 110 Trap 312 Poor Sample Recovery or Reduced Sensitivity 00 eee eseesceseeeseeeneeeeceeeeeeeeees 315 HS 40 110 Trap Only Troubleshooting 320 Monitor Vial Integrity eseese 321 Troubleshooting the Leaks eee eeeeeeee eres 324 Log Error Messages ceeceesceeseceeceseeeeeeeeeeeneees 324 Fast pressure decay acsccercscascovsacecsdtaiaestcars 324 Slow pressure decay ccsieninpsaacaseet cagcouns 325 Extended therm Trap eeeceeeeeeeeeees 325 GC not ready asics cisscdsacsegsiaasactededesonaderesses 326 Status Messages 20 0 csceesccseecoeetssceserseneceeteeeeees 327 Appendices esictikcsiepituticoniinnsacdicainmaiiaihinmiaanian 333 Appendix Accs ce ate teis cence Wie eerste tie 335 Customer Service cece eeeceesceseeeneeceeceseeeneeeaees 335 APPendixXBisics cesses dsesesieves cesses sahh donesioees hile 336 Warranty Exclusions and Limitations 336
20. Introduction When you are creating a new method normally you will optimize the method by performing analyses at various settings You can use the Status tab to enter the desired parameters and options and then run a few samples to evaluate the method You can then adjust parameters accordingly and run more samples until you obtain the desired results Once you have the method you want you can use the Save As command in the Tools menu to save the new method You can then update the method at any time or create new methods based on the current one using the Method Editor and the Edit command Principles of Headspace and Headspace Trap Analysis Headspace analysis is the analysis of the vapor lying in equilibrium over a solid liquid sample in a sealed container For practical headspace analysis the sample is sealed in a vapor tight vial placed in a thermostatted oven and heated to a preset temperature When equilibrium is reached between the solid liquid phase and the vapor phase the sample vial contains the volatile material in equilibrium between the solid liquid sample and the vapor lying over it A defined amount of the vapor is taken and carried to the column in the gas chromatograph for analysis Total vapor in the case of the headspace trap is taken and carried to the column in the gas chromatograph for analysis With this technique only volatile substances reach the column the non volatile substances remain in the sample vial
21. NOTE Ifthe trap is broken or you cannot remove it easily you will also have to loosen the screws and then carefully remove the trap and any broken pieces 253 Routine Maintenance Figure 101 7 Slide the housing off and rest the housing on the carousel as shown in the next photo 254 Routine Maintenance Figure 102 8 Remove the nut as shown in Figure 100 Use the Trap Alignment tool to remove the old O ring See the following photo for the location of the O ring 255 Routine Maintenance Figure 103 9 From the side of the instrument door take out the Trap Alignment tool See the next photo 256 Routine Maintenance Figure 104 10 As shown in the following photo use the tool to slide on and loosely screw on the brass fitting over the new O ring Do not over tighten You will notice that as you push in the tool the O ring will offer a slight resistance This is supposed to happen Remove the trap alignment tool 257 Routine Maintenance Figure 105 NOTE If you are using only the TurboMatrix Headspace mode you do not need to install the trap Use the brass button shipped with the instrument to seal the trap area from the analytical path 11 Replace the housing that is laying on the tray and tighten the screws in the housing Tighten the housing just enough that it is secure but you can still move it slightly 12 Insert the Trap Alignment tool back into the housing The tool w
22. Otherwise the protection provided by the equipment may be impaired WARNING 21 Introduction Electrical Safety Electrical Protection The following precautions have been taken to provide electrical protection Pollution This equipment will operate safely in Degree environments that contain nonconductive foreign matter up to Pollution Degree 2 as defined in IEC 61010 1 Table 3 Electrical Protection If you suspect for any reason that the instrument is not electrically safe for use do not operate it and secure it against any unauthorized operation Have the equipment inspected by a PerkinElmer Service Engineer or similarly qualified person The instrument is likely to be electrically unsafe when it e Has been subjected to severe transportation stresses e Shows visible damage e It has been subjected to prolonged storage under unfavorable conditions 22 Introduction A WARNING This instrument must be grounded for maximum protection against electric shock Intentional interruption or disconnection of the protective conductor earth ground inside or outside the instrument is prohibited Hazardous voltages are present in the instrument To prevent the risk of electrical shock the line cord must be unplugged from the AC outlet before removing any instrument covers or panels requiring the use of a tool Hazardous voltages remain present in the instrument even when it is swi
23. Refer to Changing the O Rings on page 252 In the upper needle seal assembly there is only one O ring located on the bottom of the seal assembly Do not touch the new o rings with your fingers Use forceps or tweezers to remove the o ring from its bag and place it on the seal assembly If you touch the o ring for any reason throw it out and use a clean one 12 Ensure that the correct needle seal assembly orientation is maintained The side with the o ring is placed down The assembly must be correctly seated before securing it with the adapter sleeve 13 Tighten the adapter sleeve As you tighten the adapter sleeve the needle unit drive assembly will move the rack down You will need to turn the rack counter clockwise to move it out of the way Do not over tighten the adapter sleeve as it will damage the seal assembly and cause it to leak 14 Unscrew the seal removal tool from the threaded hole M3 of the seal assembly 15 Carefully slide the needle holder back into the rack as far as the stop 16 Securely hand tighten the knurled nut Changing the Lower Seal Assembly The seal assemblies need to be replaced if they are scored or scratched on the top or bottom surfaces The graphite coated Viton o rings BO19 8110 should be changed every 1500 injections The instructions below refer to items shown in Figure 98 To change the lower seal assembly 1 Turn off all heated zones by setting the temperature to 0 Allow ap
24. STOP IN READY IN FAIL OUT NORMALLY OPEN START NORMALLY OPEN READY NORMALLY OPEN READY NORMALLY CLOSED LOTT TurboMatrix I O Port Figure 1 The HS Input Output I O Port Diagram and Photo 50 Installation HS Output Signals The Input Output Port of the HS enables communication with other instrumentation for example GCs and data handling systems NOTE The relay contacts are rated to switch 10 W maximum Do not exceed SOV or 0 5A Ready Out These signals which indicate the HS ready status are provided by a normally open relay A contact closure between pins 1 and 2 Ready Out signals that the HS is Ready or a contact break between pins 3 and 4 signals that the HS is Ready Normally the HS acts as the controller and neither of the above signals are connected Start The Start Inject signal is a relay contact closure between pin 5 and 6 Start Out and coincides with the start of an injection onto the GC column The contacts remain closed for 20 seconds The Start signal is usually used to start a GC run by connecting it to the GC Start terminals NOTE Normally the GC is used to start the data handling system or Remote Control Software or Bridge Application Fail Output Signal The HS can be used with instrumentation that is unable to read the BCD sample vial number and therefore unable to report it with the chromatographic results In this situation care is required when a chr
25. analytes Setting a high temperature may cause sample decomposition by oxidation The transfer line can also be set to any value between 35 and 210 C in steps of 1 C If you set the temperature to 0 the heaters are turned off Oven Thermostatting Temperature This is the temperature at which you will equilibrate your sample The temperature must be set so that the maximum amount of analyte is moved into the headspace in the minimum amount of time You must also consider the thermal stability of your sample when you set the thermostatting temperature Always run the instrument with the front door panel closed to prevent injury Over heating or pressurization the vial may cause the vial to implode WARNING The oven can be set to any value between 35 and 210 C in increments of 1 C If you set the temperature to 0 the heaters are turned off Temperature Mode activating the track oven option These three temperatures can be combined so that when you raise or lower the combined temperature all three settings are adjusted If for example you enable the combined option and raise the temperature by 5 C then the needle the transfer line and the thermostatting temperature will all be raised by 5 C If you choose the separate option then each temperature can be set independently Cryofocusing Temperature Headspace Only This option is only available if the cryofocusing accessory is installed This 1 B
26. e Sample vials just unloaded from the thermostatted oven into the magazine can be very hot and may still be under pressure Cool and vent the sample vials before you open or dispose of them Use the PerkinElmer venting tool P N B009 9590 TurboMatrix units provide optional automatic venting e Use only the cap removing tool to open the sample vials P N B003 8135 under the fumehood e Carefully check the sample vials after cleaning for hairline cracks and damage before reuse Do not use unsuitable vials Replace the reused sample vials regularly PerkinElmer vials are guaranteed for single use only Cleaning and Decontamination Before using any cleaning or decontamination methods except those specified by PerkinElmer users should check with PerkinElmer that the proposed method will not damage the equipment Decontamination Customers wishing to return instrumentation and or associated materials to PerkinElmer for repair maintenance warranty or trade in purposes are advised that all returned goods must be certified as clean and free from contamination The customer s responsible body is required to follow the Equipment Decontamination Procedure and complete the Certificate of Decontamination These documents are available on the PerkinElmer public website http las perkinelmer com OneSource decontamination htm If you do not have access to the internet and are located in the U S call toll free at 1 800 762 4000 or 1
27. 0 1 minute NOTE This unique Decay curve profile feature is memorized and used throughout the vials run in order to Monitor Vial Integrity alerting the operator if the decay curve for any sample run under the method is not consistent with the curve in the memory This could indicate improper vial septum seal or incorrect sample volume Leaks of a different origin and cause are also immediately detected The system optionally reports a wrong curve in the Log tab or it even stops the run choice of the Stop on Vial Error option With the Monitor Vial Integrity and the Stop and Vial Error enabled The system terminates the counting after three consecutive vials have failed the Vial Integrity test This feature and various aspects on it will be handled in the Troubleshooting chapter Cycles From the Timing tab and the Setup button we can set the Cycles number in the Trap Timing pop up screen Timing tab gt Setup button gt Trap Timing screen 201 Method Development The Cycles number can be set from 1 to 4 cycles and is the number of times Vial Pressurization and Trap Load will be performed per vial Less than 1 of the headspace vapor is lost as a vial residue More than 99 is adsorbed and focused in the HS 40 110 trap Run Status Log DryPurge Trap Hold 05 05 rap Timing Cycles Pressurize 10 min DecayTime 20 min Calibrate Decay Time i E ee ee JTemp timing Option Jepe STANDBY Oct
28. 15 Sa Rotate Tools v Figure 79 Pressurization Time After equilibrium has been reached the vial is pressurized by the catrier gas to a pressure equal to the vial pressure and for a time set as Pressurize time in the Trap Timing screen that pops up if you touch the Setup button 202 Timing tab gt Setup button gt Trap Timing screen Method Development Run Status Log DryPurge Trap Hold 0 5 05 rap Timing Cycles Pressurize 1 0 min Decay Time 20 min Calibrate Decay Time E ee JTemp Timing Option Jpepce STANDBY Oct 15 _ Stat Rotate Tools y Figure 80 You can set the pressurization time to any value from 0 1 to 999 minutes in steps of 0 1 min The default is 1 minute Trap Hold HS 40 110 Trap Only This option allows you to input the number of minutes that the trap will maintain the maximum temperature In order to release the analyte from the trap and completely clean the trap from sample residue to ready it for next sample the maximum temperature must be maintained for a sufficient amount of time A recommended trap hold time is five minutes Its range of values is 0 999 minutes in steps of 0 1 minute Dry Purge Time HS 40 110 Trap Only After trap loading is the optional step of removing the moisture from the trap tube This option allows you to input the number of minutes required for the dry purge The dry purge allows helium to
29. 203 925 4602 8 30 a m 7 p m EST and speak to Customer Support In Canada call toll free 800 561 4646 and speak to Customer Support 33 Introduction If you are located outside of the United States or Canada please call your local PerkinElmer sales office for more information Cleaning the Instrument Exterior surfaces may be cleaned with a soft cloth dampened with a mild detergent and water solution Do not use abrasive cleaners or solvents 34 Installation lt gt Installation Introduction Before the instrument arrives you may have received a pre installation checklist to ensure that your lab is setup correctly If you did not receive the checklist refer to the Pre Installation Checklist below to ensure that you have enough space and that electrical and gas supplies meet the requirements of the HS the GC and all of the related support equipment Normally the instrument is installed and set up by a PerkinElmer service engineer Installation consists of seven steps 1 Unpack the HS and place it correctly on the lab bench 2 Connect gas and electrical supplies to the HS 3 Connect to the GC 4 If you are using the optional Remote Control Software you must connect and configure a suitable PC mi Connect any optional accessories Leak test the system 7 Perform a test run to ensure all system components are operational Installation and setup of the HS are relatively straightforward The i
30. Appendix Coreene ada anne ai 337 Supplies Accessories and Replacement Parts 337 Sample Vials and Seals ec cesceeeeeeeeeeeneeenseees 337 Tools for Sample Preparation cece eres 338 Replacement Partson eienn 338 Adapter Kits for Gas Chromatographs 340 Appendix Diorren oeaan ete ie Hoe aeri i 341 Reference Material cee eeeeesceeseceseceeeeeeeeneees 341 Headspace Gas Chromatography cece 341 Laboratory Safety Practice ee eeeeeeeeeeneee 342 Multiple Headspace Extraction ceceeeeeeees 342 Bibliography isis eh tetioi ai iene 343 Contents 10 Introduction 1 lt gt Introduction Introduction In headspace sampling the sample either a gas a liquid or a solid is placed into the headspace vial which is closed immediately and equilibrated and pressurized An aliquot is then withdrawn from the closed vial and transferred directly to the gas chromatographic system or pre concentrated on a trap for focusing in headspace trap only The HS is an automatic sampler for headspace analysis Three models of the HS are available as are various accessories that enhance the operation of your system TurboMatrix Headspace The HS 16 provides automated headspace analysis of up to 16 vials not available in the trap functionality Standard PerkinElmer vials can be loaded into the vial magazine A single vial oven allows you to thermostat your sample before injection onto the GC via th
31. As with splitless operation the HS supplies the total carrier gas flow for the HS GC system To set the carrier gas flow for on column sampling 1 102 Connect the capillary column to the sample head as outlined in the section Installing the Heated Transfer Line or in the HS 40 110 trap in the Installation chapter Determine the column head pressure This information will be part of the GC method Set the HS carrier pressure so that it is the same as the required column head pressure If you have manual pressure control adjust the pressure regulator until the desired value is displayed on the PPC tab Switch to the PPC tab and enable actual so that you are viewing the current values rather than the set points See PPC Tab on page 216 Operation 5 Ifyou have PPC control enter the desired value on the PPC tab and allow the HS to reach the set point See PPC Tab on page 216 6 Turn off the supply of carrier gas at the GC Monitor the system flow from the PPC tab 7 Check the column flow rate by connecting a flow meter to the outlet of the GC column NOTE It is assumed that if a cylinder containing an Internal Standard gas is used its pressure regulator outlet is connected to the respective inlet at the back of the trap unit The Touch Screen Display You will control the operation of the instrument through the touch screen display With a stylus or your finger lightly touch the screen to enter data and issue comm
32. End A as CN Sw PTFE Tubing Plug for Heater Figure 9 The HS End of the Transfer Line 3 Slide the transfer line into the retaining collar so that the top of the tube is flush with the collar Do not tighten the mounting screws as you will need room to install the fused silica tubing The transfer line and the glass lined tube GLT adapter should be in a straight line 4 Remove the cap from the outlet of the GLT connector tubing 5 Insert the GLT connector tubing into the nut and ferrule and install these into the fitting of the needle unit 6 Tighten the nut slightly allowing some back and forth movement of the GLT connector tubing 7 Slide the GLT connector tubing into the needle unit until it stops 8 Tighten the nut to hold the GLT connector tubing in place Do not over tighten the nut as you may damage 62 10 Installation the ferrule or crack the glass in the GLT connector tubing See Figure 9 Unravel approximately 1 meter of the fused silica tubing Insert the fused silica tubing from the GC end into the transfer line until approximately 5 cm of the line extends from the HS end of the transfer tubing Slide the 1 16 sleeve nut and the graphite ferrule onto the end of the fused silica tubing between the transfer line and the GLT connector tubing Sleeve Nut P N 04961109 Fused Silica Transfer my an 09920127 Tubing Graphite Ferrule P N 04972433 GLT P N B0503956 AM
33. Gas Connections on page 75 Tubing Always use clean tubing preferably made of copper or stainless steel with the minimum possible number of joints If necessary clean the tubing by passing a stream of clean inert gas through the tubing while baking it in an oven at a temperature high enough to remove any trace organic solvents CAUTION Never clean carrier gas tubing with organic solvents Any remaining traces of solvent will contaminate your system Use compression fittings to make any joints in the tubing Do not use soldered joints especially if an ECD is to be used The flux used in solder may contain a strongly electrophilic compound 237 Routine Maintenance Sample Vials and Seals CAUTION Using sample vials caps and septa other than those supplied by PerkinElmer may result in improper operation of the TurboMatrix Headspace or Trap Headspace Sampler Damage to the instrument and or loss of sample materials or data resulting from the use of sample vials caps and septa not supplied by PerkinElmer may occur The subsequent service visit to remedy the situation caused by the choice to use these non PerkinElmer sample vials caps and septa is not included under your warranty or service contract agreement Your Service Engineer can discuss the benefits of using only PerkinElmer sample vials caps and septa When samples have been collected the vials should be analyzed as soon as possible WA
34. Guide it will be referred to as the HS 40 110 Trap The HS 40 110 Trap includes the ability to prioritize sample vials containing rush samples during an active sequence and a time saving pre programmed shut down and wake up mode that allows for complete unattended operation The HS 40 110 trap improves headspace detection limits It allows for the extraction of the full vapor content of the sample vial into the trap to the GC and subsequent transfer European Union Industrial Environment 230V 50Hz TurboMatrix headspace instruments manufactured for use in the European Union are intended for the industrial environment The instrument is to be connected to a mains power network supplied from a high or medium voltage transformer dedicated for the supply of an installation feeding a manufacturing or similar plant Industrial environments are characterized by the existence of one or more of the following conditions e industrial scientific and medical ISM apparatus are present e heavy inductive or capacitive loads are frequently switched e currents and associated magnetic fields are high These are the major contributors to the industrial electromagnetic environment and as such distinguish the industrial from other environments The instrument is not intended for connection to a public mains network supplying residential commercial and light industrial locations 14 Introduction About this Manual This manual is an inte
35. HS 40 110 Trap Before withdrawing a headspace sample for analysis the vials are thermostatted until equilibrium between the two phases is reached In the HS 16 one vial is thermostatted With the HS 40 and the HS 110 you have the option of thermostatting up to 12 vials NOTE Although the thermostatting oven has 15 positions the software will only allow up to 12 vials for simulaneous thermostatting The thermostatting temperature you set here will depend on your sample and the sample matrix There are many factors to be considered when you are setting the thermostatting temperature A detailed discussion of the effects of temperature on vapor pressure partition coefficients and headspace sensitivity is provided in Static Headspace Gas Chromatography Theory and Practice by Bruno Kolb and Leslie S Ettre P N N1011210 You can set the thermostatting temperature to any value between 35 and 210 C in steps of 1 C If you set the thermostatting temperature to 0 the heaters are turned off Although the HS will allow you to set the thermostatting temperature to a maximum value of 210 C the vial seals are rated for lower temperatures see the Seals section earlier in the chapter The seals will begin to vent when the internal vial pressure exceeds 73 psi 500 kPa Track Oven TurboMatrix Headspace and HS 40 110 trap Temperatures The Combined temperatures option is activated if you enable the Track Oven by checking its box
36. Log tab allows you to view the analysis history of the HS An entry will be made whenever a vial is analyzed Entries will also be made if an error occurs The Run tab Status tab and Log tab have three buttons displayed on the bottom of the touch screen These three buttons are Start Rotate Load and Tools The Start button will start a method or sequence If the system is not running the Rotate function will be visible If you press this button the magazine will rotate so that you can load samples with the system off You can press this button while the system is running and you will be able to add samples to the magazine while the analysis is in progress The Tools menu provides a drop down menu of options available such as Method Editor Save As Preferences Calculator etc The Run Tab Once you have created a method by which to run the samples you will load the magazine and run the samples from the Run tab See Creating a New Method in the Method Development chapter for details You can run samples using the archive or a saved method or a sequence of saved methods The options on the Run tab are determined by selections that have been made on the Method screen 104 Operation Single Method Operation To facilitate operation for routine analyses single method operation provides access to the vial range only Single method operation and the desired method are selected by touching the method window and selecting the corr
37. Monitor Vial Integrity This option is an excellent tool in HS or Trap operation This tool can help reveal additional problems These problems are brought to light by the automatic dynamic comparison of each vial s decay curve with that in the system memory from the Calibrate Decay Time procedure A couple of these problems are analyzed here Cause Loss of Sensitivity Pre Injection Peaks These two problems are attributed to and explained as follows Trap Dry Purge low flow If there are no leaks but the Trap Dry Purge flow is low correct flow is 50 ml min during the Trap Load step the system will not have transferred the entire amount of the HS vapor to the Trap before the Decay time has elapsed As a result less analyte will be injected in the Desorption step A bad pressure Decay curve is illustrated next This problem will result to a Loss of Sensitivity and possibly a poor peak repeatability 321 Troubleshooting x _ 60 0 2 jo a G 3 300 0 0 0 04 O08 12 16 2 Time min Calibration Vial 1 Time 20 Decay Time 1 0 min STANDBY 12 27 14 Figure 128 The straight line is a result of too low a Trap Dry Purge flow rate The flat line is commonly caused by failing to open the trap Dry Purge vent slide On Off valve after a gas leak test This valve should be left in the ON position pulled out toward the operator A similar result can be obtained with a very low T
38. NOTE Each Trap is shipped with a product sheet Air Monitoring 285 Routine Maintenance Trap Installation and Operating Instructions Part No 0993 6724 Split Trap Test lt Vent Bs Pd t 10mL min VALVE STATE TABLE Leak Test SVia Figure 122 Split Trap Test 286 Routine Maintenance Splitless Trap Test a eel j 10mL min t 50mL min Leak Test SVia Figure 123 Splitless Trap Test 287 Routine Maintenance System Maintenance System maintenance and a variety of part replacements can be carried out without switching the HS Trap unit off In the Tools drop down menu choose Maintenance and then touch the Column Isolate command See the next screen Run Status Log I Hi Psi Inject Method Editor Save s Operating Mode Preferences Constant Calculator Leak Test TestL_Env5_2 Temp Timing STANDBY _ Start_ Fars lumn Isolate Valve Le ak Test Rotate Figure 124 The following screen appears 288 Routine Maintenance Run Status Log 9 T HiPsi Inject system isolation mode to allow service of trap and sampling head JTemp Timing Option yppe STANDBY 10 06 04 Stat Rotate Tools w Figure 125 In Column Isolate see figure below the system supplies the Isolation Flow to isolate and protect the transfer line and the GC column At the same
39. Purge step the PPC applies the same pressure to the Trap as the one set for the Desorption step Run Status Log Column 35 0 psi Set Point Actual veqaso C JTemp Timing Option ppc STANDBY 10 06 57 Stat Rotate Tools x Figure 46 HS 40 110 Trap Status Tab PPC Tab The Log Tab Log Report The Log tab allows you to view the analysis history of the headspace An entry will be made whenever a vial is analyzed Entries will also be made if an error occurs for example Vial Integrity The start time of the current analysis or sequence is displayed along with information on completed runs 129 Operation Run Status Log Log Report _ Oven Status Run Log Oct 05 2001 11 13 54 Instrument Serial HSOO000000 Instrument Name HS110 Method DMF_45psi Vial Thermo Inject Status 5 11 14 25 11 20 26 Done 6 11 19 25 11 27 02 xThermo Estimated Run Time 0 16 00 STANDBY 10 07 00 Stat Rotate Tools v Figure 47 Log Report Tab Oven Status lIf you are operating the HS 40 or HS 110 with the 15 vial oven you can view the status of the vials in the oven The current temperature of the oven is displayed The number of the vials that are in the oven is also shown as is the location of the vial that is currently being sampled The current temperature of the heated oven and the direction of rotation are also shown The vial number the method with which it was a
40. Start Cable 55 Installation Connecting the HS to other GCs except the HP 5890 HP 6890 and HP 7890 To connect the HS to other GCs except the HP or 5890 or 6890 1 Connect the generic Ready Start Cable Assembly P N N1011206 between the Input Output socket on the HS and make the appropriate connections on the GC as shown in Figure 5 2 The HS requires a contact closure or equivalent to be applied between pin 9 Ready In and Ground pins 12 13 or 14 to receive a GC ready signal The HS provides a contact closure between pin 5 and pin 6 Start Out to start a GC run NOTE In the following illustration Pin 9 12 13 or 14 are Ready In and Pin 5 6 and 7 are Start N O 14 131 12 9 41 e mW 10 ie Zz 9g Ready 8 7 5V eo lt WMm __g 6 OV Ext CO Star 4 3 GC 2 Pin 1 TurboMatrix I O Port Figure 5 Connecting the HS to Another GC Using the Ready Start Cable 56 Installation Connecting the HS to the HP 5890 and HP 6890 The HP 6890 or 5890 GC uses one TTL connection for both Start In and Start Out and uses a second TTL connection for Ready In and Ready Out The HP 6890 GC does not have a Ready Output relay or a Ready Start relay and therefore it needs a special cable kit to communicate with the HS P N N6100410 This kit contains the parts necessary to connect a PerkinElmer sampler to a HP 6890 GC To connect the HS to the HP 6890 or 5890
41. Trap Setup Tab Stop on Vial Error This option will stop the run if there is a vial error such as a missing vial or there is something wrong with the vial Monitor Vial Integrity This option will report on the Log tab any deviation of a vial pressure decay from the Decay Time set in the method see Calibrate Decay Time If the Monitor Vial Integrity Error and the Stop on Vial Error are enabled in this tab the system will terminate the counting if three consecutive vials fail the Vial Integrity test If the Stop on Vial Error is not enabled the system will report the vial discrepancies on the Log tab but will not stop the counting Connect Tab Key Clicks This option if enabled sounds a tone each time a button is pressed This feedback confirms that you have pressed a key Bar Code tThe bar code reader is a future upgrade Contact PerkinElmer for more information 145 Operation Baud Rate Refer to the computer setup options to determine the baud rate as this value will depend on the computer The HS baud rate can be set from 300 to 57600 to match the computer s setting Handshake Select the desired Handshake mode Choose None Xon Xoff or hardware Normally you will use None Language You have a number of language options You can select the language to be displayed on the touch screen display Select the desired option from the drop down menu Press OK to confirm the selection and close the tab The tou
42. and the desired injection volume The HS will automatically calculate the corresponding injection time If you select time as the injection mode the HS will determine the injected volume from the time you have entered on the timing tab and the column flow rate The calculation of the injection time for the entered volume is based on the assumption that the vial pressure remains constant during the sampling and no other gas is supplied to the column In the case of balanced pressure sampling systems the injection volume can be controlled by the injection time The injection time should be limited to a few seconds During the injection time the transferred gas volume is determined by the actual gas velocity If we consider the same linear flow rate at the column inlet ui you can calculate the transferred volume Vu injected onto the column from the injection time t and the cross section of the column Q Vu Q uidt Equation 1 The admissible sample volume onto an open tubular column is limited by the column s sample capacity Overloading the capillary column leads to band broadening and this effect is independent of the method of sample introduction 207 Method Development Principles of High Pressure Sampling Headspace Only High Pressure Sampling This technique utilizes internally regulated carrier gas The carrier gas is supplied by the HS PPC module If you are using the high pressure injection option you will
43. assumed that if a cylinder containing an Internal Standard gas is used its pressure regulator outlet is connected to the respective inlet at the back of the trap unit 79 Installation Figure 20 Connections on back of the instrument 80 Installation Installing the Trap in the HS 40 110 Trap The HS 40 110 trap is shipped with the trap housing already installed You must install the trap NOTE When installing the trap in the instrument for the first time or you must take the trap assembly apart you must do an alignment procedure If you are just removing an old trap and replacing it with a new trap you do not need to do an alignment procedure Wear gloves when you are handling the trap Handle the trap with great care since it is made from glass and can easily break WARNING NOTE Before proceeding always have one or two spare traps on hand in case of breakage NOTE Turn off the unit and Column Isolation will be automatically applied CAUTION Do not over tighten Only finger tighten the large thumbscrew otherwise you will break the trap 1 Remove the looks cover by opening it and taking the cover off the hinges by lifting it straight up Turn off the HS40 110 trap or start the column isolation flow This will enable gas flow to continue to the GC but the trap will be blocked off 2 Remove the large thumb screw and put it in a secure location 81 Installation 3 Pull out the dry purge
44. by the choice to use these non PerkinElmer sample vials caps and septa is not included under your warranty or service contract agreement Your Service Engineer can discuss the benefits of using only PerkinElmer sample vials caps and septa 97 Operation Before beginning operation ensure you have adequate supplies of vials caps septa and other sample handling materials Ensure that the materials you are using are compatible both with your sample and your sampling method Powering up the Headspace Sampler Before beginning operation of the instrument you may want to familiarize your self with the layout of the instrument and the basic concepts of headspace chromatography Before beginning operation you should 1 Connect the electrical and gas supply lines set the required flow rates and check that all gas connections are leak tight Refer to Chapter 2 for details 2 Ensure the GC and any related support equipment and software are installed and are displaying a ready status i e GC detectors GC data acquisition systems etc 3 If you have any options installed they will be turned on with the unit and allowed to warm up or cool down as required Refer to the documentation supplied with each installed accessory 98 Operation Needle Unit Manual or PPC Thermostatting Adjustments Oven Compartment Oven Compartment Door Latch ON Switch on rear of instrument Touch Screen Display Mag
45. can be shorter down to 20 mm if 0 32 mm or 0 53 mm i d columns are being used Insert the fused silica tubing into the injector and secure the HS injector adapter Insert the column into the base of the injector and push it through the liner until it just reaches a stop about 8 cm Do not push the column too hard At this point the fused silica transfer line and the column should be at either side of the restriction in the inner liner Withdraw the column about 2 mm and tighten the column ferrule and nut The liner seems to function satisfactory at pressure drops across the transfer line at 0 5 psi or above 2 5 psi is recommended approximately 20m1 min Installation 2 The GC split flow should be set to 10 ml min or more although higher flow rates will just waste gas Connecting to a Packed Column System If you are using a packed column in your GC you must use a packed column injector 1 Install the packed column as outlined in Installing the Heated Transfer Line at the GC Injector for Split Operation TurboMatrix Headspace Only on page 68 2 Set the HS pressure accordingly You may need to use the a high pressure injection to eliminate the possibility of pre injections See the section High Pressure Sampling in the Operation chapter Gas Connections For information on the Gas Supply System see the section earlier in this chapter Always use clean tubing preferably copper or stainless steel with the
46. direct connection 1 Before connecting the transfer line to the GC injector ensure there is gas flow through the transfer line 2 Connect the transfer line to the GC as outlined in the procedure Installing the Heated Transfer Line at the GC for Direct Connection previously in this chapter 101 Operation 3 Determine the column head pressure This information will be part of the GC method and should be shown on the GC display Refer to the GC user s manual for further information Set the HS carrier pressure so that it is the same as the required column head pressure If the column head pressure is 10 psi then set the HS carrier pressure to 10 psi If you have manual pressure control adjust the pressure regulator until the desired value is displayed on the PPC tab Switch to the PPC tab and enable actual so that you are viewing the current values rather than the set points See PPC Tab on page 216 If you have PPC control enter the desired value on the PPC tab and allow the HS to reach the set point See PPC Tab on page 216 Turn off the supply of carrier gas at the GC You may want to check the column flow rate by connecting a flow meter to the outlet of the GC column On Column Connection To perform on column sampling the GC capillary column is taken through the transfer line sleeve and connected directly to the needle unit Installing the Heated Transfer Line On Column Connection previously in this chapter
47. first Once you have enabled the priority vial locations the locations are not analyzed unless you issue the Priority command Touch the Priority Run bar at the bottom of the Status screen If you issue the Priority run command the current analysis will be completed and then the priority vials will be loaded and analyzed Once the priority 142 Operation vials have been completed the HS returns to where it left off and continues analyzing the vials as specified on the Run tab After a method or sequence has been started the Rotate button located on the bottom of the display changes to the Priority vial button Press the Priority run button to initiate the analysis of the priority vials The priority vials are analyzed according to the current method The Priority feature only appears if priority vials have been selected from the Priority Vials menu When you start a priority run the priority vials are loaded into the oven carousel as soon as possible The priority vials are analyzed using the current method After starting and during a priority run the status Priority Run is displayed on the status bar NOTE It is not possible to perform a priority Run in Progressive Mode Alarm Option Use the vial alarm option to warn you when the current method or sequence is about to be completed You enter the number of vials before the end when the alarm will sound If you enter 2 when the second from last vial is loaded into
48. high the column is being overloaded Action Increase the flow of carrier gas through the transfer line and then set the transfer line temperature to 210 C Allow the transfer line to purge overnight WARNING Ensure that the column liquid phase can withstand a temperature of 210 C If not then set the transfer line temperature to the maximum allowable for the selected liquid phase of column If you are observing a severe contamination problem you should disconnect the transfer line from the GC 311 Troubleshooting Make sure that the GC oven detector and injector are at room temperature before you start working on the Headspace as instructed here WARNING Action Reduce the injection time or volume to introduce a smaller sample Action Reconfigure your transfer line connection for split injection sampling Generally splitless sampling allows less flow through the sampling area Reduced flow may lead to increased sample carry over and thus worse analyte reproducibility This is due to less efficient sweeping of the needle area System Contamination for the Headspace and HS 40 110 Trap System contamination can be avoided with proper care and maintenance of you instrument Contamination can also be avoided by ensuring that your method is suitable for the compounds that you are analyzing When you are troubleshooting the HS GC system you should first eliminate the GC as the source of the con
49. in Unload Position 305 Vial Jammed in Oven 304 Vial Load Failure 302 Vial Missing 301 Vial Unload Failure 303 Features Control Software 180 Finishing 295 Flame Arrestor 48 Fuse Holder 241 Location 241 Replacing 241 Specifications 241 G Gas Compressed Safety Practices 28 Cylinders Storage 28 Regulator Safety Practices 28 Supply System 46 Gas Chromatograh Connections 46 49 Gauge Pressure 195 GC Cycle Time 113 GC Injector Zero Dilution Liner 168 GC Liner Zero Dilution 168 GC Not Ready 295 H Hand Crimped Vial sealing 177 Hand Crimper 176 Adjusting 271 Crimped Top Vials 176 348 Stamper Assembly 272 Stop Pin 271 272 Using 176 Handshake Mode 146 Headspace Analysis 185 Control Software 180 Gas Connections 78 Layout 98 Shutdown 160 Headspace Sampling Packed Column 227 High Background 312 High Pressure Build up in the Sample Vial 178 Sampling Option 208 High Pressure Sampling 159 Method Development 217 Principles 208 HS 40 110 Trap removing 276 HS 40 110 Trap Connections 79 103 HS 40 110 Trap Desorb Braze Assembly replacing 280 HS 40 110 Trap Maintenance 276 HS 40 Emulation 138 Humidity Laboratory 40 Hydrogen 48 I Information Chemical Safety 26 274 Safety 21 Sample Vials 32 Initializing 295 Inject Pressure 118 128 Inject Pressure Option PPC Tab 118 128 Inject Time 295 Injection Cannot Enter High Pressure 308 Mode 115 207 Number 117 214 Period PID 114 Phase 187 Preventi
50. in the oven When you are loading the HS 110 you must leave the load and unload spots empty You must also leave one further location on the outside ring empty for the HS to unload any vials that may be present in the oven The HS will search the outer ring until it locates the empty position To reduce the initialization time leave location 1 empty This is the first location that the instrument will look for the empty position Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses Fault Vial Jammed in Oven 304 Cause The nut that holds the needle in place has loosened and the needle cannot be lifted out of the vial Action Remove the needle See the section on The Sampling Needle in the Routine Maintenance chapter for more details Cause The vial is slightly eccentric or has material on the outside Action Turn the HS oven power off Allow time for the oven to cool Turn the power on and check if the cooled vial is removed during initialization Cause A mechanical problem has occurred Troubleshooting Action Contact your PerkinElmer service engineer Fault Vial in Load Position Cause You have placed vials in the load position of the HS 110 Action When you are loading the HS 110 you must leave the load and unload spots empty You must also leave one further location on the outside ring empty for t
51. in the air filling the vial Such volatile contaminants can be eliminated by storing the empty vials in a clean room and or by purging them with an inert pure gas before the sample is added to the vial NOTE If you are handling hazardous samples you may need to perform the following steps in a fumehood To prepare sample vials 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 48 147 Operation 1 Place the vial in a vial holder rack N930 1304 The rack is recommended to keep vials upright during filling and capping 2 Use a syringe or an appropriate pipet to fill the sample vial with liquid samples Do not fill the vial over the maximum fill volume for liquid samples Observe the maximum filling volume of 15 mL for liquid samples when using 22 mL sample vials Ensure the sample does not come in contact with the top of the vial 3 Load the cap Place the star spring into the cap and then using tweezers or forceps place the seal on top of the spring Push the seal into the cap so that it is flat Place the cap on the vial 4 Place the crimper over the cap Place one hand over the stamper to stabilize the crimper on top of the vial Use the other hand to squeeze the crimper Keep the hand crimper level when sealing the cap See the Accessories chapter Sample Vial section for further details The vials for HS GC analysis are produced in large quantitie
52. inappropriate Call your PerkinElmer Service Representative Trap duty error power is being applied to the heater but inappropriate results achieved Call your PerkinElmer Service Representative The following status messages are displayed during normal operation to indicate the current status of the instrument or the current analysis If there is more than one fault occurring at a time the instrument will cycle through them and display them one at time until they are corrected The following faults cause the instrument to stop immediately All heated zones are turned off and a message is shown on the display localizing the error Record the details of the failure before switching off the instrument Fatal error can only be remedied by switching the instrument off with the power switch waiting ten seconds and switching it on again The instrument will then restart and attempt to initialize itself If the error recurs please make note of the exact wording of the error message and contact your PerkinElmer service engineer Before you contact service ensure you have the following information e What you were doing when the error occurred e Any corrective action that you have taken e The exact wording of the error message and any numerical error codes e Additionally you should have this manual at hand 327 Troubleshooting Status Description Analyzing An analysis is i
53. injector for split operation 1 Turn off the GC and allow the injector to cool 2 Use a wafer scribe P N N9301376 or other column cutting tool to score and break the fused silica transfer 68 Installation tubing leaving a length of fused silica tubing extending 10 to 15 cm past the end of the transfer line break Figure 15 Cutting the Fused Silica Transfer Line 3 The transfer line is connected to the gas chromatograph using a stainless steel adapter and a septum 4 Place the septum into the adapter 5 Carefully push the fused silica tubing through the adapter piercing the septum GC Injector Adapter Septum Knurled Nut Capillary Column Transfer Line Assembly Figure 16 6 Connect the adapter to the end of the transfer line 7 The fused silica tubing must be cut so that 5 cm extends from the end of the stainless steel adapter not from the 69 Installation end of the insulated transfer line See the following figure D3 Silica Adapter i c Transfer Tube To HS Needle Unit Figure 17 Length of Transfer Line that Must Extend Past the Adapter for Installation at GC 8 Remove the septum retaining nut from the GC injector port Store this nut in a safe location for later use Transfer Line Fused Silica Transfer Tube 3 Re connect Threaded Collar to Adapter 4 Adapter Injector __ PIN B050 5266 1 Remove Septum Nut Septum Cap Septum P N N610 0153
54. obtain the required column flow Make a note of this pressure for later use On a manual system read the column head pressure in the GC injector from the pressure gauge on the GC This is the carrier gas pressure required to obtain the required column flow for the analysis Record this pressure for later use Allow the GC oven to cool 227 Method Development T Adjust the carrier gas flow to the packed column injector to 2 5 mL min with the flow meter at the column NOTE The bulk of the carrier gas is supplied from the HS A small flow from the GC is required in order to purge the carrier gas line and the top part of the injector This purge flow eliminates dead volume as well as back diffusion of headspace sample It is an important precaution in order to avoid sample carry over and ghost peaks A higher flow can be used but it will result in dilution of the headspace sample 228 8 10 1 12 Remove the septum cap from the packed column injector and connect the HS heated transfer line to the injector using the injector adapter Take care not to break the fused silica transfer line See the procedure Installing the Heated Transfer Line at the GC Injector for Split Operation in the Installation chapter Set the headspace carrier gas pressure P1 to a value approximately 3 psi higher than the column pressure recorded in step 5 P1 must be higher than the headspace pressure in the thermostatted vial
55. of the instrument is covered in this section Method parameters are listed along with a brief description A detailed discussion of HS method parameters and method development are provided in Chapter 5 Safety Precautions To protect yourself from harm and to avoid damaging the instrument please observe the following notes e Before using this instrument read and observe the safety information in Chapter 1 e Do not attempt to analyze sample carbon disulfide or other solvents with a self ignition point of 100 degC or less e Always follow the correct safety procedures and the manufacturer s recommendations when using any solvent Refer to the MSDS sheets for compound specific information e Do not touch moving parts of the instrument during operation e Do not operate the instrument with any covers or parts removed Supplies The TurboMatrix and HS 40 110 trap is shipped without sample vials septa caps or a crimper tool These parts are necessary to operate the HS and are available either individually or in the HS Starter Kit B050 5601 CAUTION Using sample vials caps and septa other than those supplied by PerkinElmer may result in improper operation of the TurboMatrix Headspace or Trap Headspace Sampler Damage to the instrument and or loss of sample materials or data resulting from the use of sample vials caps and septa not supplied by PerkinElmer may occur The subsequent service visit to remedy the situation caused
56. reinstall causing leaking See the following figure Figure 116 6 Use the trap removal tool P N N6701077 to carefully remove the trap See the following photo 278 Routine Maintenance Figure 117 7 Wearing gloves carefully remove the new trap from the box and insert it into the trap housing Figure 118 8 Put the ferrule on the trap the tapered edge must face towards the front at the front of the HS unit See the following photo LE n N PTFE Ferrule er Figure 119 9 By hand gently push the new trap in as far as you can 279 Routine Maintenance 10 Use the Alignment Rod P N N6700122 to gently push the trap into the O ring into the proper position You will feel a small pop as the trap goes through the O ring and is seated properly in the trap housing 11 Retighten the back nut until it stops 12 Inspect the dry purge assembly to see that it is not damaged Feed the dry purge assembly into the trap until it stops NOTE If the dry purge assembly is damaged see this chapter for information on replacing this assembly 13 Reinstall the trap housing Do not use any tools only fingertighten to tighten the thumb screw since it will damage the ferrule 14 The trap must be conditioned see the Routine Maintenance chapter for this procedure before analytical use by establishing carrier gas flows and heating the trap several times to remove any volatile impurities from the trap packi
57. s Guide P N 09936625 for detailed operational instructions If you are using another GC you must adapt the following instructions accordingly To configure your GC for split sampling PPC only 1 Configure the Split Splitless injector to be used in the AutoSystem XL or the Clarus 500 for HS 40 operation 2 Inthe AutoSystem XL or the Clarus 500 configuration set the Split Flow Offset to zero for your injector 3 Inthe GC method set the Split Flow to at least 2 mL min NOTE Split flow refers to the amount of carrier gas supplied to the injector from the GC A low split flow will result in less dilution of the injected headspace gas but will not deliver enough carrier gas to the GC injector to support a pressure program The split flow can be changed during a chromatographic run through the GC method timed events 4 After you determine a value for P1 open the PPC tab and enter the carrier gas pressure P1 5 Check your GC manual for the optimal column head pressure of your analytical column Adjust the split flow until the GC shows a pressure 10 kPa below the optimal column head pressure 6 Open the carrier gas regulator on the GC and increase the pressure Pac until you reach the optimal column head pressure as read on the GC gauge or PPC display 221 Method Development If you are using an instrument equipped with PPC with an AutoSystem XL or the Clarus 500 that also has PPC observe the following guidelin
58. s manual for instructions 3 Using gloves check the outer and inner liner components of the new composite liner for contamination or damage 170 Accessories NOTE Do not touch any parts of the liner with your fingers as you will contaminate the injector NOTE NOTE 4 5 Insert the inner liner into the outer liner Install the composite liner into the injector using a standard o ring The outer liner should be gently inserted into the injector Replace the injector head and secure with a wrench Thread a length of 0 32 mm i d deactivated fused silica tubing through the transfer line and attach it to the HS sampling head as outlined in Jnstalling the Heated Transfer Line at the HS Needle Unit TurboMatrix Headspace Only on page 62 The other end of the tubing should be threaded through the septum in the HS septum nut Score and cut the fused silica so that 62 mm is left protruding from the septum 57 mm from the edge of the septum nut This length can be shorter down to 20 mm if 0 53 mm i d columns are being used 9 Insert the fused silica tubing into the injector 10 Insert the column into the base of the injector and push it up through the liner until it just reaches a stop about 8 cm Secure the HS injector adapter Do not push the column too hard 11 At this point the fused silica transfer line and the column should be at either side of the restriction in the inner liner Withdraw t
59. set the injection pressure here You must first enable the option on the Options tab This option is available if you have PPC installed You can enable it on the PPC tab You will enter the desired injection pressure on the PPC tab in the Status tab or on the Method Editor tab High Pressure P2 must be higher than the internal vapor pressure in the headspace sample vial Ensure that pressure P2 does not exceed 500 kPa 70 psi Both P1 and P2 are supplied by the PPC module at V1 The PPC module automatically increases the pressure from P1 to P2 at the start of pressurization The PPC module returns the pressure to P1 after the withdrawal time or vent time GC Injector Figure 82 High Pressure Sampling 208 Method Development Standby Carrier gas at pressure P1 is applied to the inlet of solenoid valve V1 by the PPC module During sample thermostatting the system is in the standby position Carrier gas flows through V1 to the GC column The needle purge flow enters the needle cylinder and vents via V2 See Figure 83 Pressurization At the end of the thermostatting time the needle enters the sample vial Simultaneously the PPC module will now supply pressure P2 The sample vial is pressurized with carrier gas at pressure P2 See Figure 84 P2 is also supplied to the GC In direct connect mode this high pressure flows directly through the GC column In the standard HS connection at the injector the high pr
60. should have all of the equipment ordinarily required for the safety of individuals working with chemicals fire extinguishers first aid equipment safety shower and eyewash fountain spill cleanup equipment etc Due to the explosive nature of hydrogen NEVER use hydrogen gas as a carrier gas in any GC headspace system WARNING Compressed Gases High pressure gas cylinders can be dangerous if mishandled or misused Always handle gas cylinders with caution and observe your local regulations for the safe handling of gas WARNING cylinders Handling Compressed Gas Handle cylinders of compressed gas with care in accordance with local regulations We recommend that gas cylinders be located outside the laboratory and the gases fed to 27 Introduction the laboratory through approved gas supply lines Use only approved tubing connectors and regulators for gas supply lines Cylinders of compressed gas such as the carrier gas and calibration gas must be handled with care Please observe the following handling procedures e Ensure each cylinder is clearly labeled e Do not store cylinders in hazardous locations Store cylinders in an upright position away from possible sources of heat or sparks e Do not heat the cylinders or expose them to direct sunlight The cylinders may rupture at high temperatures e Do not mutilate cylinders e Do not drag or roll cylinders Large cylinders should only be moved
61. stop the run if a vial with such a mechanical problem is spotted Calibrate Decay Time Pressure psi 08 12 1 4 Time min Calibration Vial 6 Time 2 0 Decay Time 2 0 min STANDBY 18 20 25 CJE ese Figure 44 Example of Fast Pressure Decay Curve If the calibration curve is correct and the same vials in content and volume are run then a leak is probably present It could be due to 126 Leak in the vial seal or septum Leak due to needle sealing upper and lower O rings or even the needle itself scratched or dirty or bent Leak at the tee piece and connections between the sampling head and the back in board inlet of the trap Leak at the front end of the Trap PTFE ferrule Decay Flow is increased beyond the regulated value by the Trap Dry Purge Fixed Pr Regulator 50m1 min Leak at the connection of the transfer line or column to the Sampling Head The isolation flow is not correct too low The decay pressure branches to Transfer Line column Isolation flow Operation should be 12 15 ml min The Trap Dry Purge flow is high The Fixed Pressure Regulator is possibly misadjusted or defective and gives higher flow it should be 50 ml min Status Screen Option Tab for the HS 40 110 Trap The Option Tab for the HS 40 110 trap provides some additional options from those just listed with the Headspace only Options tab On the Operating mode menu select Trap In the Option screen for
62. tab Utilizing the options on the Preferences Run tab allow you to simplify the operation of the instrument for routine analysis Preferences Run Config Setup Connect Single Method Operation with preselected method default e _ Multiple Method Operation M disable method editing M HS 40 Emulation Firmware Version 2 11 46 Serial Number M41L294 Instrument Name RCStest OK Cancel Figure 51 Single Method Operation If you select single method operation the options on the Run tab allow you to enter a range of vials to be analyzed and allow you to select a method from a drop down menu These instructions are provided on the Status Run tab 137 Operation Single Method Operation with a Pre selected Method This option allows you to select the method to be used for the selected vial range The Run tab is further simplified to allow the user to enter the vial range only The method you select here displays on the Run tab Enable the option and then select the desired method from the drop down list of pre programmed methods Multiple Method Operation If you have selected multiple method operation users are able to use any of the pre programmed methods to run analyses or create a sequence Multiple Method Operation with Method Editing Disabled You can disable method editing by selecting this option The user can select any of the pre programmed methods to run analyses or create a sequence but the user canno
63. technique a portion of the capillary column is fed through a Teflon tube through which a coolant gas is passed The coolant gas is cooled by passing it through a copper coil immersed in a Dewar vessel containing liquid nitrogen The gas flow is switched on and off by means of a solenoid valve SV6 fitted to the HS This valve is controlled by the HS and the cryofocusing temperature is maintained by switching this valve Refer to the user s manual for the Cryofocusing Accessory P N M041 3578 for detailed instructions on operating the cryofocusing option The cryofocusing temperature can be set to any value between 100 C to 30 C The value to which you set the temperature will be 193 Method Development determined by your application For optimizing the coolant gas temperature for you application refer to Static Headspace Gas Chromatography Theory and Practice by Bruno Kolb and Leslie S Ettre P N N1011210 Timing Tab You can view the timing values for HS operation on the Timing tab Once all the correct timing values have been entered the period from injection to injection PII is automatically calculated by the Headspace Pressurization Time Headspace and HS 40 110 Trap After equilibrium has been reached the vial is pressurized The pressurization time is the duration you want the vial to be in the carrier gas flow Excess gas pressure is vented through the needle purge port When you are using capillary colum
64. the injection before the sample needle is withdrawn from the sample vial or lowered into the vent position During this time the needle remains in the vial The withdrawal time can be set to any value between 0 1 and 99 minutes The default time is 0 2 minutes Pre Post Cryofocusing Time Headspace only These optional parameters appear only if the cryofocusing accessory is installed They define the cryofocusing time before and after sample injection Pre and post cryofocusing time can be used to optimize the cryofocusing duration before and after sample injection The pre cryofocusing duration allows the head of the GC column to cool to the set cryofocusing temperature The post cryofocusing time maintains the head of the column at the low temp until the sample has been collected and unretained compounds have cleared the column These values are determined when optimizing the cryofocusing The total cryofocusing time comprises the pre before and during sample injection and post after injection cryofocusing times Both pre and post cryofocusing time can be set to any value between 0 1 and 99 minutes Relays This dialog box provides access to the timed events for the relays on the options board See Timed Events on page 163 for details on connecting remote accessories and programming the on and off times Period from Injection to Injection PII The HS will calculate the period from injection to injection PII from the timing
65. the HS 40 110 trap you can set the following options Outlet Split If a split is desirable in your analysis you should check this box This setting will instruct the system to keep SV2 in the Needle purge outlet open during the Desorption Injection step This split flow is preset in the factory at 15 ml min and is not accessible to the user Dry Purge If Trap Dry purge is desirable you should check this box Dry purge pressure will be the same as the desorb pressure Internal Standard This field will not appear if this option is not installed in the HS Trap unit If the internal standard is present you can inform the system that an internal standard will be used by checking this box NOTE When using the Trap in the Operating Mode you do not have an option for Inject Mode because you are sampling the entire vapor The Operating Mode has the following choices in the drop down window in addition to the standard headspace modes Trap Standard trap mode using over lapping thermostatting Use the trap for concentrating the analytes before injection into the GC column Trap Clean uses high temperatures to vent the contaminates from the trap Trap Test a dummy injection is made into the GC where the material from the trap using the trap high temp is sent down 127 Operation the column for analysis Run Status Log Inject F Outlet Split Operating Mode SI dropdovm mero F intemal Standard Constant r EVS P
66. the Isolation Flow is shut off thus allowing the trap desorption effluent to be transferred injected into the transfer line and the analytical column The analytical head pressure is now supplied by the PPC module See Figure 122 if you are running split setup See Figure 123 if you are running a splitless setup e Ifthe analytical requirements demand an HS Split operation check the Outlet Split box on the OPTION tab The VENT solenoid valve SV2 is kept open and a Split Flow of approximately 10 ml min is used Needle Purge outlet See Figure 122 e IfHS splitless operation is used SV2 is closed See Figure 123 e Ensure that In the GC the correct method is setup and GC is READY Dry Purge outlet flow is 50 ml min To run a Trap Test 1 2 3 6 On the HS screen select the Option tab In the Option tab select Trap Test On the Status page select the Temp button and set the Trap Temperature to the value you have used for your standard method On the same Status page select the Timing button and set the TRAP HOLD time your typical method time this time can vary from 5 to 45 minutes If you used Split operation check the Outlet Split box Option tab Touch the START to begin the TRAP TEST procedure NOTE If running in sequence mode be sure to start the active method not the sequence the sequence will activate the saved method Monitoring of the GC baseline will show the condition of the Trap
67. the first vial will be loaded up to 12 vials at a time and then vials are loaded as required based on the time established by overlapping thermostatting For more detailed information on allowing access to various Run Modes see the Preferences Tab Section page 35 later in this chapter Creating a Sequence You can use a sequence of methods to analyze a series of vials The options on the Run tab allow you to select a range of vials and then specify a method to analyze the samples You then select the next range of vials and select another method You can also analyze the same range of vials using different methods The sequence can be used on a daily basis or it can be edited as required 106 Operation You will not be able to edit any of these methods if method editing has been disabled from the Tools button Run Status Log vials 31 tol 38 Method dett sf Sequence Sequence Methods Vials STANDBY 14 47 48 Stat Rotate Tools 7 Figure 34 Run Tab Sequence Operation To create a new sequence refer to the Run Configuration in Preferences 1 2 Select the Run tab Press the Start vial entry box and then press the plus or minus button to select the desired start vial Next enter the desired end vial From the method drop down box select the method to be used for the selected range of vials Press the Add button to add the entry to the sequence Repeat these steps until you have c
68. the system to the Column Isolate position and perform system maintenance On completion of the maintenance press the Done button to return the system back to the Standby position Set the zones temperatures Needle Oven Trap to their method values 291 Routine Maintenance 292 Troubleshooting r4 lt gt Troubleshooting Status Messages The following status messages are displayed during normal operation to indicate the current status of the instrument or the current analysis Status Description Messages Initializing The instrument is testing all motors and internal systems at start up Standby The instrument is ready and waiting for an analysis to begin Preparation The HS is moving the first vial to the load position Equilibration The sample vial set points are being met GC Not Ready The HS is ready to inject the sample or load a vial into the oven and has received a not ready signal from the GC Thermostat Time The sample vial is being thermostatted Pressurize Time The sample vial is being pressurized Ext Thermostat GC oven temperature is not ready the cycle time is probably not enough Inject Time The sample is being injected onto the GC column Withdrawal The needle is being retained in the vial after injection Time Vent Time The vial is being vented Analysis Time This is the GC analysis time Finishing
69. there is no reduction or only a very limited reduction in sensitivity This is due to the operating principle of pressure balanced sampling where during injection carrier gas is replaced by sample gas from the pressurized headspace vial The headspace vapors are not diluted by carrier gas during the sample transfer unless additional carrier gas is supplied by the GC pneumatics For split injection a split splitless or programmable split splitless PSS injector must be installed in the GC When performing split sampling the carrier gas pressure P1 is supplied by the HS PPC module to control the pressure Pac in the split injector Headspace Injector gt Split Vent Figure 91 Split Sampling In dual pressure regulated split sampling as seen in Figure 91 catrier gas continuously purges the split splitless injector to avoid back diffusion and sample carryover When operating with PPC control a minimum flow of approximately 2 mL min should be supplied by the GC s injector split pneumatic modules to purge the GC carrier gas lines Keeping this flow smaller than the septum purge flow ensures that no dilution of the injected headspace sample 219 Method Development takes place in the injector A higher flow from the GC pneumatics can be applied to dilute the injected sample if necessary In order to prevent pre injections P1 should be greater than the headspace pressure in the vial at the preselected thermostatting tem
70. thermostatting oven an audible alarm will sound Press the screen to acknowledge the alarm Enter a value of 0 to disable the vial alarm option Vent Time Headspace only The vial venting time is the length of time during which the vial is vented to atmosphere If you enable this option venting occurs immediately after the withdrawal time The default venting time should be 0 3 minutes 18 seconds If the compounds contained in the vials are hazardous this option should be disabled and the vials should be vented into a fume hood or other well ventilated area to avoid exposure to hazardous vapors Sample vials just unloaded from the thermostatted oven into the magazine can be very hot and may still be under pressure Cool and vent the sample vials before you open or dispose of them WARNING 143 Operation Economy Mode Economy mode allows the instrument to remain on while conserving power and carrier gas To use economy mode you must enable the option and then enter the desired settings When the instrument goes into economy all of the heaters are switched off the needle purge valve SV2 is closed and the touch screen display dims Any key press interrupts the Economy Mode and the instrument returns to Standby A visual note and an acoustic effect accompany the activation of economy mode To enable and use this option 1 Open the Setup tab 2 Press the Economy Mode check box A check mark will appear in th
71. time is the time that it takes the analytes to be released from the trap into the transfer line 121 Operation Trap Hold This option allows you to input the number of minutes that the trap will maintain the maximum temperature In order to release the analytes from the trap the maximum temperature must be maintained for a sufficient amount of time A recommended trap hold time is five minutes In addition this will help clean up the trap to prepare for the next sample Setup By touching the Setup button the HS Trap Timing screen will appear This allows you to set the HS Trap Timing based on the cycles pressure and decay time Run Status Log gt Dy Purge Trap Hold 05 05 rap Timing x Cycles Pressurize 1 0 min Decay Time 2 0 min Calibrate Decay Time i OK JTemp Timing Option Jepe STANDBY Oct15 _ Stat Rotate Tools y Figure 41 HS 40 110 Trap Setup Screen The Timing screen has the following variables Cycles you can set the cycle number from 1 to 4 This number represents the number of times that the vial pressurization and trap load cycles will be performed per vial For example should you select 4 cycles and a vial pressure of 40 psi More than 99 of the material will be adsorbed and focused in the HS 40 110 trap Pressurization A fter equilibrium has been reached the vial is pressurized by the carrier gas to a pressure equal to the Vial pressure See P
72. to edit a method but do not want to affect your sequence then save the revised method with a different name You use up to 8 methods in your sequence If you need to use more than 8 methods you must use the PC control software NOTE You will not be able to edit any of the selected methods if method editing has been disabled from the Tools button 7 Press the green Start button to run the sequence The HS will configure itself based on the method parameters The instrument status will be Not Ready until the instrument reaches all of the set points at which time it will become Ready When the GC and the data handling system are ready a vial will be loaded into the oven The vial will be thermostatted and the analyses will continue as determined by the method 154 Operation If you are using the an HS 40 or HS 110 with the 15 vial oven the first vial will be loaded and then vials are loaded as required based on the time established by overlapping thermostatting Editing a Sequence To delete an entry from the sequence select the entry in the list and press the Delete button To change the vial range you must add a new entry with the revised vial range and then delete the old entry If you edit the methods called by your sequence the sequence will use the revised methods If you need to edit a method but do not want to affect your sequence then save the revised method with a different name Logic Flow Diagram A Descript
73. to the Start Normally Open Pin 5 4 Connect one of the black wires to the Ground Pin 12 Connect the red wire to the Ready In Pin 9 6 Connect the remaining black wire to the Start Normally Open Pin 6 14 13 D aa a Se Fe 12 Black 9 Pin Connector snell 11 x Red 4 99K 8 2N5088 7 1N4148 6 e Black 5 White 4o f Connector DBI 3 2 Pin 1 TurboMatrix I O Port Figure 6 Schematic of the HP Sampler Cable Installing the Heated Transfer Line Installing the heated transfer line is an important procedure for the GC The headspace version and the HS 40 110 trap have different requirements for this procedure NOTE For the headspace setup the best and most typical configuration is Installing the Heated Transfer Line at the GC Injector for Split Operation For the headspace only configuration split the heated transfer line connects the sampling head to the GC The sample moves through 58 Installation the sample line from the vial to the GC column Normally at the GC end you will connect the fused silica tubing to the injector If your GC injector supports it it is best to split the sample The carrier gas is supplied and controlled by both the Headspace and GC See the procedure Installing the Heated Transfer Line at the GC Injector for Split Operation later in this chapter NOTE For optimum pe
74. values that you have entered The PII value is shown on the Timing tab For optimum sample throughput i e the greatest number of samples analyzed in the shortest time it is essential that the PII value is only slightly longer than the cycle time The PII value lets you see the effects of your analysis timing changes on vial throughput 114 Operation If you are running the 15 vial oven it is possible to overlap the thermostatting times and reduce the PII The Status Tab Option Tab Headspace The Option tab provides access to the headspace method options Select the options that you have installed If you have an option installed but do not need to use it then de select here You can enable vial venting the shaker cryofocusing and high pressure injection from this tab High pressure injection is only available if you have the PPC option installed The cryofocusing option will only be available if the option has been installed on the HS and in the GC column oven Run Status Log I Hi Psi Inject Inject Mode Operating Mode 5 Constant E Volume E TestL_Env5_2 CIJ Jemp Timing Option JppeE STANDBY him uth Stat Rotate Tools w Figure 37 Option Tab You will also select the operating mode and the injection mode from this tab Injection Mode The volume of the injected sample can be entered as an injection Time or an injection Volume The injection volume 115 Operation mL is based on you
75. which can be measured using a flow meter The latter flow is comprised of the HS transfer line flow the flow from the GC PPC module Column flow Action Action Turn off the split leak Press SYSTEM from the GC keyboard then keep pressing ENTER until it shows SPLIT FLOW OFFSET 1 FIXED On the Clarus GC touchscreen select Tools gt Configuration gt Injector icon and adjust the offset value to 1 00 Install the zero dilution interface at the GC injector See Installing the Zero Dilution Liner in the Accessories chapter This liner allows you to purge the injector with GC carrier gas without diluting the HS sample entering through the transfer line this liner also eliminates peak tailing HS 40 110 Trap Only Troubleshooting Cause Excessive carryover Action 320 Perform a trap clean procedure refer to the Clean the Trap in the Routine Maintenance chapter You might need to clean the trap a few times to lower the excess carryover Troubleshooting Action The HS 40 110 trap is designed for low level volatile analysis therefore if you cannot resolve the excess carryover you may need to use a smaller sample size lower concentration Cause Blank sample contamination Action Bake out the system at elevated temperatures Make sure you are using PerkinElmer cleaned vials and PTFE Silicone septa If the analysis requires extreme low levels the vials and caps should be baked out overnight at 120 C
76. with FID very low permeability Pack of 100 Seals B0104243 Pack of 1000 Seals B0104244 Pack of 1000 Seals pre assembled ready to use B4000022 PTFE Coated Silicone Septa for temperatures up to maximum of 190 C weak interference peaks with FID very low permeability Pack of 100 Seals B0104241 Pack of 1000 Seals B0104242 Pack of 1000 Seals pre assembled ready to use B4000028 Table 23 Sample Vials and Seals 337 Appendices Tools for Sample Preparation Description Part Number Hand Crimper N9302785 Cap Removing Tool N9301270 Benchtop Crimper N6621006 Vial Gauge B0151737 Pressure gauge with needle for vials B0501377 Gauge for checking 22 mL vial dimensions B0151737 Table 24 Tools for Sample Preparation Replacement Parts Description Part Number Fuse 5 x 20MM 10 A 250V TC M0417002 Fuse 5 x 20MM 5 A 250V TC M0417038 Jet needle stainless steel 3 grooves B0510363 Jet needle Siltek platinum iridium 3 grooves B0510364 HS Needle Seal Assembly without O Rings B0500833 O Rings for Needle Seal Assembly Pack of 10 B0198110 Deactivated fused silica transfer capillary 5 m i d 0 25 mm N9301356 Deactivated fused silica transfer capillary 2 5 m W 0 32 B0698537 mm Extended transfer line 1650 mm heated M0413532 Transfer Line heated M0413531 Headspace Starter Kit see the following table B0505601
77. 10 is removable You can maintain multiple magazines so that while one is in use you can be 269 Routine Maintenance loading the other The magazine on the HS 16 cannot be removed by the user To remove and replace the magazine 1 Turn the HS off 2 With one hand holding the magazine loosen the magazine cap nut by turning it counter clockwise 3 Remove the cap nut and then lift off the magazine 4 Place the new magazine on the instrument and replace the magazine cap 5 Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized correctly NOTE You can clean the magazine using warm soap and water Do not immerse the magazine in water simply use a damp cloth and wipe plastic Do not use organic solvents to clean the magazine as you will damage the plastic Cleaning the Magazine If dirt is allowed to build up on the magazine the sample vials may stick and will not be loaded correctly To prevent a build up of contamination on the magazine only load clean sample vials Never use adhesive tape or any other type of adhesive materials on the vials The magazine should be cleaned every six months or more frequently if build up is obvious With the HS disconnected from line power clean each well of the magazine with a weak soap solution or suitable solvent using a cotton swab Rinse with clean water using a fresh cotton swab and allow the ma
78. 11 192 Transfer Line 111 191 Test Command 135 Cryo 135 Leak 135 Sample Injection System 86 Thermostat Time 295 Thermostatting Constant Mode 212 Effect on Vial Pressure 195 MHE Mode 117 213 Mode 212 Optimizing Time 196 215 Overlapping 196 Phase 186 Pressurization when Using Overlapping 222 Progressive 214 Progressive Mode 116 Temperature 111 192 Time 112 115 196 Threshhold Limit Values TLV 29 Time Cryofocusing 114 204 GC Cycle 113 Injection 113 Pre PostCryofocusing 114 Index 204 Pre Cryofocusing 205 Pressurization 112 122 Setting 147 Thermostatting 112 115 196 Withdrawal 114 198 Timed Event Programming 163 Relays 54 Timing Analysis 112 Cryofocusing 173 Method Parameters 112 Options 112 Post Cryofocusing 173 Pre Cryofocusing 173 Tab 194 TLV 29 Tool Adapter Sleeve 248 Method Editor 133 Needle Seal Removal 248 250 O Ring 252 Spigot Key 250 Tools Button 133 Calculator 135 Menu 205 Reset 136 Touch Screen Brightness 146 Display 103 Language Options 146 Options Tab 115 Run Tab 104 Status Tab 108 Transfer Line Adapter for GC Injection Port gyl Contaminated 313 Direct Connection 71 355 Index Installation 58 Installation at GC 68 Installation at Needle Unit 62 65 Installing Collar 275 On Column Connection 72 Temperature 111 191 Trap Conditioning 282 Maintenance 282 status tab 128 Trap Accessories 182 Trap Connections 79 Trap Installtion 81 Trap Maint
79. 2 mm of the sleeve nut and then tighten the mounting screws on the collar Figure 14 Installation of Transfer Line at the Needle Unit 67 Installation 15 Pull the sliding insulation tube from the transfer line all the way down so that it touches the needle unit in order to protect the fused silica tube connections and to keep the area heated 16 Plug the electrical connector into the receptacle above the retaining collar The connector is polarized so that it will only fit one way Do not force the connection Installing the Heated Transfer Line at the GC Injector for Split Operation TurboMatrix Headspace Only Once the transfer line has been connected to the HS and the connections have been leak tested you can then connect the transfer line to the GC An AutoSystem XL or Clarus 500 GC adapter is supplied with your instrument If you have another type of GC contact your PerkinElmer service engineer The threads on the adapter are sharp and can cause cuts to your fingers or hand Use the proper protection a paper towel or gloves before tightening the adapter WARNING f j g Liner Recommendations We recommend using certain liners when installing different injectors on an Autosystem XL or Clarus 500 GC Packed Injector Standard Liner No Packing Capillary Injector 2 mm or 4 mm Liner No Packing PSS Injector 2 mm or 1 mm Liner No Packing To install the heated transfer line at the GC
80. 40 110 Trap 121 Gas Leaks Detected by Monitor Vial Integrity Dynamic leak Testsscciystse ssk cosets eseese 123 Status Screen PPC Tab for the HS 40 110 Trap 128 ThE tos Tab prere eteteari a EEE aN areas 129 IROTO E AEE E E E T 133 Method Editt erareto eieiei 133 TESE NEEE E EOE E N T 135 Log Out Headspace and HS 40 110 Trap 135 Calculator srann tones oee dEr E EEA 135 Resetre g eana aE ERT 136 Preferences Tab Headspace and HS 40 110 Trap 136 Run Fabes na e i ee 137 Contig TaD csi ls sceesisscsestesubestelaasstalecat oea Ei 138 Setup Tabi was Anke A EEE ar aa 141 HS 40 110 Trap Setup Tab 145 Connect Tab eisene e an 145 Starting a Run TurboMatrix Headspace and HS 40 110 IRET D A E Gia ei Han sehen 147 Preparing Samples eseseeeeeeeeeeereseesreerreresrrsrees 147 Loading the Magazine ee eeeeseeseceseeereeenees 148 Single Method Operation on the HS 149 Multiple Method Sequence Operation 150 Using the Tray Rotation Feature While Running A Vial SEQu enCes v eswsienea reeset aie rel aes 151 Creating a Sequence eee ereerreresessre 153 Editing a Sequence eee eeeceseceeeeeeeeneeeneeeeeeees 155 Logic Flow Diagram A Description HS 40 110 Trap Only ceesseeseceneceeeeeeeenaees 155 High Pressure Sampling Headspace Only 159 HS AO LOT Pap cssccttstesssscessteteetace larsoladoserbetevanteds 160 Shutdown Headspace and HS 40 110 Trap 160 PECOSSONES siisec ci c
81. 45 psi See Carrier Gas section earlier in this chapter 6 Open the Tools drop down menu and select Maintenance and then select Leak Test If the leak test fails you will get the following screen Go to step 8 for the procedure of a failed leak test 90 Installation Run Status Log Trap Hold Dry Purge Initial Final Pressure Pressure psi psi Tests Gas Leak 33 16 STANDBY 10 33 35 Stat Rotate Tools x Figure 29 Failed Test Red Text If the leak test passes you will get the following screen Run Status Log 9 Column a 35 0 psi Leak Test Result Tests Initial Final Pressure Pressure psi psi GasLeak 34 94 STANDBY 09 55 42 Stat Rotate Tools x Figure 30 Passed Test Black Text Installation 7 The HS sampling system is now a closed pressurized system The pressure displayed on the PPC tab must not drop by more than 1 psi over a period of 40 seconds 8 Ifa leak is detected check all of the connections with a helium Leak Hunter or concentrated ethanol and water solution 50 ethanol and 50 water solution Once you have checked and no leaks are detected then run the leak test again See the next page for more leak check details 9 Reduce the carrier pressure to the pressure specific to the method 10 Because of the sensitivity of the HS trap make sure to trim the column w
82. 7 Show Option 138 Shutdown 160 Signal BCD 53 Fail 51 Input 53 Output 51 Ready In 53 Ready Out 51 Start Inject 51 Start In 54 Stop In 54 Silicone Septa 179 PTFE Coated 180 Single Method Operation 105 137 149 Software HS Control 180 Specifications Carrier Gas 46 Power 44 Purge Gas 48 Spigot Key 250 Split Flow Calculating 222 Description 221 Total 223 Split Injector Zero Dilution 168 Split Sampling 218 AutoSystem XL with PPC 222 Setting Carrier Gas Pressure 100 Splitless Sampling 223 Connections 71 Direct Connection 101 224 Disadvantages 223 On Column Connection 102 224 354 Setting Carrier Gas Pressure 101 Splitting Broadening of Peaks 309 Stamper Assembly 272 Standby 295 Star Spring 177 Start Inject Signal 51 In Signal 54 Starting Analysis 149 Run 149 Sequence 150 the Headspace Sampler 98 Status Messages 295 327 Oven 130 132 Tab 108 Status Tab PPC Tab for the HS 40 110 Trap 128 Temp Tab for the HS 40 110 Trap 119 Stop In Signal 54 Storing Compressed Gas Cylinders 28 Instrument 40 Supplies 97 AC Line Voltage 45 Vials and Seals 337 Surge Electrical 45 System Unrecoverable Error 297 327 T Tab Config 138 Connection 145 Log 129 Options 115 206 Preferences 136 Run 104 Setup 141 Status 108 Temperature Actual Value 109 Analysis 109 Extreme 29 Laboratory 40 Method Parameters 109 Mode 111 191 Needle 110 191 Options 109 Set Points 109 Thermostatting 1
83. AC power supply See Electrical Connections later in this chapter When the instrument arrives 6 Check the instrument and any other equipment for any visible signs of damage If you find that something is damaged file a claim with the authorized carrier immediately and inform your nearest PerkinElmer office 7 Ensure that all ordered accessories have been delivered Some accessories such as the PPC and the vial shaker will be installed at the factory 8 Check that nothing is missing a list of the equipment delivered is provided in Table If you find that 38 10 11 12 13 14 Installation something is missing inform your PerkinElmer representative Contact your local PerkinElmer office to arrange for the installation The service engineer will go over the pre installation checklist to ensure all required pneumatic and electrical requirements have been met A PerkinElmer service engineer will install the instrument and put it into operation for the first time All packing materials should be retained at the time of installation to ensure that nothing is mistakenly discarded The customer should then retain the packing material for recycling storage or further shipment Ensure that you have an adequate supply of sample vials septa and caps You will also need a crimper to seal the vials and a decapper to empty the vials If you have a GC other than an AutoSystem XL or a Clarus 400 500 or 600 ens
84. NOTE If you set the needle transfer line or thermostatting temperature to a value below room temperature the whole instrument must be cooled i e in an environmental chamber to a temperature 5 C below the thermostatting temperature This is outside the operational specifications of the HS 192 Method Development HS 40 110 Trap Temperatures The speed of Trap temperature rise and the maximum allowable Trap temperature can be selected and set on the Trap Setup Tools gt Preferences gt Config tab gt Trap Setup You can choose either Fast or Slow Heat Rate from the drop down list The default Trap Maximum Temperature is 400 C It depends upon the Trap material Unauthorized changes to higher values should be avoided CAUTION Follow the manufacturers recommendations for the upper trap temperature If the temperature is set too high the trap and instrument could be severely damaged Cryofocusing Temperature Headspace Only Cryofocusing or cold trapping is the technique of sample concentration through the application of low temperature The injected analytes are pre concentrated on the capillary column The sample is cooled at the column inlet the volatile components in the headspace are separated from the unretained gases and concentrated If the cryofocusing accessory M041 3411 is installed and enabled the cryofocusing temperature options will be displayed on the Temperature tab In the cryofocusing
85. PC You select the desired view by selecting the corresponding radio button on the lower half of the touch screen See the following figure You can view the actual settings as they are on the HS or you can view the set points When you are viewing the set points the parameters are displayed in black When you are viewing the actual values the parameters are highlighted in yellow and displayed in red until they have come into control The name of the method that is currently loaded on the Run tab is also displayed You can change the settings and then save the revised method Normally you will use the status display to monitor the instrument You can also use the status tab to create a method By using the status tab rather than the method editor you can enter parameters run an analysis change the settings based on the results and then perform another analysis You can proceed in this manner until you have obtained the desired method parameters Once the method is complete you can save it and use it on the Run tab NOTE Additional Headspace trap features in the HS 40 110 Trap 108 Operation section beginning on page 114 Temperature Screen Headspace and HS 40 110 Trap There are three standard temperature settings for the HS The needle temperature the transfer line temperature and the HS oven thermostatting temperature If you have the cryofocusing accessory installed you will also set the cryofocusing temperature from this
86. PC tab You can set the pressurization time to any value between 0 1 and 999 minutes The default value is 1 minute 122 Operation Decay tThe time for the complete headspace vapor to be decayed out of the vial on to the trap To calibrate the decay time press the Calibrate Decay Time button to bring up the calibration screen Calibrate Decay Time 30 0 Pressure psi 0 0 0 O04 O08 12 16 2 Time min Calibration Vial Time 0 0 Decay Time 0 1 min STANDBY 11 4514 Star SS Close Figure 42 HS 40 110 Trap Calibrate Decay Time Screen Place a vial of a typical sample in position 1 The HS 40 110 trap will thermostat your calibration vial for two minutes then pressurize it to the vial pressure in the method The calibration vial needs to have the same volume and composition as the samples This will determine the decay time and this decay time can be entered in the decay time position NOTE Later you will be able to determine if you had a vial that was not sealed properly or was under filled or over filled Gas Leaks Detected by Monitor Vial Integrity Dynamic 123 Operation Leak Test Gas leaks can also be detected by the option Monitor Vial Integrity see the Preferences section later in this section Here it is fundamental that the Decay curve produced by the Calibrate Decay Time procedure gives a good decay profile See in earlier chapter the Calibrate Decay Time description and notes
87. Practice New York Wylie VCH Inc 1997 343 Appendices 344 Index A AC Line Connections 45 Accessory Cryofocusing 172 High Pressure 159 Options Board 163 PPC 167 Vial Shaker 166 Water Trap 174 Zero Dilution Liner 168 Activate Method 134 Adapter GC Injector 68 71 Sleeve 248 Sleeve Tool 248 Transfer Line 71 Adjusting Crimp Plunger 272 Hand Crimper 271 Stop Pin 271 Adsorption Trap Water for Cryofocusing 174 Air Extra Dry 48 Alarm Maintenance 138 Altitude Laboratory 40 Aluminum Coated Septa 179 Analysis Headspace Description 185 Starting 149 Analysis Time 295 Appendix Customer Service 335 Reference Material 341 Replacement Parts 337 Warranty Exclusions and Limitations 336 Assembly Lower Needle Seal 249 Safety Closure 177 Upper Needle Seal 247 Automated Leak Test 261 AutoSystem XL Connecting HS 55 Injector Adapter 68 PPC and Split Sampling 222 Auxiliary RS 232 Port 146 B Baud Rate 146 BCD Data Logic 166 Signals 53 Binary Coded Decimal Interface 165 Broadening Splitting of Peaks 309 Butyl Rubber Septa 179 PTFE Coated 179 C Cable HP6890 Ready Start 57 Ready Start 55 Calculator 135 Cap Transfer Line 275 Capillary Column Headspace Sampling with Wide Bore 226 Carbon Disulphide 26 Carrier Gas Cleanliness 237 Connection 76 Contaminated 312 Delivery Pressure 76 In Port 78 Lines 46 Pressure Fault 297 345 Index Purity 46 Selecting Type 138 Setting Pressure 100 Specifica
88. RNING Using sample vials caps and septa other than those supplied by PerkinElmer can result in damage to the instrument and or injury if you attempt to remove the broken glass vials Avoid storing vials that contain a sample in places where there are high levels of organic vapors such as refrigerators car trunks and airline storage hangars Store caps and septa in a clean environment preferably a clean heated desiccator when they are not being used You may want to heat new septa to 100 C for 2 to 3 hours before putting them into use Important Carrier Gas Shut Off There are cases where you are instructed to switch off the carrier gas supply to the headspace However in certain cases as in HS 40 110 trap the carrier gas should not be shut off as the Isolation Flow that protects the analytical column will be stopped and you will starve your transfer line and detector of helium 238 Routine Maintenance Under normal circumstances you can do all your maintenance and troubleshooting with the carrier gas on However in some cases you may be required to do maintenance that requires a complete shutdown of the carrier gas to prevent oxidation You should not attempt maintenance in the Headspace or HS 40 110 trap unit unless you have ensured the following in the GC 1 Ifthe detector is a flame one FID NPD etc the flame should be off 2 If the detector is an MS the transfer line and ion source if pres
89. S Hydrocarbon Moisture Oxygen Charcoal Filter Filter Filter Filter Gas Cylinder Figure 19 Connecting Filters to the Gas Supply System Ensure that gas lines containing filters are protected from excessive pressure WARNING To connect carrier gas to your HS 1 Locate the carrier gas tanks in a secure location See the section on Compressed Gases earlier in this chapter 2 Connect a clean high purity two stage regulator to the carrier gas tank The regulator should also have a 1 8 parallel compression fitting with which to connect the regulator to the HS The delivery pressure must be adjustable to 90 psig 620 kPa NOTE The regulator must be absolutely clean and free from any oil or other contamination 3 Connect any filters that are required as close as possible to the HS 76 Installation 4 Connect the regulator to the HS Carrier In port Use copper or stainless steel tubing only Securely tighten all fittings 5 Open the tank and set the delivery pressure to 90 psig 620 kPa The carrier gas delivery pressure must not exceed 100 psig 690 kPa and it must be sufficient to maintain the required column head pressure at the gas chromatograph Do not set the delivery pressure higher than 100 psig 690 kPa WARNING Dry Air If you are running an HS 110 or HS Trap with an internal standard accessory you will also require a supply of dry air Th
90. Temperature 60 C Needle Temperature 65 C Transfer Line 110 C Temperature GC Cycle Time 3 min Injections per Vial 1 Thermostatting Time 22 0 min Pressurization Time 3 0 min Injection Time 0 04 min Withdrawal Time 0 5 min Table 12 Capillary Column Parameters 240 Routine Maintenance Changing the Fuse The fuses should normally not need to be changed A blown fuse may indicate a more serious problem and you should contact your PerkinElmer service engineer unless you can identify a cause external to the instrument incorrect line voltage power surge lightning etc The operating voltage of the instrument is set at the factory Only a PerkinElmer service engineer or similarly qualified person is authorized to change it if required Before changing the fuse s observe the following precautions WARNING To prevent potential injury to yourself and damage to the instrument switch off all instruments in the system and disconnect them from the line power supply before you change any fuses To replace fuses 1 Ensure that the power cord is disconnected from the power entry module on the rear left side of the instrument The fuse drawer is located in the top portion of this module Refer to Figure 95 Carefully pry the fuse door open with a flathead screwdriver Use the flathead screwdriver to slide out the fuse drawer Remove the blown fuse and replace it with a new one of the correct typ
91. TurboMatrix Headspace Sampler and HS 40 110 Trap User s Guide Release History M0413401 F February 2008 User Assistance PerkinElmer Inc 710 Bridgeport Avenue Shelton CT 06484 4794 email info perkinelmer com Notices The information contained in this document is subject to change without notice PerkinElmer makes no warranty of any kind with regard to the material including but not limited to the implied warranties of merchantability and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of PerkinElmer Inc Copyright 2008 PerkinElmer Inc Produced in the UK Trademarks Registered names trademarks etc used in this document even when not specifically marked as such are protected by law PerkinElmer is a registered trademark and TurboMatrix and PPC are trademarks of PerkinElmer Inc HP is a registered trademark of Hewlett Packard Corporation Swagelok is a registered trademark of the Crawford Fitting Company Teflon Tefzel Viton and Vespel are registered trade
92. Withdrawal Time Headspace Only This is the length of time after the injection before the sample needle is withdrawn from the sample vial or lowered into the vent position During this time the needle remains in the vial You can set this value to 0 0 to 9 9 min in steps of 0 1 min 10 to 99 min in steps of 1 min When you are using the high pressure sampling option you must set the withdrawal time correctly to avoid double injections See Setting the Withdrawal Time for High Pressure Sampling earlier in this chapter Setup HS 40 110 Trap Only Decay Time After vial pressurization the next step is to use the pressure in the vial in order to load the trap with the largest possible part of the headspace vapor a reverse flow Consequently this step should last until the pressure in the vial has decayed to its lowest value The Decay time to be set in the method appears in the Trap Timing screen as shown below 198 Method Development Run Status Log DryPurge Trap Hold i o5 0 5 Pressurize min Decay Time min A a ee Temp Timing _ Option STANDBY Oct 15 SBA Aotate Rotate E Tools Figure 76 This value is decided after the Calibrate Decay Time procedure is chosen in the Trap Timing screen above Pressure psi a ee oe Time min Calibration Vial i Time 0 0 Decay Time 0 1 min STANDBY LEARNA Stat E Cose Figure 77 199 Method Development The ab
93. a R R k Transfer Line A Transfer Line p p a e e gt gt ca Y R p aa Figure 70 Thermostatting Figure 71 Pressurization Phase Phase 186 Method Development Injection or Trap Load Phase After the pressurization phase the solenoid valves V1 and V2 are closed stopping the carrier gas flow The compressed gas in the vial flows onto the column or trap After the pre selected injection time the solenoid valves V1 and V2 are again opened completing the sampling phase The carrier gas now flows directly onto the column and branches to the sample vial preventing additional sample vapor reaching the column dl V Transfer Line I Figure 72 Injection Phase HS 40 110 Trap Sampling Technique NOTE The previous three illustrations show a generalized flow and do not represent the exact plumbing for the HS 40 110 trap This sampling technique incorporates some additional steps to the HS Sampling Technique The HS 40 110 trap Sampling technique and the HS Sampling Technique share the Thermostatting Pressurization and Injection or Trap Load phases see the explanation of these phases on the previous page Unique to the HS 40 110 trap are the Pressure Decay phase the Dry Purge phase and Desorb split splitless phase Pressure Decay Phase This phase allows for the pressure inside the vial to decay into the HS 40 110 trap The column isolation flow preven
94. action steps follows the mathematical relationship of a first order reaction That is the decreasing concentration over time is proportional to the prevailing concentration 229 Method Development dC kC Equation 4 dt where t is time C is concentration and k is a constant Since the concentration at any time C depends on the initial concentration Co and the exponent k the equation becomes C C e Equation 5 Since the extractions are performed in steps the time t may be replaced by the number of extraction steps n The initial concentration CO is replaced by the peak area from the first extraction step Al which occurs at time t 0 or n 1 The constant k which now includes instrument parameters becomes k A A e e Equation 6 This can be expressed in the form of a linear equation InA k n 1 InA Equation 7 A simple regression analysis provides a straight line plotted through the values of the peak areas derived from three or four extraction steps This line gives the values for the slope k and y intercept Ao The total peak area of the volatile compound in the sample is then determined by summing the partial peak areas from each extraction step Using Equation 7 as a geometric progression the total area An becomes vA A Ite t e e Equation 8 Written in a more general form the equation for the sum of the areas is 230 Method Development DA j k Equation 9 Applying th
95. ak and then press MHE again Enter as many runs as you have performed and press the button after the last button to calculate the total concentration Reset Use the Reset command to reset the instrument This may be because of a fatal error or software problem If the instrument is reset you must load your last active method and allow the HS to reach all of its set points before beginning an analysis If you reset the HS during a sequence adjust the start and stop vials so that the sequence includes only the vials that have not been analyzed NOTE When you begin the new sequence the log information from the previous sequence is lost Preferences Tab Headspace and HS 40 110 Trap You use the Preference tab to set the configuration options for the HS The selections you make here enable or disable various options on the Status screen and in the Method Editor The Preferences screen contains four tabs related to the operation of the HS e Run tab e Config tab e Set Up tab 136 Operation e Connect tab The Run tab sets the options for the running samples The Config tab contains information on the type of carrier gas pressure units various calibrations trap setup etc The Setup tab displays various HS options information The Connect tab contains access to the communication parameters required for RS 232 connections and the Date Time button Run Tab The Preferences Run tab configures the options on the Status Run
96. ak the fused silica column if necessary to remove the ferrules Feed the column up through the injector until it clears the top of the injector Place the septum into the adapter Carefully push the fused silica column through the adapter from the bottom side piercing the septum 10 11 12 13 14 15 Installation Loosen the threaded collar from the stainless steel adapter and using the threads on the adapter as a handle screw the adapter into the injector port Insert the capillary from the GC end into the transfer line until approximately 5 cm of the line extends from the HS end of the transfer line Slide a 1 16 sleeve nut and graphite ferrule onto the end of the fused silica column between the transfer line and the deactivated tube adapter Score and break the fused silica column to remove any graphite residue which may block the carrier gas flow Push the fused silica column into the deactivated tube until it reaches the needle Slide the ferrule and nut into position and hand tighten Mark the position on the fused silica at the end of the nut For the TurboMatrix Headspace withdraw the fused silica column 1 to 1 5 cm back from the needle and tighten the nut For the HS 40 110 trap do not withdraw the column at all See Figure 13 Plug the other end of the column and leak test the system before you finish assembling the transfer line See Leak Testing later in this chapter for details o
97. alyzed directly by headspace gas chromatography since it is not possible to prepare reference solutions This function is used for method development and validation as well as for quantitative analysis of difficult solid samples NOTE Does not work with compounds with a high concentration of Potassium In MHE mode the headspace gas in the sample vial is extracted and analyzed successively with pressurization of the sample vial between each extraction and automatic venting between extractions Up to nine extractions can be taken with the HS During venting a portion of the headspace vapor escapes As each successive extraction and analysis is run the peak areas of the constituents decrease If the extraction is run to exhaustion it is only necessary to sum the peak areas of the analyte to determine its concentration in the sample In practice it is not necessary to run the extraction to exhaustion After a minimum of two extraction steps the sum of the peak areas can be calculated from the geometric progression 213 Method Development 7 7 7 I IE ES i i Extraction 1 Extraction 2 Extraction 3 Figure 89 MHE Mode Progressive Mode This function is used for initial method development to determine the thermostatting time required for a specific application The function can also be used for kinetic studies Vial position one must be filled For every vial positi
98. ample vial The HS40 110 Trap allows multiple headspace vapor loading steps into the cold trap in order to remove from vial most of the headspace and so achieve a pre concentration of the compounds of interest up to 100 times lower detection limits An optional step after the last trap loading allows a cold dry purge of the trap to remove moisture and or very volatile components Last comes the desorption step of the pre concentrated sample in the trap by a fast increasing of the trap temperature and a simultaneous reverse carrier gas flow through the trap in order to inject the sample to the transfer line and the following GC analytical column Throughout all of the preparative steps before desorption injection the transfer line and analytical column remain pneumatically isolated constantly supplied with carrier gas through a pressure balance system Isolation Flow In addition TRAP CLEAN and TRAP TEST modes of operation offer trap cleaning as well as a trap cleaning quality test Built in systems reveal possible sample leaks and or not equal sample volumes and provide accurate calculation of the vial thermostatting temperature The Trap system is also supported by the Internal Standard option that allows the addition to the sample of selected gaseous internal standard components Another feature of the HS 40 110 trap is column isolation This ensures GC MS stability with the carrier gas flow into the GC being maintained d
99. ands NOTE Do not use sharp objects such as pens and pencils to activate the touch screen as you may damage the display Using the three screen tabs you can control the operation of the HS The touch screen interface allows you to communicate directly with the HS so that you can e set and view current configuration parameters Status tab e run analyses using one or more methods Run tab e view instrument information Log tab With the PPC option installed you can control all of HS functions directly from the touch screen You can then monitor the carrier pressure from the touch screen If PPC is not installed you must use the pressure regulator to set the carrier pressure The interface consists of three tabs The Status tab provides information on the current HS settings You can also make changes to the HS parameters directly from the status screen Changes you make on the Status tab will take effect immediately unless an analysis is in progress Editing parameters will be disabled until the analysis is complete You can use the Status tab to create and test new methods Alternately you can save or recall the methods using 103 Operation the Tools button on the Run page and selecting the Method editor option The Run tab allows you to create a sequence of methods to be used on a series of samples You create a sequence by selecting a range of vials and then specifying a method by which these vials will be analyzed The
100. ange on the Run tab to exclude the vials that have already been run and press the Start button to continue your analyses Cause A mechanical problem has occurred Action Contact your PerkinElmer service engineer Fault Elevator Motor Stalled Cause An obstruction has caused the elevator to halt Action Turn the HS off and disconnect the power cord from the AC mains Remove the obstruction and reconnect the line cord Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized correctly You must update the vial range on the Run tab to exclude the vials that have already been run and press the Start button to continue your analyses Cause A mechanical problem has occurred Action Contact your PerkinElmer service engineer Fault Oven Motor Stalled Cause An obstruction has caused the oven to halt rotation Action Turn the HS off and disconnect the power cord from the AC mains Remove the obstruction and reconnect the line cord Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized correctly You must update the vial range on the Run tab to exclude the vials that have already been run and press the 298 Troubleshooting Start button to continue your analyses Cause A mechanical problem has occurred Action Contact your PerkinElmer service engineer Fault Needle Mot
101. are set in the method Desorb Pressure and Desorb Time This desorb pressure will create a reverse carrier gas flow through the trap from back to front via an appropriate switching of the solenoid valves SV1 and SV9 GC analysis program starts at this step After the initial short Desorb time the system switches the PPC module to the appropriate column pressure that sweeps the desorbed analytes out of the trap and into the transfer line and the column for the GC analysis The column pressure value is set in the HS Trap method Trap Hold This keeps the trap at the desorption temperature for the Trap Hold time that we have set in the method At the end of this time the system interrupts the heating of the trap and starts cooling it with a fan back to the low trap temperature set in the method default 40 C Simultaneous with the Trap Desorption the system checks whether this is the last vial in the method If yes it terminates the HS Trap operation and goes to standby If not it moves to the next vial which it loads into the thermostatting oven to start its preparation The term PIT Algorithm Period from Injection to Injection algorithm that appears in the flow diagram denotes a software that enables the HS to calculate the period from injection to injection from the timing values that are entered in the method and the GC cycle time The PII value is shown on the Timing tab of the HS screen For optimum sample throughput i
102. arts have been received undamaged see Tables 1 and 2 16 Introduction The following items should be included with your HS instrument Part No Description Qty 00090652 Septum Kit Fairprene 50 Pkg 1 09903157 Nut 1 16 1 L1003026 Graphite Vespel Ferrule 1 6 mm ID 3 04966624 Wrench Open End 1 04972433 Graphite Ferrule 0 5 mm ID 3 B0131410 Tool O Ring Assembly 1 B0147449 O Ring Extractor Tool 1 B0151737 Vial Gauge 1 B0500843 Spigot Key 1 B0503956 Glass Lined Tube Adapter 1 B0505266 HS Injector Adapter 1 B0510403 Transfer Line Cover 1 09907233 Wrench Open End 1 4 in x 5 16 in 1 M0415330 Top Seal Changing Tool 1 M0417030 Terminal Block Plug 14 Poles 1 N1011206 HS Start Ready Cable 2 N9301357 Fused Silica Transfer Line 0 32 ID 1 N9301376 Wafer Ceramic Cutter 10 Pkg 1 09904956 Rheodyne Nut 1 16 in 1 M0417002 Fuse 5x20 MM 10A 250V TD 2 M0417038 Fuse 5 x 20MM 5 250V TD 2 M0413401 Users Manual 1 Table 1 TurboMatrix 16 40 110 Headspace Shipping Kit Part No M041 3403 17 Introduction The following items should be included with TurboMatrix Trap Part No Description Qty 00090652 Septum Kit 1 04966624 Double Ended Wrench 2 L1003026 Graphite Vespel Ferrule 1 6 mm ID 3 M0413628 Air Monitor Trap 1 09903392 Nut Union 1 16 1 09900105 Graphite Vesp Ferrul
103. assembly P N N6700112 See the following photo Figure 21 4 Carefully loosen the nut in the back of the trap assembly Turn it 1 4 to 1 2 turn only since if you loosen it too much the O ring inside it will be out of alignment and difficult to reinstall See the following photo 82 Installation Figure 22 5 Use the trap removal tool P N N670 1077 to carefully remove the trap See the following figure 83 Installation 6 Wearing gloves carefully remove the new trap from the box and insert it into the trap housing hollow tube end first wire end last Figure 23 7 Put the ferrule on the trap the tapered edge must face towards the front See the next photo Figure 24 8 By hand gently push the new trap in as far as you can 9 Use the Alignment Rod P N N6700122 to gently push the trap into the O ring into the proper position You will feel a small pop as the trap goes through the O ring and is seated properly in the trap housing 10 Retighten the back nut until it stops 11 Inspect the dry purge assembly to see that it is not damaged Feed the dry purge assembly into the trap until it stops Installation NOTE If the dry purge assembly is damaged see the Routine Maintenance chapter for information on replacing this assembly 12 Reinstall the trap housing Do not use any tools only fingertighten to tighten the thumb screw since it will damage the ferrule 13 The trap must be
104. ast or Slow Heat Rate from the drop down list The default Trap Maximum Temperature is 400 C It depends upon the Trap material Unauthorized changes to higher values should be avoided CAUTION Follow the sorbant manufacturers recommendations for the upper trap temperature If the temperature is set too high the trap and instrument could be severely damaged Trap Setup Heat Rate a Max Trap Temp 400 C Em E A Figure 53 Internal Standard This button allows you to input the loop load loop equilibrium and the inject time 140 Operation Preferences Run Config Setup Connect Loop Load 0 5 Loop Equil 0 8 min Inject Time 0 5 min M Load IS Loop Reset Counter L OK Cancel Figure 54 Loop Load The time required to fill the sample loop Loop Equil The time required for the sample loop to drop to a constant pressure Injection Time The time required for the carrier gas to inject the standard into the vial Load IS Loop This box is checked off only when you are first calculating the loop equilibrium time Setup Tab The options on the Setup tab provide access to vial and system configuration Password Protection You can protect the instrument from unauthorized access using the password protection When enabled users must enter a password to gain access to the interface 141 Operation To enable and use this option 1 Open the Setu
105. azine HS 40 One Priority Vial Position Magazine Cap Nut Figure 32 Layout of the TurboMatrix Headspace Sampler 4 Press the On switch The power switch is located on the rear panel of the HS 5 The HS splash screen is displayed 6 Press anywhere on this screen 7 The log in message displays Enter your password and press OK hstd is the default password The local HS control interface displays 8 If you are using the HS control software connect the computer to the instrument as outlined in the control software manual Start the software and install the HS on the Lab tab as outlined in the control software guide Ensure the computer is communicating with the instrument 9 When the HS is first powered up it starts an 99 Operation initialization process lasting approximately 10 seconds and resets the hardware to default status During initialization vials which are still in the thermostatted oven are unloaded For this purpose the instrument looks for one empty magazine location in outside ring to unload the vials If there is no empty location the initialization process will be interrupted and the following error message is shown on the display Magazine Full Refer to Loading the Magazine on page 148 for details 10 If the initialization process was interrupted you must remove sample vials from the magazine before you can restart the initialization process again 11 Once the vials have been unloaded
106. be used for more than two days you may opt to shut it down If the instrument is to be disconnected from the GC be sure to cap the end the fused silica transfer line to prevent contamination of the system To shut down the automatic headspace sampler 1 Stop the running Headspace Method by pressing the Stop button 2 Wait until all the sample vials have been unloaded from the thermostatted oven 3 Unload the magazine Press the Rotate button to access vials that are under the oven 4 Press the power switch to turn the HS off NOTE Before proceeding to next step ensure that GC and injector detector conditions meet those in the Carrier Gas Shut Off paragraph in the Routine Maintenance chapter 5 Turn off the carrier gas supply 6 Turn off any related accessories and close the gas supplies With the HS 40 110 trap the column isolation mode will stay on and maintain column flow even when the trap instrument is powered off You can power down the HS 40 110 trap and still have flow going through the column If you are using an MS you can leave the MS pumped down 160 Accessories 4 Accessories 162 lt gt Accessories Options Board An options board is available for the instruments This board provides Four programmable time dependent switch relays the BCD interface one RS 232C port and support for the shaker and HS 110 automation module The HS 110 utilizes the options board for control of the cran
107. between the wide bore column and the detector The restrictor P N N9301354 has a 1 0 m x 0 18 mm I D A deactivated fused silica capillary is typical for this purpose 226 Method Development Headspace Sampling Using a Packed Column and a Packed Column Injector Packed columns are normally used in splitless operation They are typically installed onto a packed column injector which has a separate flow controller for carrier gas To set up your headspace analysis using packed columns and a packed column injector 1 Disconnect the HS heated transfer line from the packed column injector and replace the septum cap Make sure the GC is released from external control From the AutoSystem XL keypad or the Clarus 500 touch screen set the carrier gas flow to the level needed for your analysis if you have PPC If PPC is not installed on your GC adjust the flow controller to obtain the required head pressure From the AutoSystem XL keypad or the Clarus 500 touch screen set the required oven temperature and allow the system to stabilize for one minute at the required oven temperature Press the Carrier Prog button on the GC keypad for the AutoSystem XL or the Clarus 500 touch screen to access the carrier gas control display for the injector that that the HS 40 110n Trap is connected to For the AutoSystem XL press the Arrow Set key and read the GC injector pressure from the display This is the carrier gas pressure required to
108. ble vials it is possible that 175 Accessories vials will stick in the oven With the vial gauge P N B0151737 you can check the sample vials for e Outside diameter and circularity of the vial body and neck e Concentricity of the vial neck with respect to the vial body e Height of the vial If in doubt check the vials as shown below and discard any unsuitable vials Also check the vials visually for any damage r Vial is unsuitable Vial can be for use in HS used in HS Figure 68 Using the Vial Gauge Crimped Top Sample Vials The patented safety closures star springs incorporate pressure relief features which guarantee safe operation with the high pressure that may develop during thermostatting If a vial should burst you risk injury from glass splinters and possible damage to the instrument NOTE Such damage is not covered under the warranty Use only the cap removal tool P N N9301270 to open the sample vials See Decapping the Vials on page 274 Carefully check the sample vials after cleaning for hairline cracks and damage before reuse Do not use unsuitable vials Replace reused sample vials regularly PerkinElmer vials are guaranteed only for single use Hand Crimper for Crimped Top Vials The hand crimper P N N9302785 is required for sealing the vials You cannot seal the vials correctly without the crimper A b
109. boMatrix Headspace Leak Checking Error Messages Error Messages Description Vial x pressure error The vial standard headspace pressure is incorrect Table 17 Standard Headspace Leak Checking Error Messages Log Error Messages Error Messages Description Run terminated vial integrity errors Run stopped due to missing vials and or dynamic leak check failures Three consecutive vials fail the Vial Integrity Test and the run is stopped Too many vial integrity errors Run stopped due to missing vials and or dynamic leak check failures Three consecutive vials fail the Vial Integrity Test and the run is stopped Table 18 Vial Integrity Log Error Message 329 Troubleshooting Log Messages Description Extended therm GC not ready The instrument is not ready Extended therm Cryo temp Cryo temperature is not within tolerance of its setpoint for injection Extended therm Trap temp Trap temperature is not within tolerance of its setpoint for trap loading Extended therm Heated zones Heated zones oven needle transfer line are not within tolerance of their setpoints Extended therm Carrier Pressure Insufficient carrier pressure Table 19 Extended Thermostatting Log Message NOTE The extended thermostatting is checked during the pre injection phase for standard headspace that is before pressurizat
110. by position the pressure returns to P1 High pressure sampling is necessary if the vial pressure exceeds the column head pressure The standard balanced pressure sampling technique requires the column head pressure to be higher than the internal vapor pressure in the thermostatted sample vial When using wide bore capillary columns 0 53 mm internal diameter or high thermostatting temperatures it is possible that the internal pressure in the vial generated by the partial vapor pressures of the sample components can exceed the column head pressure In this case the differential pressure between column head pressure and vial pressure becomes negative The high pressure sampling accessory can be used with packed columns and open tubular capillary columns It can be operated independently or in combination with other installed pneumatic accessories such as the cryofocusing accessory 159 Operation HS 40 110 Trap Isolation Flow Pre Injection Peaks For the HS 40 110 trap the isolation flow should be carefully adjusted to 5 to 10 ml above the analytical column flow in order to prevent Pre Injection peaks For details see the paragraph Loss of Sensitivity Pre Injection Peaks in the Troubleshooting chapter Shutdown Headspace and HS 40 110 Trap Normally you do not need to shut down the instrument You can put the instrument into economy mode overnight and over the weekend See Setup Tab on page 141 If the instrument will not
111. ch screen will now be displayed in the selected language Preferences Run Config Setup Connect IV Key Clicks V BCD Negative Baud Rate g600 HandShake None F Language English En F Brightness AuxRS232 Notusea Date Time ea C OK Cancel Figure 56 Connect Tab Brightness The brightness controls the touch screen display Set the brightness so that the display is clearly visible under all lab conditions Auxiliary RS 232 This port is currently not available 146 Operation Date Time Press the date time option to enter the correct date and time The Time Date dialog box opens as shown below Select the desired date format and then enter the correct date Next enter the desired time format and the correct time Press OK to accept the new time x Dae Me OK 16 E Cancel Time i407 EE Figure 57 Date Time Dialog Box Starting a Run TurboMatrix Headspace and HS 40 110 Trap Preparing Samples In some methods pre cleaning the vials by washing with a detergent solution followed by rinsing with distilled water and drying in an oven is recommended Normally the headspace vials are sufficiently clean and no pretreatment is necessary In fact such washing particularly with a detergent may add impurities to the vial The main source for blank peaks from an empty vial is not contamination on the vial s inner surface but bleeding of the septum and or impurities
112. conditioned see the Routine Maintenance chapter for this procedure before analytical use by establishing carrier gas flows and heating the trap several times to remove any volatile impurities from the trap packing If you heat the trap to high temperatures take care that the analytes do not degrade at these high temperature For example if the halogenated hydrocarbons are present in the sample the temperature should not exceed 325 C When the trap is heated to 325 C trimethyl benzenes are released quantitatively For higher boiling species it may be necessary to use a higher trap temperature Flow during collection of sample es ae Flow during Trap Heat ae a NESS rene Figure 25 Air Monitoring Trap M041 3628 See the Routine Maintenance chapter in this guide for information on testing conditioning and cleaning the trap Checking the Needle Purge Gas Flow TurboMatrix Headspace and HS 40 110 Trap The purge gas flow through the needle unit is set to 15 3 mL min The flow is used to purge the needle of residual sample and to keep it clean between injections The flow is fixed and you only need to initially measure the flow to ensure that it is within the recommended range 85 Installation To check the needle purge gas flow 1 Ensure the carrier gas is connected Connect a flowmeter to the Purge vent Switch on the instrument Set the pressure for 5 psi If the flow rate is correct then disconnect
113. ction configuration ensure that the column liquid phase material can withstand a temperature of 210 C If not then set the transfer line temperature to the maximum allowable for the selected liquid phase If you are observing a severe contamination problem you should disconnect the transfer line from the GC Make sure that the GC oven detector and injector are at room temperature before you start working on them WARNING Action Replace the fused silica transfer line See Installing the Transfer Line Cap in the Routine Maintenance chapter of this manual Action When the transfer line is heated there must always have flow through the transfer line This 313 Troubleshooting 314 Action Action Action becomes more critical if you are using an on column configuration that utilizes the GC column as the transfer line When you are changing the supply tanks and if direct or on column connection you must power down the instrument and allow the transfer line to cool Also insure that the GC oven injector detector is cool and the MS filaments are off If the transfer line is disconnected from the GC for any period of time protect the end of the fused silica tube with the transfer line cap P N B0510403 See Installing the Heated Transfer Line in the Installation chapter The fused silica tube transfer line may need to be further de activated for your application Contact the PerkinElmer for further
114. d 0 eee eeceeceseeereeeeeeeeens 189 Temperature Tab Headspace and HS 40 110 Trap 191 Needle and Transfer Line Temperatures 191 Temperature Mode eee eesceseceeeeeeeereeenseeeeeeees 191 Thermostatting Temperature Headspace and HS 40 110 Trap sti chien hss vale taite te tere loess 192 HS 40 110 Trap Temperatures eee 193 Cryofocusing Temperature Headspace Only 193 Timing Tab esee enr aea 194 Pressurization Time Headspace and HS 40 110 Trap eee 194 Vial Pressurization Carrier Pressure Headspace Only 0 cece ceeeeeeeeseceeceseeeeeeeeenees 194 Injection Time Headspace Onlly eee 195 Thermostatting Time Headspace and HS 40 110 Trap eee 196 Injection Volume Headspace Only 0 197 Withdrawal Time Headspace Only 198 Setup HS 40 110 Trap Only eee 198 Contents Decay Mergen so an eR ne 198 el ol en Ree ee ne er 201 Pressurization Time cece eeeeeeeeeee 202 Trap Hold HS 40 110 Trap Only eee 203 Dry Purge Time HS 40 110 Trap Only 203 Desorb Time HS 40 110 Trap Only 204 Pre Post Cryofocusing Time Headspace Only 204 The Option Tab wi 23 c n 20h nears oe 206 Injection Mode Headspace Only cece 207 Principles of High Pressure Sampling Headspace Only ooreen e 208 Setting the Withdrawal Time eeeeeeeeeeeeeeee 211 For High Pressure Sampling 000 211 Water Trapero eane au ce
115. d You must use the same type and quality of carrier gas for the HS that you are using for your GC 3 Press Calibrate Sensor bar gt PPC Calibration bar gt Zero Disconnect the carrier gas to the Carrier In port 5 Press the Zero button The PPC module sets its zero point 6 Once you have completed the operation the date will be entered for future reference 7 Press OK to accept the settings and close the tab 8 Reconnect the carrier gas to the carrier in port and set to 90 psi See PPC Tab in the Method Development chapter for details on configuring the PPC module and creating methods that utilize the PPC options 275 Routine Maintenance HS 40 110 Trap Maintenance The HS 40 110 trap differs from the other headspace samplers in that it also has a solid end trap P N N6701170 The following sections review the unique maintenance issues for the trap Removing and Replacing the Trap After prolonged use the packing in the trap may become contaminated begin to decompose or shift This will cause the retentive properties of the trap to diminish indicated by decreased output when a standard test sample is analyzed or by skewed peaks If in doubt replace the trap with a new one replacing all ferrules at the same time Wear gloves when you are handling the trap Handle the trap with great care since it is made from quartz and can easily break WARNING NOTE Before proceeding always have one or tw
116. d by the PII time Using the Tray Rotation Feature While Running A Vial Sequence To optimize the TurboMatrix throughput cycle and avoid analyzing empty vial positions Firmware version 2 14 83 for the HS 40 and 151 Operation HS 110 includes a Tray Rotation countdown dialog The main objective of this dialog is to rotate the autosampler tray enough to make the vial positions under the oven accessible alert users when the instrument will be ready to load the next vial and rotate the autosampler tray back to its position so that the TurboMatrix can continue with the analysis To access this functionality while a sample sequence is being analyzed the Rotate button becomes available after the run has started The button label changes to Load once a run is started see figure on left The Load button will only be enabled if the Priority Vials feature is set to None under Preferences Pressing Load will activate the Tray Rotation countdown dialog see figure on right and rotate the tray to enable access the next available vial locations Each time the Rotate button in the Tray Rotation countdown dialog is pressed the tray continues to rotate approximately 90 degrees to provide access to additional vials The Tray Rotation countdown dialog will be open and active during the countdown time displayed at the top of the window This countdown timer expires approximately 10 seconds before the next autosampler action is due to activate e g
117. d in the GC Injector During sampling the vial is first pressurized P1 with carrier gas P1 must be higher than the column head pressure at the GC injector P2 Carrier is gas supplied to the injector via the normal carrier gas supply P2 Excess carrier gas is vented through the injector splitter at arate of 15 ml min or more During the sample injection the sample will elute from the transfer line into the hourglass and immediately enter the chromatographic column Excess sample eluting from the transfer line will exit 169 Accessories through the gap between the end of the transfer line and the constriction in the hourglass and will mix with carrier gas flowing though the injector outer liner and out through the split vent The excess sample flowing out of the hourglass acts as a barrier to the carrier gas flowing through the outer liner and prevents it from reaching the inlet to the chromatographic column and so no dilution or dispersion of the sample takes place Fused Silica Transfer Line Carrier Gas Pa Inlet P2 i Eo l f T I Figure 64 Sample Flow Through the Zero Dilution Liner Hourglass Insert Outer Liner GC Column Installing the Zero Dilution Liner To install the zero dilution liner in the GC injector 1 Turn off the GC and the HS Allow the GC oven and injector to cool 2 Remove the column and existing injector liner Refer to the GC user
118. d on the left side of the GC the HS should be fitted with the optional long transfer line P N M0413532 In these cases approximately 180 cm 72 of bench space will be required for the HS GC system This does not include the space required for the computer and related hardware The spacing requirements will increase if you are using the TurboMass Mass Spectrometer or an AutoSampler If the cryofocusing accessory M0413411 is installed a 35 liter Dewar flask B0500924 is required for the liquid nitrogen and should be placed under the lab bench The Dewar flask is approximately 50 cm 20 inches high x 25 cm 10 inches wide For maximum performance and minimum maintenance the site for the instrument and any accessories must e Be located close to the required electrical supply and gas supplies e Have sufficient room to work comfortably with the instruments and allow you to reach connections at the rear of the instruments e Have space to place the gas chromatograph near the HS ina convenient position e Have space to place the computer and any hardware associated with the data handling system near the instrument in a convenient position If you are connecting a printer make sure that there is enough space for the printer and associated paper supply Electrical Connections AC Line Connections To prevent potential injury to yourself and damage to the instrument switch off all instruments in the system and discon
119. d to the plumbing area between the PPC module exit SV1a and the inlets of the solenoid valves SV1 and SV9 See following figure It does not involve the trap the Sampling Head and Needle and their plumbing Nor does it involve the transfer line and the GC column As you can see in the following figure all three solenoid valves SV1la SV1 and SV9 are closed In this way this plumbing area is closed and pressurized As shown in the following figure Isolation Flow to the transfer line and the GC column is shut off SV8 is vented to atmosphere If you are using high flow rates Be sure to protect the GC column and the detector by e If an MS detector is used in this channel ensure that the filament is switched off e Ifno carrier gas is supplied to the HS Transfer Line cool it down if using a transfer line with a stationary phase 267 Routine Maintenance Isolation Flow Shut Off Cool the transfer line Cool and protect GC column and detector before starting this test Ea net sv2 Eig VALVE STATE TABLE SV STATE la OFF 1 ON 2 OFF 8 ON 9 OFF A Trap Dry Purge outlet Leak Test Slide On Off valve must be Ea SVia open pulled outwards SV1a SV1 SV9 are closed This plumbing area is pressurized Figure 111 Valve Leak Test During this Valve Leak Test the Needle Purge SV2 is open The slide On Off valve at the Trap Dry Purge outlet must be o
120. dard mode In this mode the sample vials have the same thermostatting time This mode is generally used for all routine operations The instrument software calculates the PII value Period from Injection to Injection from the parameter values entered The PII value is shown on the display For optimum sample throughput i e the greatest number of samples analyzed in the shortest time it is essential that the PII value is only slightly longer than the cycle time of the selected GC method If the above conditions can be fulfilled then the thermostatting times for the individual samples will overlap Analysis Time il Thermostatting Time JW Sample 1 Sample Injection f MA INTANT JW kl Sample 2 N Ii Ml Sample 4 PI 4 Figure 87 Overlapping Thermostatting 212 Method Development In the worst case the samples will be sequentially thermostatted You can normally achieve optimum thermostatting conditions by making slight adjustments to the thermostatting time or the GC Cycle time Analysis Time j Thermostatting Wih Time 1 Sample 1 hk Sample JW at jection k Sample 2 Kl Injgction Sample 4 AWE Sample 3 le PII gt Figure 88 Sequential Thermostatting MHE Mode The MHE mode Multiple Headspace Extraction is used to quantitatively determine an analyte in a sample It is especially useful in the analysis of voliatiles in insoluble samples Such samples cannot be quantitatively an
121. ded for the HS 40 110 trap 712 Composite Zero Dilution Split Injector Liner for Headspace Interfacing 74 Installation Instructions 0 0 00 eee eee 74 Operations ta n e EE ees ESES 74 Connecting to a Packed Column System 75 Gas Connections ce eeeesceseceneeeeeeseceseceeeeeeenaees 75 Carrier GaS ene oee test eek ae a iese 75 HS 40 110 Trap Connections 79 Installing the Trap in the HS 40 110 Trap 81 Checking the Needle Purge Gas Flow 85 TurboMatrix Headspace and HS 40 110 Trap 85 Leak Testing the Headspace 86 Leak Test the HS 40 110 Trap 89 OPGrallON wciiiiiissesieecciissasssrieacteecieandsdiisecasnsnencie 95 Introdlictiones isseas iia die iiia Receeatleed aa 97 TurboMatrix Headspace and the HS 40 110 Trap 97 Powering up the Headspace Sampler 98 Setting the Carrier Gas Pressure 100 The Touch Screen Display 0 0 eceseeeeesseeseeeneceeees 103 The Run Tabiin secs oti aie eli neh ude ai 104 Single Method Operation 105 Creating a Sequence 0 eee eeeeseereceneceteeeeeeees 106 Status Tab Headspace and HS 40 110 Trap 108 Temperature Screen Headspace and HS 40 110 Trap 109 Contents Timing Tab Headspace and HS 40 110 Trap 112 The Status Tab Option Tab Headspace 115 HS 40 11 O T rap yesivedete Sante tector aie as 119 Status Tab Temp 0 eee ceseceeeeeeeeeesneeenseeseeees 119 Status Tab Timing Tab for the HS
122. desired start vial 3 Enter the desired end vial 4 From the method drop down box select the method to be used for the selected range of vials 5 Press the Add button to add the entry to the sequence 6 Press the Start vial entry box again and enter the start end vials Select the method to be used for the selected range of vials from the drop down box and then press Add to add the entry to the sequence 7 Repeat these steps until you have created the desired sequence To delete an entry from the sequence select the entry in the list and press the Delete button To change the vial range you must add a new entry with the revised vial range and then delete the old entry 8 If you edit the methods called by your sequence the sequence will use the revised methods If you need to edit a method but do not want to affect your sequence then save the revised method with a different name NOTE You will not be able to edit any of the selected methods if method editing has been disabled from the Preferences tab 9 Press the Green Start button to run the sequence The HS will configure itself based on the first method The instrument status will be Not Ready until the instrument reaches all of the set points Once it has reached the set points the vial will be loaded and the analyses will continue as determined by the method If you have the HS 40 or HS 110 with the 15 vial oven vials will be loaded at regular intervals as determine
123. does not seal against the outer liner thus ensuring gas flow between the two Outer Liner Fused Silica P N N101 1445 Transfer Line Inner Liner P N N101 1446 i V VN GC Capillary Column Figure 62 Zero Dilution Split Injector Liner The assembled liner is installed inside the injector in the same manner as a normal injector liner The fused silica transfer line is installed at the top of the injector and the chromatographic column is introduced through the bottom of the injector 168 Accessories The GC column is pushed up through the outer liner and insert until it rests against the hourglass constriction The column is further inserted and lifts the hourglass insert up until the constriction stops as it contacts the end of the transfer line The GC column is then withdrawn about 2mm to leave that distance between the end of the transfer line The insert is held and is loosely sealed on the end of the column by gravity The end of the column is then secured and sealed at that position by a nut and ferrule Fused Silica Transfer Line HS Injector wa Septum Adapter Carrier Gas a Inlet P2 M Splitter End of Fused Silica Transfer Line End of GC Column VI Column Nut GC Column and Ferrule Figure 63 Cross Section of the Zero Dilution Split Injector Liner Installe
124. e Close the cylinder valve when it is not in use e Do not subject the regulator to an inlet pressure greater than recommended e Do not move or detach the regulator when it is pressurized or when it is in use e Before connection ensure the cylinder valve and the regulator CGA connection are clean e When connecting a regulator to a large gas cylinder turn the valve on the cylinder clockwise to close the cylinder Turn the regulator off Open the cylinder valve slowly and check for leaks Adjust the delivery pressure and then open the regulator outlet valve Adequate Ventilation If compound threshold limit values TLVs are exceeded you should use a fumehood to prepare samples and vials and provide adequate ventilation for the vial venting option You must also vent the GC detector and split vent ports Use flexible tubing fitted with adapters to vent these ports to a fumehood or outdoors The pressure set by the method will determine the outlet flow rates at these ports Extreme Temperatures High Temperatures The heated zones oven needle transfer line in trap of the headspace sampler can generate temperatures up to 210 C to 400 C in trap Do not touch any part of the oven or recently unloaded vials until they have cooled down to room temperature Low Temperatures Liquid nitrogen is used as a cooling medium in conjunction with the cryofocusing accessory TurboMatrix 40 110 29 Introduction Headspace onl
125. e heated transfer line You can upgrade the HS 16 to an HS 40 or an HS 110 Up to 40 vials can be loaded into the magazine of the HS 40 The oven can accommodate up to 12 vials and overlapping thermostatting allows the instrument to obtain maximum sample throughput An optional shaker device is available to reduce equilibration time You can upgrade the HS 40 to an HS 110 NOTE The HS 40 and HS 110 have exactly the same function except for the number of vials The HS 110 can accommodate up to 110 vials The 12 vial oven is standard and overlapping thermostatting allows the instrument to obtain maximum sample throughput The advanced automation system can be programmed to run series of vials according to preset methods The HS 110 also comes standard with BCD output capability which is optional on the other models NOTE The 12 vial oven is in reality a 15 vial oven but the software only allows up to 12 vial simultaneous loading and overlapping thermostatting Programmed pneumatic control PPC provides the electronic control of pressures and flows for inlet and auxiliary gases This option can be installed on any one of the above models to automate 13 Introduction gas handling and delivery in the HS PPC comes standard on the HS 40 110 trap High pressure sampling is supplied as part of the PPC option HS 40 110 Trap NOTE The Trap model is offered with two vial options for either 40 or 110 but for the purposes of this Users
126. e the greatest number of samples analyzed in a given time it is essential that the PII value is only slightly longer than the GC cycle time The PII value shows the effects of the timing changes in the analysis on the vial throughput In a 15 vial oven it is possible to overlap the thermostatting time of the vials and reduce the PII 157 Operation Load vial into oven Thermostat vial Decay pressure through trap Withdraw needle Trap Dry Purge optional Step Yes Figure 58 HS Trap Logic flow Diagram Retum vial to magazine Chromatography Pll Algorithm No 158 Operation High Pressure Sampling Headspace Only The high pressure sampling option is automatically available if you have the PPC option installed The high pressure sampling technique is used to prevent pre injection Pre injection occurs when the internal pressure of the sample vial is greater than the sampling head pressure In such cases the sample expands onto the transfer capillary as soon as the sampling needle moves down into the vial This causes split peaks and double peaking on the chromatogram High pressure sampling permits sampling in such cases without these secondary effects A higher pressure P2 is applied during pressurization of the vial and injection of the sample After injection of the sample i e immediately after withdrawal time and vent time and when the needle is in the stand
127. e and rating Consult the fuse chart Both fuses must have the same rating Replace the drawer and close the fuse door Reconnect the line cord Resume normal instrument operation 241 Routine Maintenance For protection against fire hazard replace only with the same type and rating of fuse WARNING Voltage Fuse Part Number 50 60 Hz 250V rated 100 T 10A M041 7002 120 T 10A M041 7002 220 T5A M041 7038 230 240 T5A M041 7038 Table 13 HS Fuses F sse Fuses Drawer Power Switch e a Fuse Door AC Connector Line Cord Connector Figure 95 Replacing the Fuse 242 Routine Maintenance The Sampling Needle Every 1500 injections a maintenance display is shown indicating that the three o ring seals on the needle need to be replaced The injection interval can be changed depending on your application To acknowledge the message and clear the display press the display This display will be shown on two more occasions and then again after the next interval of 2500 injections It is only necessary to change the sampling needle when it is damaged or when you wish to change to another needle type You may also want to replace the needle if you are changing applications A platinum iridium Pt Ir needle is available for highly corrosive applications and Siltek inert coated needle is available for r
128. e and robotic arm that are used to load the vials into the oven The BCD option and the shaker both require the option board to be installed and enabled NOTE The shaker is not available for the HS 16 Timed Events The optional timed event connector has terminals for 6 programmable relays External devices may be timed by these relays CAUTION nput voltage must not exceed 50 V DC Input current must not exceed 0 5 A DC You may program the events using the event tab To program events 1 Open the Status tab or the Method Editor tab and select the Timing tab 2 Press the Relay button to open the Event Relays tab NOTE If the Relay button is not displayed on the Timing tab it must be enabled from the Preferences Run tab See Run Tab on page 137 163 Accessories 164 Event Relays Relay Number 2 Event Time 10 sec Action for E Relay Time Action Cancel a Figure 59 Event Relays Dialog Box 3 Enter the relay number that you want to activate or deactivate 4 Enter the Event time and the required action Turning a relay on and off requires two events 5 Press the Add button to add the event to the listing To delete an event from the list select the event and then press the Delete button 6 Repeat this step for each event that you require You can enter up to 6 events 7 Press OK to accept all of the events and close the window 8 Ifyou are using the Method Ed
129. e box to enable the option 3 Press the Config button to open the configuration dialog box Economy Mode Activate during fie 00 08 00 E After being idle for 30 El minutes Wake up instrument M ee ea Figure 55 Economy Mode Dialog Box 4 The HS only goes into economy mode after a predetermined interval during which there is no activity You can select this time If you select 0 then the instrument will go into economy mode at the beginning of the selected interval providing an analysis is not in progress If you enter 30 minutes then the instrument will go into economy mode 30 minutes after all analyses have been completed 5 Now enter the time for the HS to wake up At the wake up time the HS switches on the heaters and re activates the purge valve The instrument configures 144 Operation itself according to the method specified on the Run tab 6 Once you have entered the desired settings press OK to accept the settings and close the tab 7 Confirm that the date and time are correct If necessary enter the correct date and time Display Font You can select from a number of different display fonts to customize your touch screen To change the font 1 Press the Font option and select the desired font from the drop down list 2 Press OK to close the dialog box You must log out and then open the interface again before the font change will take effect HS 40 110
130. e dry air is used to drive the pneumatics required for the automation system The purity of the dry air and delivery lines is not an issue as this gas does not come into contact with the sample A high purity stainless steel regulator is not required for the dry air as this gas does not come into contact with the sample A brass regulator will be suitable You can use Teflon or copper tubing to connect the regulator to the HS NOTE If you are running more than one instrument from a single supply of dry air you must ensure that your supply system can deliver a minimum of 3 liters per minute at 70 psi for each instrument under all sampling conditions To connect the dry air supply to your instrument 1 Connect a clean two stage regulator to the dry air tank The regulator should also have a 1 8 parallel compression fitting with which to connect the regulator to the HS The delivery pressure must be adjustable to 90 psig 620 kPa 2 Connect the regulator to the HS Dry Air in port The purge connection at the rear of the HS is a 1 8 brass fitting 77 Installation 3 You can use Teflon tubing for the dry air supply lines If you are using Teflon tubing ensure the lines can withstand pressures of 100 psig 4 Securely tighten all fittings 5 Open the tank and set the delivery pressure to 90 psig 620 kPa Do not set the delivery pressure higher than 100 psig 690 kPa WARNING Connector Di
131. e normal method pressure Unplug the fused silica line and ensure that there is no septum material blocking the fused silica line If you are leak testing the HS sampling system you should check the following connections first 262 O rings in the upper and lower needle sealing elements Transfer line connection to the needle unit Routine Maintenance e Column connection at the injector outlet or to a transfer line in case of a direct connection e Sample vial closure old septa caps not crimped correctly e Trap fittings If you are testing the whole chromatographic system leakage may be occurring at the GC connections NOTE Ensure the HS sampling system is leak tight before connecting the transfer line to the GC Refer to the GC manual to leak test the injector and detector connections The following list provides further locations to test the GC connections e The connection of the heated transfer line with the GC injector septum e Column connection at the injector outlet or to a transfer line in case of a direct connection Leak Testing the HS 40 110 Trap You must leak test all the connections for the GC as outlined in this procedure You must also leak test the trap the fittings that connect the trap to the transfer line and the fittings inside the HS 40 110 trap to determine that there are no helium leaks 1 Let the GC cool down Cool the headspace transfer line 2 Undo and remove the chromato
132. e test command provides access to the leak test and the cryofocusing test Use the leak test to ensure that your HS sytem is leak tight See Leak Testing the Headspace in the Installation chapter for details on performing the leak test NOTE Cryo Test is disabled in the HS Trap version The cryofocusing test enables you to determine the length of time required to reach the cryofocusing temperature You will need this information to set the Pre cryofocusing time See Pre Post Cryofocusing Time Headspace Only on page 204 for details on performing the cryo test Log Out Headspace and HS 40 110 Trap The Log Out command closes the tabbed interface and logs out The HS splash screen is displayed Calculator You can use the calculator in standard view to do simple calculations The calculator can be used to do MHE calculations To perform a simple calculation 1 Enter the first number in the calculation 2 Click to add to subtract x to multiply or to divide 135 Operation Enter the next number in the calculation Enter any remaining operators and numbers Click ON OY e Sqrt calculates the root of the displayed number X 2 calculates the square of the displayed number 7 Press the close button x on upper right corner of the title bar of the window to close the calculator 8 If you are performing MHE runs you can enter the integrated peak area and press MHE Enter the integrated area of the second pe
133. e values determined by the regression analysis you will get at an extrapolated total peak area number which directly corresponds to the total amount of the compound present in the sample Once the total area for a particular component has been determined its concentration in the sample can be calculated by using total peak areas derived from previous MHE analyses of a calibration standard 1 PerkinElmer Inc HS 40 Control Application July 1990 p 31 32 231 Method Development 232 Routine Maintenance 6 lt gt Routine Maintenance Introduction This chapter describes the maintenance procedures that can be performed by the user Do not attempt to make adjustments replacements or repairs to this instrument except as described in the accompanying user documentation WARNING NOTE This equipment requires no specified inspection or preventive maintenance to ensure the continuous functioning of its safety features The instrument is constructed with high quality components and requires little maintenance other than to keep it clean and free of dust The HS does require some regular maintenance and replacement parts which will vary with usage This will ensure optimum operating efficiency You should only perform the maintenance procedures described in this section NOTE In most cases the procedures in this chapter involve gaining access to internal parts of the instrument It is therefore extr
134. eactive samples this needle is shipped with the HS 40 110 trap Types of HS Needles The jet needle can be used for both packed and capillary columns Depending on the sample type the jet needle is available in three different materials e Standard stainless steel needle P N B4000011 This needle has three grooves at the top of the needle to differentiate between the stainless steel needle and the Pt Ir needle e Platinum Iridium Needle for free volatile organic acids bases and other corrosive compounds The Pt Ir needle has 4 grooves at the top of the needle P N B0510364 e Siltek inert coated needle standard with the HS 40 110 trap If you have a manual pressure regulator the wide bore needles may also be used Wide bore needles offer quicker pressurization of the sample vials Removing and Replacing the Needle Headspace Only To change or replace the needle see the following figure 1 Turn off all heated zones by setting the temperature to 0 Allow approximately 30 minutes for the needle assembly and transfer line to cool down 2 Once the system has cooled switch off the instrument 243 Routine Maintenance 10 11 12 Turn off the gas supplies to the instrument In the case of direct or on column connections ensure that the flame is out if using an FID and that your oven injectors and detectors are at room temperature Disconnect the instruments from the electrical supply Pull gently on t
135. eases the crimping pressure Replace the crimp lever and the pin but not the snap ring or circlip Seal an empty vial with a septum star spring and crimp cap and check the closure carefully to ensure that it has been sealed correctly Repeat steps 10 to 13 until a perfect seal is obtained Seal the plunger into the stamper with a thread sealant Reassemble the hand crimper 273 Routine Maintenance Decapping the Vials Some chemicals may be hazardous or may become hazardous after completion of an analysis Do not store handle or work with any chemicals or hazardous materials unless you have received appropriate safety training and have read and understood all related Material Safety Data Sheets MSDS Use store and dispose of chemicals that you require for your analyses in accordance with the manufacturer s recommendations and local safety regulations You must comply with all federal state and local laws related to chemical storage handling and disposal You must work under a suitable hood when handling and mixing certain chemicals The room in which you work must have proper ventilation and a waste collection system Always wear appropriate safety attire full length laboratory coat protective glasses gloves etc as indicated on Material Safety Data Sheets Once the vials have cooled you can decap them The caps cannot be reused The vials should only be re used if they can be cleaned reliably and if the vial
136. ecaacus oe tes nade ceandavedenateinnes aa 161 Options Boardercross nernet artie iis 163 Timed Eyentsn sanin aneen ank naa 163 BCD Intertace ccs eerie a ate 165 The Vial Shaker ACCESSOTY ceeceeseeseceteceteceeeeeees 166 PPO nk ihe neat Hise A e honda 167 Contents Composite Zero Dilution Split Injector Linet 168 Description na uii ie Gan hanes 168 Installing the Zero Dilution Liner 170 Operation of the Zero Dilution Liner 00 0 171 Cryofocusing ACCESSOLY cc eecsseceseeeecereeereeeaeeneeens 172 Principle of Operation 172 Cryofocusing with the Water Adsorption Trap 174 Sample Vials icaeoie aeii 175 Using the Vial Gauge to Check Sample Vials 175 Crimped Top Sample Vials cece eeeeeeeeees 176 Hand Crimper for Crimped Top Vials 0 0 0 0 eee 176 Sealing the Hand Crimped Vials 0 0 0 177 Screw Top Sample Vials 2 0 0 0 eeeeseeeseceeeees 178 Accessories Screw and Crimp Cap Vials 178 Seal Swiss t elie sie Glen es See RTA 179 Headspace Control Software s es 180 HS 40 110 Trap Accessories n s 182 Method Development cceeeeseseeees 183 TntrOdUcti On ei 22i chivdivet ooeee pantens a E eee pea 185 Principles of Headspace and Headspace Trap Analysis ce eseeseeeeeereeseeeneeeneees 185 The HS Sampling Technique cee cece eneeeeeees 186 HS 40 110 Trap Sampling Technique 187 Creating a New Metho
137. ect method from the choices See Single Method Operation on the HS on page 149 for details Run Status Log Vials 1 to 12 i Method en H 1 Enter vial range Use buttons 2 Select Method 3 Load vials 4 Touch Start button to begin run E el STANDBY 14 45 47 l Stat Rotate Tools 7 Figure 33 Run Tab Single Method Operation To start single method operation 1 If a single method operation with a pre selected method has been selected then you only need to enter the vial range The selected method is displayed Beside the Vials option you enter the start and stop vials Press the desired entry box to select the option Press the plus or minus button to select the desired start vial then enter the desired end vial From the Method drop down box select the method to be used for the selected range of vials Press the Start button to begin the analysis A Start Run window will appear Press the OK button 105 Operation NOTE A message will appear if the instrument is not at equilibrium and what functions are not ready The HS will configure itself based on the method parameters The instrument status will not start until the instrument reaches all of the set points When the GC and the HS are ready a vial will be loaded into the oven The vial will be thermostatted and the analyses will continue as determined by the method If you are using the HS 40 or HS 110 with the 15 vial oven
138. ectrical Connections 000 0 ee eeeessceeseceeeeseeeeeeeeeneeees 43 AC Line Connections 0 ce eeeeeceeseceseeeneeeeceseeees 43 Electrical Surges Tongen irus iaren 45 Connecting the HS to a Gas Chromatograph 46 Gas Supply System occ es ceecsseeseeeeeeeeeeneeeeeeseeees 46 Gas Supply Specifications 47 Electrical Connections 0 e ee eeeeseeseceeeeeeeeeeeeeeneeees 49 The HS Input Output Port sosser 49 HS Output Signals neersien 51 HS Input Signals s iccis ene aites waite 53 Timed Event Relays 0 cece eeesesseesceeecereeeeeeneeees 54 Connecting the HS to the AutoSystem XL or Claris 500 GC orte tiect eere iee eee aiea 55 Contents Connecting the HS to other GCs except the HP 5890 HP 6890 and HP 7890 00 eeeeeeeeeeeneeeneeeteeeees 56 Connecting the HS to the HP 5890 and HP 6890 57 Installing the Heated Transfer Line eee 58 Installing the Heated Transfer Line at the HS Needle Unit TurboMatrix Headspace Only 62 Installing the Heated Transfer Line at the HS Needle Unit HS 40 110 Trap Only 65 Installing the Heated Transfer Line at the GC Injector for Split Operation TurboMatrix Headspace Only 68 Liner Recommendations c ccccceceees 68 Installing the Heated Transfer Line at the GC for Direct Connection ccccccceesesssecescecccececsceceeeeees 71 Recommended for the HS 40 110 trap 71 On Column Connection cccccccccecseseeceeeceneees 72 Recommen
139. edle that is too hot For best reproducibility set the needle temperature to a value 5 10 C higher than the sample temperature HS oven temp This also applies to the transfer line Set the temperature at or slightly above 5 10 C the thermostatting temperature You must also consider the GC oven and injector temperatures Do not set the transfer line below the injector temperature You must remember that in the heated transfer line the headspace gas is a mixture of air with trace concentrations of the analytes thus too high a temperature may cause sample decomposition by oxidation Temperature Mode Three temperatures can be combined so that when you raise or lower the combined temperature all three settings are adjusted If for example you enable the Combined option and raise the temperature by 5 C then the needle the transfer line and the thermostatting temperature will all be raised by 5 C If you choose the Separate option then each temperature can be set independently Track Oven Headspace and HS 40 110 Trap The Combined temperature option is activated if you enable the Track Oven by checking it s box NOTE The needle and transfer line must be maintained at 5 10 C higher than the thermostatting temperature 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 71 191 Method Development Thermostatting Temperature Headspace and
140. edle Seal Assemblies 247 O Ring Seals 252 Reproducibility Test 239 RS 232 Auxiliary Port 146 Standard Port 54 Run Starting 149 Tab Configuration 136 Tab Options 104 S Safety Chemical Information 26 274 Safety Closure Assembly 177 Safety Information Sample Vials 32 175 Vials 175 Safety Practices 21 Adequate Ventilation 29 Compressed Gases 28 Laboratory 27 Regulator 28 Sample Carryover 310 Leak Testing Injection System 261 Loss 315 Overloaded GC Column 310 Poor Recovery 315 Preparation 177 Sample Vial Checking 175 Cleanliness 238 Replacement 337 Safety Information 32 Sealing 176 Sample Vials 175 crimped top 176 Sampling Index High Pressure 159 High Pressurel Option 208 Packed Column 227 Split 218 Splitless 223 Supplies 97 Wide Bore Capillary Column 226 Save Save As Command 134 Seal Removal Tool 248 250 Sealing Vials 176 Seals 179 Assembly 177 Changing Lower Needle 249 Changing Upper Needle 247 Cleanliness 238 Replacement 337 Sensitivity Reduced 315 Sensitivity Reduced 219 Sensor Failure Fault 301 Septa 179 Aluminum Coated Silicone 179 Butyl Rubber 179 PTFE Coated Butyl Rubber 179 PTFE Coated Silicone 180 Sequence Creating 106 Multiple Methods 106 Starting 150 Service Before You Call 235 Contacting 335 Customer 335 Setting Carrier Gas Pressure 100 Date Time 147 Setup Tab 141 Shaker Accessory 166 Activating 117 353 Index Frequency Scanning 215 Method Development 215 with MHE 11
141. em Always wear appropriate safety attire full length laboratory coat protective glasses gloves etc as indicated on Material Safety Data Sheets Do not sample carbon disulfide or other compounds with a self ignition point of 100 C or less Refer to the MSDS sheets for compound specific information These types of compounds should not be sampled due to the risk of self ignition of the CS in the thermostatting oven or at other heated parts of the system The responsible body e g Laboratory Manager must take the necessary precautions to ensure that the surrounding WARNING workplace is safe and that instrument operators are not exposed to hazardous levels of toxic substances chemical or biological as defined in the applicable Material Safety Data Sheets MSDS or OSHA ACGIH or COSHH documents 26 Introduction OSHA Occupational Safety and Health Administration United States ACGIH American Conference of Government Industrial Hygienists United States COSHH Control of Substances Hazardous to Health United Kingdom If you are working with volatile solvents toxic substances etc you must provide an efficient laboratory ventilation system to remove vapors that may be produced when you are performing analyses You must vent hazardous fumes and vapors Disposal of wastes must be in accordance with all national state and local health and safety regulations and laws WARNING Your laboratory
142. emely important to heed all warnings regarding especially electrical and mechanical hazards Carefully review the safety information in Chapter 1 Before starting any maintenance e Switch off all the instruments in the system e Disconnect the instruments from the electrical supply e Allow hot parts of the instrument to cool down e Follow the maintenance instructions exactly as described in this manual 235 Routine Maintenance Item Operation Frequency Clean the Needle Every 500 injections Replace Needle Seal Assembly Every 2500 injections Replace o ring seals Up to 1500 injections Change trap HS 40 110 Trap Only As required Run reproducibility test As required Clean the magazine As required Zero the PPC module As required Table 11 Maintenance Schedule General Laboratory Cleanliness Headspace Sampling and gas chromatography are very sensitive techniques If proper precautions are not taken the surrounding environment will contaminate your system NOTE All users must be made aware of the circumstances that can lead to contamination of the system The degree to which precautions are necessary depends on the sensitivity required for your application Trace level determinations at ppb or ppt levels require substantially more care than determinations at ppm levels Background interference can be kept to a minimum if you take sensible precautions Cleaning and Decontamination Befo
143. emperature limit than the bulk material or vice versa Cause The PPC on the GC has not been setup for operation with an HS Action You can check by pressing SYSTEM from the GC keyboard then keep pressing ENTER until you see HEADSPACE Config installed YES if not set it to YES On the Clarus GC touchscreen select Tools gt Configuration gt Injector icon and insure that the HS control box is checked Cause The split flow has not been set correctly Action If you have a split set up you will normally experience some dilution from the carrier added to the GC injector through the pneumatic modules in the GC This flow needs to be higher 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 52 319 Troubleshooting Action Action than zero in order to keep analytes and other contaminants from diffusing back into the pneumatic lines and contaminating the GC system To reduce the dilution effect use the smallest available injector liner 2mm for Split Splitless injector P N N6121002 or zero dilution split injector P N N1011445 and P N N1011446 1 mm for PSS injector P N N6121006 Reduce the split flow in the GC method On PPC instruments this is the flow added to the GC injector by the PPC module alternatively you can use the zero dilution liner NOTE Do not confuse this with the total flow through the split outlet or vent on the GC
144. en Operation Tools Pressing the Tools button opens a pop up menu of tools that enable you to perform various functions such as creating and editing methods and configuring the options available on your instrument Run Status Log I Hi Psi Inject Method Editor Save As Operating Mode Preferences Constant A Calculator Test Env 2 Maintenance p JTemp Timing STANDBY Figure 50 Oven Status Screen Tools Menu Method Editor The Method Editor command opens the Method Editor tab This tab allows you to create and store methods for your application You can store up to 9 methods Once the methods have been saved they can be recalled at any time for use in a sequence or can be recalled for editing The Method Editor tab is similar to the Status tab in appearance See Chapter 5 for details on developing and testing methods Open the File Menu 133 Operation New Method To create a new method open the method editor enter the desired method parameters and then save the method Open To revise an existing method select the Open command from the File menu Select the method that you want to edit and press OK Save Save As Use these commands to save new methods or update existing ones To create a new HS method 1 Open the Method Editor tab and enter or update the desired method parameters 2 Select Save if you are updating an exiting method The Method will be saved with t
145. enance 282 Trap Status Tab 119 Trap Toubleshooting 327 328 Trap Water Adsorption 174 Tray Rotation Feature 151 Troubleshooting Instrument Faults 297 Procedures 307 Sample Carryover 310 Tubing Cleanliness 237 TuboMatrix 40 110 Trap leak test 89 263 Turbo Matrix 40 110 Trap Troubleshooting 320 TurboMatrix 40 110 Trap Installation 81 TurboMatrix 40 110 Trap Accessories 182 TurboMatrix 40 110 Trap Troubleshooting 320 U Unpacking Instrument and Accessories 16 Unrecoverable System Error 297 327 User s Manual 15 V Valve 356 Cylinder 29 Cylinder Protection Cap 28 Vent Time 295 Ventilation 29 Venting Vial Option 116 Vial 175 Checking 175 Decapping 274 Filling 177 Gauge 175 Jammed in Oven Fault 304 Load Failure 302 Load Position Fault 305 Maximum Fill Volume 177 Missing Fault 301 Pressure Gauge 195 Priority 142 Range 105 106 Replacement 337 Safety Information 32 Sealing 176 Shaker Accessory 166 Unload Failure 303 Unload Position Fault 305 Venting Option 116 Vials No First Last Fault 302 Virtual Store 335 Volume Injection 113 197 Maximum for Sample Vials 177 W Warnings Operational 21 Warranty Exclusions and Limitations 336 Waste Disposal 30 274 Water Adsorption Trap 174 Water Trap Option 116 212 Weight Instrument 42 Wide Bore Index Sampling with 226 Z Withdrawal Time 114 198 Zero PPC Module 275 276 295 Zero Dilution Split Injector Liner 168 357
146. ench top P N N6621006 and electronic crimpers P N N9302595 are also available Refer to the PerkinElmer catalogue for more information 176 Accessories Sealing the Hand Crimped Vials NOTE If you are handling hazardous samples you may need to perform the following steps in a fume hood To seal sample vials 1 Place the vial in a vial holder rack N930 1304 The rack is recommended in order to keep vials upright during filling and capping Use a syringe to fill the sample vial with liquid samples Do not fill the vial over the maximum fill volume for liquid samples Observe the maximum filling volume of 15 mL for liquid samples when using 20 mL sample vials Ensure the sample does not come in contact with the top of the vial Load the cap Place the star spring into the cap and then using tweezers or forceps place the seal on top of the spring Push the seal into the cap so that it is flat Place the cap on the vial Crimp Cap Star Spring hw Septum with coated side below eee Sa Sample Vial ma Figure 69 Safety Closure Assembly Place the hand crimper P N N9302785 over the cap When using the hand crimper Place one hand over the stamper to stabilize the crimper on top of the vial Use the other hand to squeeze the crimper Keep the hand crimper level when sealing the cap Release the crimper and check the seal The cap and septum must not be kinked or damaged The safety 177 Accessories closu
147. ent should be cool 3 GC oven injector and detector in the HS analytical column channel should be cool Following the above steps will protect you in case of being busy with the HS TRAP maintenance or troubleshooting and you forget that the GC is still at a high temperature which will damage the column and possibly the transfer line if the carrier gas is cut off Reproducibility Test Headspace Check the reproducibility of the HS sample injection system at regular intervals to ensure the reliability of your analysis results To do this create a method with the system parameters provided below If you have already run this test you simply need to load the saved method 239 Routine Maintenance Run the test mixture ten times and save the results The relative standard deviation for the peak heights or peak areas should be less than or equal to 1 8 Test Column Capillary Column 25 m 0 32 mm I D OV 101 Permaphase DMS 1 um Test Mixture 0 4 v v ethanol in water i e 1 mL ethanol in 250 mL water Test Volume 2 mL test solution GC Parameters Oven Temperature Isothermal 60 C FID Detector Sensitivity High Detector Temperature 200 C Injector Temperature 120 C Carrier Gas Helium Carrier Gas Pressure 100 kPa Split open minus 0 2 min Split Flow 50 mL min Analysis Time 2 5 min Headspace Vial 1 16 1 40 1 110 Parameters Oven
148. eplace only with the same type and rating of fuse WARNING Voltage Fuse Part Number 50 60 Hz 250V rated 100 T 10A M041 7002 120 T 10A M041 7002 220 T5A M041 7038 230 240V T5A M041 7038 Table 5 HS Replacement Fuses 24 Introduction Electromagnetic Compatibility EMC Europe All information concerning EMC standards is in the Declaration of Conformity and these standards may change as the European Union adds new requirements This autosampler has been designed and manufactured having regard to the state of the art to ensure that a the electromagnetic disturbance generated does not exceed the level above which radio and telecommunications equip ment or other equipment cannot operate as intended b it has a level of immunity to the electromagnetic disturbance to be expected in its intended use which allows it to operate without unacceptable degradation of its intended use United States FCC This product is classified as a digital device used exclusively as industrial commercial or medical test equipment It is exempt from the technical standards specified in Part 15 of the FCC rules and Regulations based on Section 15 103 c Use of this product in residential areas may cause interference and such use should be avoided unless special measures are taken by the user to restrict emissions to a level that allows the reception of broadcast emissions CAUTION The TurboMatri
149. er a period of 40 seconds 8 Ifa leak is detected check all of the connections with a helium Leak Hunter or concentrated ethanol and water solution Once you have checked and no leaks are detected then run the leak test again 9 Reduce the carrier pressure to the normal method pressure 10 Because of the sensitivity of the HS trap make sure to trim the column where you plugged the end with a septum Wear gloves when you trim the column 11 Reopen the desorb slide flow path when finished by pulling the brass fitting out If you are leak testing the HS sampling system and it has failed the leak test you should check the following connections first e Headspace O rings in the upper and lower needle sealing 266 Routine Maintenance elements e Transfer line connection to the needle unit e Leak check all nuts around the trap e Be sure the trap is not cracked or broken e Check flow valve connection NOTE During shipping the valves may become loose and start to leak If this happens please go the next procedure HS 40 110 Trap Valve Leak Test HS 40 110 Trap Valve Leak Test CAUTION When you run this test there will be no carrier gas going into the transfer line In case of high flow rates make sure that any hot zones i e the GC oven transfer line are cooled to prevent damage to the instrument NOTE Use this procedure as a diagnostic tool only if you are having problems This leak test is limite
150. er the accessory after your instrument has been delivered a service engineer must install the option Please contact PerkinElmer for further information PPC Programmed Pneumatic Control PPC is the electronic control of pressure for sampling and the GC column The PPC control module regulates pressure using an electronically driven variable flow restrictor The control module also contains pressure transducers to provide feedback for complete monitoring The PPC system is composed of one valve The carrier valve is used to maintain the pressure of the gas through the system The module will be calibrated when the instrument is installed and does not need to be calibrated again See PPC Tab on page 216 for details about setting the sampling pressure The PPC option is installed in the factory If you order the accessory after your instrument has been delivered a service engineer must install the option Please contact PerkinElmer for further information 167 Accessories Composite Zero Dilution Split Injector Liner Description The zero dilution split injector liner is composed of an inner hourglass insert and an outer liner There is a sufficient gap between the outer wall of the insert and the inner wall of the outer liner to allow gas flow between the two The insert is flared at the top to help with the insertion of the fused silica transfer line from the HS The bottom of the insert is beveled to ensure that the insert
151. es 1 16 x 0 5mm 3 09926067 O Ring 0 0145 ID x 0 070 WD 5 B0131410 O Ring Tool Assembly 1 N6701077 Trap Removal Tool Tygon B014 7449 O ring Extract Tool 1 B1511737 Vial Gauge 1 B0500843 Spigot Key for All Systems 1 B0505266 HS Adapter Injector 1 B0510403 HS 40 110 Transfer Line Cover 1 L4271302 Ferrule Trap Tube PTFE 5 M0413401 Users Manual 1 M0415010 Locking Nut 1 M0415330 Top Seal Changing Tool 1 M0417002 Fuse 5x 20mm 10 0A 250V TD 2 M0417030 Terminal Block Plug 1 M0417038 Fuse 5x 20mm 5 0A 250V T 2 N1011206 Cable Assembly for All Systems 2 N6701053 Washer non trap 1 09200061 Wrench 5 8 in 1 18 Introduction Part No Description Qty N6701079 Valco Ferrule Removal Tool Kit 1 N9301357 Empty Fused Silica Tubing 0 32 1 N9301376 Wafer Ceramic Cutter 1 Table 2 HS 40 110 Trap Shipping Kit Part No N670 0116 If any of these items are missing or are damaged please contact PerkinElmer immediately In the event of damage file an immediate claim with the carrier and report the matter to your PerkinElmer office 19 Introduction Symbols Used on the Instrument Indicates alternating current M Indicates the off position of the main power switch Indicates the on position of the main power switch Indicates the Protective Conductor Terminal Indicates Hot Surface Indicates Risk of Electric Shock Indicates an earth ground terminal Caution risk of danger Docume
152. es 243 Removing and Replacing the Needle Headspace Only ee escssceseceseeereeeeceeeeeeeees 243 Removing and Replacing the Needle AS 40 110 Trap Only 245 Cleaning the Jet Needle oo eeeeseceteeeeeeees 246 Changing the Upper Needle Seal Assembly 247 Changing the Lower Seal Assembly 249 Changing the O Rings 0 0 cece eeeeseceneceteeeeeeees 252 Changing the O Ring in the HS 40 110 Trap 253 Converting the HS 40 110 Trap to a TurboMatrix Headspace Mode e ee eseesseeseceseceeeeeeeeeseeaeees 261 Leak Testing the Sample Injection System 0 261 Leak Testing the HS 40 110 Trap 263 HS 40 110 Trap Valve Leak Test ee 267 Magazine Maintenance cece ceeeeseceseceseeeeeeeneenees 269 Removing and Replacing the Magazine 269 Cleaning the Magazine s es 270 Adjusting the Hand Crimper cecceeeeeeseeseenseees 271 Adjusting the Stop Pin eee eee ceneceneeeeeeees 271 Adjusting the Crimp Plunger eee 272 Decapping the Vials 0 0 0 cee eeeesesseceseceeeeeeeeeeeeneees 274 Installing the Transfer Line Cap cece eee eeeereee 275 Zeroing the Carrier Gas PPC Module eee 275 HS 40 110 Trap Maintenance 276 Removing and Replacing the Trap ee 276 Trap Breaks Inside the Trap Assembly 280 Replacing the Dry Purge Assembly 280 Trap Maintenance 00 ees eeceseeeseeesecseeceseeeeeeees 282 Introduction for Conditioning the Trap 282
153. es when you are creating a pressure program e The pressure of the GC injector should not be programmed to a higher value than the HS sampling head pressure e You should disable the PPC alarm in the AutoSystem XL or the Clarus 500 when performing pressure programming for headspace sampling e Pressure flow or velocity programming requires the split flow in the GC method to be set 50 mL min greater than the sum of the column flow GC septum purge flow HS needle vent flow e The split flow is the total flow added to the system by the AutoSystem XL or the Clarus 500 pneumatic module e To calculate the split flow value use the final highest column flow in the flow pressure program The septum purge flow is approximately 3 mL min the HS needle purge flow is approximately 15 mL min when you are using Helium To the sum of these values add 50 mL min to obtain the required split flow to be entered into the GC method e Slow or fast flow programming may require a lesser or greater split flow setting To maintain proper flow programming rates it is important not to have leaks in the system See Leak Testing in the Installation chapter for details on leak testing the HS sampling system During overlapping thermostatting the HS may pressurize a vial before the previous analysis has been completed To ensure that all vials are pressurized to the correct pressure always consider the pressurization time when calculating the GC cycle time f
154. essed NOTE When the Available positions parameter has a indicating that no vials remain scheduled for sampling pressing OK will not rotate the tray back to its original position Creating a Sequence You can use a sequence of methods to analyze a series of vials The options on the Run tab allow you to select a range of vials and then specify a method to analyze the samples You then select the next 153 Operation range of vials and select another method You can also analyze the same range of vials using different methods The sequence can be used on a daily basis or it can be edited as required You will not be able to edit any of these methods if method editing has been disabled from the Preferences tab To create a new sequence 1 Select the Run tab 2 Press the Start vial entry box and then press the plus or minus button to select the desired start vial Next enter the desired end vial 3 From the method drop down box select the method to be used for the selected range of vials 4 Press the Add button to add the entry to the sequence Repeat these steps until you have created the desired sequence To delete an entry from the sequence select the entry in the list and press the Delete button To change the vial range you must add a new entry with the revised vial range and then delete the old entry 6 If you edit the methods called by your sequence the sequence will use the revised methods If you need
155. essure P2 is supplied to the injector but is reduced to Pac as it passes through to the GC column 209 Method Development wy Transfer Transfer Line Line SS Pac ae Poc GC J GC Figure 83 High Pressure Figure 84 High Pressure Standby Pressurization Sampling At the end of the pressurization time the PPC module stops the flow of carrier gas Vapor from the vial headspace expands onto the column due to the pressure drop across the transfer line See Figure 85 Again in direct connect mode this high pressure flows directly through the GC column In the standard HS connection P2 is supplied to the injector but is reduced to Pac as it passes through to the GC column At end of the injection time the solenoid valves V1 and V2 open Carrier gas flows onto the column where separation of the sample takes place Withdrawal aAt the end of the injection time the needle withdraws from the sample vial The system is once again pressurized to P2 In the direct connect configuration high pressure carrier gas continues to flow over the GC column for the duration of the withdrawal time Vial Venting At the end of the withdrawal time the sampling needle is positioned to vent the vial if vial venting is enabled When the sampling needle returns to the standby position the PPC module establishes the original pressure P1 210 Method Development p Transfer Line
156. essure control adjust the pressure regulator until the desired value is displayed on the PPC tab Switch to the PPC tab and enable actual view so that you are viewing the current values rather than the set points See PPC Tab on page 216 5 Ifyou have PPC control enter the desired value on the PPC tab and allow the HS to reach the set point See PPC Tab on page 216 You must also ensure the needle purge flow has been established Splitless Operation In splitless operation the fused silica transfer line is connected directly to GC column inside the GC oven direct connection Alternatively the GC capillary column is brought through the injector and connected directly to the HS sampling head on column connection In this configuration the HS supplies the total carrier gas flow for the HS GC system Set the pressure at the headspace to the correct head pressure your column requires i e 30m 0 25u column 16 psi Splitless operation is necessary for cryofocusing Splitless sampling is less suitable for capillary columns that have a low pressure drop i e 0 53 mm columns Direct Connection In the direct connection configuration the transfer line and the analytical column are directly connected together using a butt connector inside the GC oven Two types of butt connectors are available press fit connectors which can only be used once and standard low dead volume unions which can be reused To set the carrier gas flow for
157. essure in the vial during thermostatting may also be due to the use of a solvent with a boiling point that is too low for the application Ensure that your solvent is suitable for you application You can use the vial pressure gauge P N B0501377 to measure the vial pressure Cause The sample is being absorbed by the septa sealing the sample vial Action Butyl rubber septa P N B0159356 BO159357 318 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 71 Troubleshooting are known to absorb non polar compounds Use PTFE coated septa if your solvent or sample is non polar Cause The septa used to seal the vial is not suitable for the temperature requirements of your application Action Ensure the temperature limit of the septa is within the range required for your analysis see page 179 With respect to the temperature limit of the septa it is important to emphasize that it applies not only to the temperature of the vial but also to the temperature of the instrument s needle used for pressurization and sample transfer which is heated to prevent condensation If for example the vial is at 80 C but the needle is heated to 150 C the hot needle may decompose the septum material resulting in spurious peaks in the chromatogram and a leak around the needle This may also occur with laminated septa where one of the layers may have a lower t
158. ethod Development resonance frequency depends on the sample viscosity and its volume To overcome this problem the frequency scanning shaker varies its frequency automatically during equilibration through a broad frequency range so that each sample in the oven reaches its resonance frequency A shaker is recommended for the determination of non polar volatile organic compounds VOCs in aqueous solutions exceeding a volume of about 3 mL On the other hand shakers do not have much effect on polar compounds in aqueous solutions Equilibration of a solid sample in general but not necessarily always takes longer than the equilibration of a liquid sample and it depends on the structure of the solid and also on the equilibration temperature Long equilibration times are often characteristic of solid samples where the diameter and thickness of solid particles will determine the time of diffusion The porosity and surface area of the solid sample is important and influences the speed of equilibration Therefore some porous solid samples with a high surface area often 1 have surprisingly short equilibration times The activated sample shaker remains in standby and only starts an automatic shaking program when a headspace method that utilizes the shaker is started It is possible to shake some vials and not others using a sequence of methods In MHE mode the optional shaker remains switched off as the needle remains in the vial between a
159. fer line to cool down In the case of direct or on column connections ensure that the flame is out and that your oven injectors and detectors are at 261 Routine Maintenance NOTE room temperature Once the system has cooled switch off the instrument Disconnect the instrument from the electrical supply Undo and remove the chromatographic column at the detector inlet Use a blanking plug to seal the detector column fittings Seal capillary columns with a new clean septum Switch the HS on Open the Temperature tab and reduce the set points to ambient or lower It may be necessary to touch some of the fittings if the leak test fails so set the temperature of the needle and transfer line to ambient or lower If you enter a value of 0 the heaters are shut off 7 8 10 11 12 13 Set the carrier pressure to 45 psi If using a headspace trap close the desorb slide in front of the instrument When the instrument is in the Standby mode open the Tools menu and select Maintenance Then select Leak Test The HS sampling system is now a closed pressurized system The pressure displayed on the PPC tab must not drop by more than 1 psi over a period of 40 seconds If a leak is detected check all of the connections with a helium Leak Hunter or concentrated ethanol and water solution Once you have checked and tightened all of the connections then run the leak test again Reduce the carrier pressure to th
160. from the oven reload your sample vials and then begin operation Setting the Carrier Gas Pressure Once the gas has been connected at the rear of the instrument and you have established a flow of carrier gas through the system you will need to set the carrier gas pressure through the transfer line If you have connected the fused silica transfer line to the GC for splitless injection direct connection or installed the GC capillary column directly to the HS needle unit on column connection then the HS will also supply the GC carrier gas You must establish the column flow as well as set any pressure or flow programs that are required as part of the GC method Split Operation In this configuration you have connected the transfer line to the GC injector The carrier gas pressure that you set at the HS moves the sample from the vial through the transfer line and onto the GC column To set the carrier gas flow for normal operation 1 Connect the transfer line to the GC as outlined in the section Installing the Heated Transfer Line in the Installation chapter 2 Determine the column head pressure This information will be part of the GC method 100 Operation NOTE Set the split vent flow to a typical setting of 25 to 30 ml min 3 Set the HS carrier pressure at 5 to 10 psi higher than the GC column head pressure If the column head pressure is 10 psi then set the HS carrier pressure to 15 20 psi 4 If you have manual pr
161. gazine to dry CAUTION Do not use organic solvents to clean the magazine as it will damage the plastic 270 Routine Maintenance Adjusting the Hand Crimper Adjusting the Stop Pin An adjustable stop pin is located on the lower arm of the hand crimper To adjust the hand crimper 1 Loosen the lock nut to allow adjustment of the pin 2 Ifthe crimper is not crimping firmly enough then shorten the stop pin by tightening it several turns until a satisfactory position is set 3 If the crimper is crimping too tightly then lengthen the pin by loosening it several turns 4 After you make the required adjustment to the crimper seal a few test vials to ensure that the crimper is working correctly NOTE An additional test to confirm good seals is to put several drops of a volatile solvent i e acetone into a vial Seal it and using tongs immerse the vial into a beaker of boiling water If no bubbling is seen around the crimper seal the crimper has been adjusted correctly 5 Finally retighten the lock nut Adjusting Pin m a oa Lock Nut ED J Figure 112 Hand Crimper Locking Nut 271 Routine Ma intenance Adjusting the Crimp Plunger If the stop pin cannot be adjusted further but the hand crimper is still not crimping correctly then you need to alter the position of the crimp plunger To adjust the crimp plunger 1 Crimp Lever Securing Pin
162. gral part of your automatic headspace sampler product It begins with unpacking and general safety information in Chapter 1 Installation and setup are described in Chapter 2 Operation of the instrument is covered in Chapter 3 Optional accessories are described in Chapter 4 and method development is offered in Chapter 5 A routine maintenance schedule and the related procedures are discussed in Chapter 6 Chapter 7 contains lists of possible fault and error messages and some basic troubleshooting procedures If you find an error in this manual or have any comments or suggestions please let us know so that we can correct the mistake or improve the manual Contact information is provided in the Appendix A Conventions in this Manual In the text you will also find various warnings and notes Warnings other cautionary information and notes are denoted in the text as follows This indicates a warning We use the term warning to inform you about situations that could result in personal injury to ourself or other persons WARNING 4 d E CAUTION This indicates a caution note We use the term caution to inform you about situations that could result in serious damage to the instrument or other equipment NOTE The term Note indicates any significant information that can help you avoid false analytical results or deterioration in instrument performance Other Manuals and Reference Material Before you install or use your automat
163. graphic column at the detector inlet or inside the GC oven at the transfer line connection 3 Use a blanking plug to seal the detector column fittings or the transfer line outlet Seal capillary column or the transfer line with a new clean septum 4 Open the Headspace front door and locate the desorb outlet the brass fitting Close the desorb flow by sliding the fitting in to open the fitting slide the fitting out 263 Routine Maintenance Figure 108 5 Set the carrier pressure to 45 psi See Setting the Carrier Gas in the Installation chapter 6 Open the Tools drop down menu and select Maintenance and then select Leak Test If the leak test fails you will get the following screen see the following figure Go to step 8 for the procedure for a failed leak test 264 Routine Maintenance Run Status Log Dry Purge Trap Hold Te st Result Leak Initial Final Pressure Pressure psi psi GasLeak 3316 2391 Tests STANDBY 10 33 35 SA Roe Toos Figure 109 If the leak test passes you will get the following screen see the following figure 265 Routine Maintenance Initial Final Pressure Pressure Tests psi psi GasLeak 34 94 OK STANDBY 09 55 42 _ Start Rotate Tools v Figure 110 7 The HS sampling system is now a closed pressurized system The pressure displayed on the PPC tab must not drop by more than 1 psi ov
164. hat the motor is working too hard Check the needle to ensure it is clean Also check the o ring and the seal assemblies See the section on Changing the Upper Needle Seal Assembly in the Routine Maintenance chapter and Changing the Lower Seal Assembly in the Routine Maintenance chapter Cause The needle seals have not been installed correctly Action The needle seal assemblies have not been aligned correctly and the needle is bending Remove the seal assemblies and ensure they are aligned correctly See Changing the Upper Needle Seal Assembly in the Routine Maintenance chapter and Changing the Lower Seal Assembly in the Routine Maintenance chapter Action An extra seal o ring has been installed in the upper seal assembly Remove the upper seal assembly and ensure that only the lower o ring is installed Cause The needle has not been installed correctly Action Remove the needle and ensure it has been installed correctly See Removing and Replacing the Needle in the Routine Maintenance chapter Cause A mechanical problem has occurred Action Contact your PerkinElmer service engineer Fault Crane Motor Stalled Cause An obstruction has caused the crane to halt Action Turn the HS off and disconnect the power cord from the AC mains Remove the obstruction and reconnect the line cord Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized cor
165. he HS to unload any vials that may be present in the oven The HS will search the outer ring until it locates the empty position To reduce the initialization time leave location 1 empty This is the first location that the instrument will look for the empty position Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses Fault Vial in Unload Position Cause You have placed vials in the unload position of the HS 110 or the HS 40 Action On instruments with the 15 vial oven it is possible to turn the instrument off while vials are still in the oven When the instrument is turned on again it will attempt to unload the oven You must provide an empty spot in the outside ring of the magazine so that the HS can unload the oven When you are loading the HS 40 you can place vials in all positions except for one You must leave one spot open in order for the HS to unload any vials that may be present in the oven When you are loading the HS 110 you must leave the load and unload spots empty You must also leave one further location on the outside ring empty for the HS to unload any 305 Troubleshooting vials that may be present in the oven The HS will search the outer ring until it locates the empty position To reduce the initialization time leave location 1 empty This is the first location that the instrument will loo
166. he column about 2 mm and tighten the column ferrule 12 Establish a flow of carrier gas and leak test your GC connections Operation of the Zero Dilution Liner The liner operates well as the pressure drops across the transfer line A pressure at 0 5 psig or above 2 5 psig is recommended 20ml min The GC split flow should be set to 10 ml min or more Higher flow rates will just waste carrier gas 171 Accessories Cryofocusing Accessory The cryofocusing accessory is available for the HS 110 and HS 40 NOTE The cryofocusing accessory is not available on the HS 16 The HS component of this option is installed in the factory The GC component must be installed on site Refer to the cryofocusing manual for details of installation If you order the accessory after your instrument has been delivered a service engineer must install the option Please contact PerkinElmer for further information Cryofocusing or cold trapping is the technique of sample concentration through the application of low temperature The sample is cooled at the GC column inlet and the volatile components in the headspace are separated from the rest of the unretained gases and hence concentrated The volume of the headspace gas sample can be increased and so the detection limit can be lowered by a factor of up to 50 This is advantageous when you are using capillary columns which can normally only handle small sample volumes in the range of 100 300
167. he magnetic door release to open the door Loosen and remove the knurled needle nut Knurled Needle Nut Needle Holder in Securing Nut Needle Figure 96 Changing the Sampling Needle Lift the needle holder out of the rack Loosen the securing nut and pull the needle out Place the new needle in the needle holder nut The top of the needle will butt up against the bottom of the needle holder Tighten the needle holder nut The nut must be finger tight Clean the needle with a lint free cloth or tissue If necessary dampen the cloth slightly with methanol Carefully slide the needle holder with the new needle back into the rack as far as the stop CAUTION Do not touch the lower half of the needle with your fingers 244 Routine Maintenance 13 Rotate the needle so that the holes line up with the transfer line 14 Securely hand tighten the knurled nut 15 Close the front panels and reconnect the instrument to the electrical supply 16 Turn on the gases 17 Power up the instrument Removing and Replacing the Needle HS 40 110 Trap Only To change or replace the needle see the previous figure 1 Click on the Tools button From the drop down menu select Maintenance and then select Column Isolation Flow This will turn on the column isolation flow and your column will continue to get carrier gas while the needle is changed 2 Pull gently on the magnetic door release to open
168. he same name 3 Select Save As if you are creating a new method Touch the highlighted name field Enter a new name for the method by pressing the name field An alphabetic keypad is displayed Enter the desired name To enter numeric characters press the Num key To enter upper case text press Cap 4 Press Alpha to return to the alphabetic keypad NOTE If aname is already displayed in the name field press the Red Return key to delete the characters 5 Press OK to enter the new name for your method and then press OK to save the method 6 Select Exit Editor from the File menu Activate This command makes the currently selected command active The method is loaded from memory and the instrument is heated or cooled to the new settings Delete Use this command to remove an existing method from memory You can store up to 9 methods If you need to store more methods you must use the PC control software The control software allows you to store a greater number of methods for various applications 134 Operation Exit Editor The Exit command closes the Method Editor and returns you to the default screen Test Maintenance The Maintenance command provides access to the following tests and maintenance support e Leak Test e Valve Leak Test HS 40 110 Trap only e Column Isolate HS 40 110 Trap only These tests and maintenance procedures will be presented and discussed in the Routine Maintenance chapter Th
169. hen filters are included in the supply lines Oxygen filters N930 1179 moisture filters N930 1193 and charcoal filters N930 1192 are recommended for carrier gas lines When these filters are used together they should be installed in the gas line in the following order gas cylinder hydrocarbon filter moisture filter oxygen filter and HS If you use filters from other suppliers refer to the installation notes that are supplied by the manufacturers Gas Supply Specifications Carrier HS carrier gases require a minimum purity of 99 995 Carrier gas with a purity of 99 999 is required if you are using a TurboMass or ECD detector on your GC Pressure differences are minimized when helium is used as a carrier gas 47 Installation Dry Air Dry air or nitrogen is used to drive the pneumatic automation systems on the HS 110 Use medical grade air The purity of the dry air and dry air delivery system is not an issue as this gas does not come into contact with the sample Liquid Nitrogen If the HS is fitted with a cryofocusing accessory it requires a supply of liquid nitrogen The liquid nitrogen does not come into contact with the sample Nitrogen An inert gas such as nitrogen is required as the coolant for the cryofocusing accessory Do not use compressed air as a coolant gas at low temperatures condensation can cause a potentially dangerous enrichment of oxygen The purity of the co
170. here you plugged the end with a septum Wear powderless gloves when you trim the column and reinstall 11 Reopen the desorb flow path by sliding the brass desorb fitting out when finished Make sure when you complete this procedure to reopen the desorb flow path by sliding out the brass desorb fitting WARNING If you are leak testing the TurboMatrix Headspace or the HS 40 110 trap sampling system and it has failed the leak test you should check the following connections first also check the gas leak schematic below e O rings in the upper and lower needle sealing elements e Transfer line connection to the needle unit e Leak check all nuts around the trap e Be sure the trap is not cracked or broken e Check complete flow path and all valve connections NOTE In the following figure no Internal Standard Accessory is 92 Installation installed If your system has an Internal Standard Accessory installed the leak test will be different Vent amp sve wee fo aa 4 v f isolate VALVE STATE TABLE sv8 SV STATE t la Orr 1 orr ou Carrier on Ou eon Figure 31 NOTE During shipping the valves may become loose and start to leak if this happens please go the HS 40 110 Trap Valve Leak Test Procedure in the Operation chapter 93 Installation 94 Operation 3 lt gt Operation Introduction TurboMatrix Headspace and the HS 40 110 Trap Basic operation
171. hes the needle unit in order to protect the fused silica tube connections and to keep the area heated 16 Plug the electrical connector into the receptacle above the retaining collar The connector is polarized so that it will only fit one way Do not force the connection 64 Installation Installing the Heated Transfer Line at the HS Needle Unit HS 40 110 Trap Only To install the heated transfer line at the HS needle unit 1 Cut the white PTFE sleeve that extends from the transfer line so that it is nearly flush with the outer shell of the transfer line Ensure that the sliding insulation tube is in the transfer line Place the electrical connector through the retaining collar Sliding Insulation Lug Cable Guide End PTFE Tubing Plug for Heater Figure 12 The HS End of the Transfer Line Slide the transfer line into the retaining collar so that the top of the tube is flush with the collar Do not tighten the mounting screws as you will need room to install the fused silica tubing The transfer line and the deactivated tube adapter should be in a straight line Remove the cap from the outlet of the deactivated tube adapter Insert the deactivated tube adapter into the nut and ferrule and install these into the fitting of the needle unit Tighten the nut slightly allowing some back and forth movement of the deactivated tube adapter Slide the deactivated tube adapter into the needle unit until i
172. hole chromatographic system leakage may be occurring at the GC connections NOTE Ensure the HS sampling system is leak tight before connecting the transfer line to the GC Refer to the GC manual to leak test the injector and detector connections The following list provides further locations to test the GC connections e The connection of the heated transfer line with the GC injector septum e Column connection at the injector outlet 88 Installation Leak Test the HS 40 110 Trap You must leak test all the connections for the GC as outlined in the above procedure You must also leak test the trap and connections including the manifold column isolation flow connection valves and the connection from the needle to the transfer line nut area for the HS 40 110 Trap to determine that there are no carrier gas leaks 1 Switch off the gas chromatograph Let the instrument cool down 2 Undo and remove the chromatographic column at the detector inlet or inside the GC oven at the transfer line connection 3 Use a blanking plug to seal the column outlet Seal capillary columns with a new clean septum 4 Open the door and locate the desorb outlet the brass fitting as shown in the next photo Close the desorb flow by sliding the fitting in to open the fitting slide the fitting out when the desorb valve is in the valve is off See the following photo 89 Installation Figure 28 5 Set the carrier pressure to
173. ic headspace sampler and in order to get the best results you should be familiar with all the instruments in the system and know how to operate them You must also be aware of the safety procedures that are in effect in your laboratory 15 Introduction Details of gas chromatography are not covered in this manual but a working knowledge of your gas chromatograph and the theory of gas chromatography are required to operate this instrument Refer to the documentation supplied with your GC Some accessories are supplied with separate installation guides and user manuals If you have any of these accessories installed please refer to the associated manual for detailed information on operation troubleshooting and maintenance of the accessory For information on the TurboMatrix Control Software refer to the TurboMatrix HS Control Software User s Guide A list of reference materials covering the theory of headspace chromatography and various applications is provided in this manual Refer to Appendix C Unpacking the Instrument Keep the original packing materials for possible future storage or reshipment Observe the following information when unpacking the instrument 1 Open the carton at the top folding the flaps outward On top of the instrument is a foam insert containing various accessories 2 Lift out the insert and accessories using the hand grips at the side 3 Lift out the instrument 4 Check that all ordered p
174. ide a mechanically stable heated adapter for the transfer line Splitless sampling configurations are generally simple to set up in principle The sample is transferred directly to the GC column or to the HS 40 110 trap Split ratios and GC flow rates are not required Splitless operation is necessary for cryofocusing High pressure sampling can also be used with splitless sampling Splitless sampling is less suitable for capillary columns that have a low pressure drop short and or wide bore Examples of the two methods of splitless sampling are given below In the direct connection configuration the transfer line and the analytical column are directly connected together using a butt connector inside the GC oven For on column sampling the GC capillary column is connected directly to the HS sampling head through the heated transfer line There are however some disadvantages to this sampling method if using this only with headspace Less flow through the sampling area may lead to an increase in sample carry over and thus increased 223 Method Development relative standard deviation RSD and broader peak with small k This is due to less efficient sweeping of the needle area It is also easier to service and troubleshoot since the HS and GC can easily be separated pneumatically to be leak tested separately but plugging the column end This configuration also offers less flexibility if you need do the occasional liquid injectio
175. ill refit the O ring pack into place 13 With the tool pushed in there will be a gap between the housing and the tool With the tool still in place tighten 258 Routine Maintenance the three screws If the tool is not sliding in well you may need to tighten the screws in the front and side of the housing NOTE As you are pushing in the Trap Alignment tool you should feel it move in slowly with only a slight resistance 14 Use the plastic trap removal tool P N N6701077 to reinsert the trap With the trap in the plastic tool slowly twist the tool as you insert it 15 Take the Trap Alignment tool out and use it to push the trap in See the next photo Figure 106 16 Carefully continue pushing in the trap with the Trap Alignment tool Push in until it is about 1 2 mm flush with the front surface See the next photo NOTE If you cannot push in the trap enough to have it 1 2 mm flush with the front surface the trap is not positioned properly You will need to redo this procedure 259 Routine Maintenance Figure 107 17 Tighten the back nut until it stops 18 Return the Trap Alignment tool to its holder on the side of the instrument door 19 Re attach the Dry Purge Assembly and knurled nut 260 Routine Maintenance Converting the HS 40 110 Trap to a TurboMatrix Headspace Mode To convert the HS 40 110 trap to use for a standard headspace see the section later in this chapter HS 40 110 Trap Ma
176. illary B0508598 column HS adapter kit for FISIONS Series 8000 Trace B4000012 2000 HS adapter kit for Thermo Trace N6201030 HS adapter kit for SHIMADZU GC 9Ra 14A B0505889 14B packed columns 17A HS adapter kit for SHIMADZU GC 16 B0508521 HS adapter kit for SHIMADZU GC 14A B B4000033 HS adapter kit for CARLO ERBA VEGA B0506603 MEGA HS adapter kit for GERSTEL CIS B0506539 Table 28 Adapter Kits for Other Gas Chromatographs 340 Appendices Appendix D Reference Material Headspace Gas Chromatography Hachenberg H Schmidt A R Gas Chromatographic Headspace Analysis Heyden amp Son Ltd 1977 Kolb B Auer M Pospisil P Applications of Gas Chromatographic Headspace Analysis Applied Chromatography No 20E PerkinElmer 1978 Kolb B Applied Headspace Gas Chromatography Heyden amp Son Ltd 1980 Kolb B Auer M Pospisil P Multiple Headspace Extraction a Procedure for Quantitative Analysis of Volatile Compounds in Solid Samples Applied Chromatography No 35E PerkinElmer 1981 Kolb B Multiple Headspace Extraction A Procedure for Eliminating the Influence of the Sample Matrix in Quantitative Headspace Gas Chromatography Chromatographia Vol 15 No 9 587 594 1982 Kolb B Pospisil R Applications of Gas Chromatographic Headspace Analysis Applied Chromatography No 33E PerkinElmer 1984 Kolb B Analysis of Food Contaminants by Headspace Gas Chromatog
177. information If you are using the direct or on column connect configuration ensure that the injection time or the injection volume is suitable for the column and does not overload the column Cause The sampling head is contaminated Action Action Increase the flow of carrier gas through the transfer line and set the transfer line temperature to 210 C Allow the transfer line to purge overnight If you are using the on column connect configuration ensure that the column liquid phase can withstand a temperature of 210 C If not then set the transfer line temperature to the maximum allowable temperature for the selected liquid phase If you are observing a severe contamination problem you should disconnect the transfer line from the GC and replace the transfer line If purging does not reduce or eliminate the contamination parts of the sampling head may need to be replaced Contact your PerkinElmer Troubleshooting service engineer Cause The fittings connecting the transfer line to the sampling head have degraded or they are contaminated Action Disconnect the transfer line from the sampling head and replace all the nuts and ferrules Also replace the deactivated tube adapter Reconnect the transfer line to the sampling head as outlined in Installing the Heated Transfer Line at the HS Needle Unit in the Installation and Setup chapter Increase the flow of carrier gas through the transfer line and set the t
178. ing Take care not to damage the o ring seat of the seal assembly Do not touch the new o rings with your fingers Use forceps or tweezers to remove the o ring from its bag and place it on the seal assembly If you touch the o ring for any reason throw it out and use a clean one 5 Place a replacement o ring P N B0198110 into the seal assembly The upper seal assembly contains one o ring on the lower surface The lower seal assembly contains two o rings With the broader flat end of the o ring tool press the o ring into the seat Take care not to damage the o ring or the seat Replace the needle seal assembly See Changing the Upper Needle Seal Assembly on page 247 or Changing the Lower Seal Assembly on page 249 Routine Maintenance Changing the O Ring in the HS 40 110 Trap 1 2 Turn off the instrument Check the conditions in the earlier section Carrier Gas Shut Off then shut off the gas supply Remove the knurled nut and the Dry Purge Assembly See the following photo Using a 5 8 inch wrench loosen the nut in the back by turning it 1 4 to 1 2 turn See the following photo Figure 100 Use the plastic trap removal tool P N N6701077 to remove the trap If you encounter any resistance loosen the nut on the other side some more Twist the plastic removal tool and pull out slowly as you remove the trap Use a philips screw driver to loosen but not remove the three screws shown in the next photo
179. intenance Removing and Replacing the Trap and use the solid end trap P N N6701170 other than the trap that was shipped with the instrument Once you have done this you must go to the touch screen into the Method and change the Operating Mode to Constant CAUTION Once you have converted your HS 40 110 trap to a TurboMatrix Headspace mode do not run the system in Trap mode The plastic retainer will melt at the 400 C temperatures for the trap methods A melted plastic retainer will result in serious damage to the instrument Leak Testing the Sample Injection System If a leak is occurring and you cannot isolate the source it is suggested that you separate the HS from the GC and leak test each instrument separately Once each instrument is leak tight you can then connect them and test them together The automated leak test will leak test the sampling system You must plug the end of the fused silica transfer line or if the fused silica line has been connected directly to the GC column then plug the outlet of the GC column To leak test the sample injection system NOTE If you use a split splitless injector the split and purge outlet must be closed for the leak test If you intend to leak test only the HS remove the fused silica line from the injector and plug the fused silica line with a septum 1 Turn off all heated zones by setting the temperature to 0 Allow approximately 30 minutes for the needle assembly and trans
180. intenance instructions You can check the number of injections that have been made and then adjust the maintenance interval at any time HS 40 110 Trap Status Tab Config Tab The trap can be heated to 400 C without damaging the packing but care must be taken that the analytes do not degrade at the high temperature For example if the halogenated hydrocarbons are present in the sample the temperature should not exceed 325 C When the trap is heated to 325 C trimethyl benzenes are released quantitatively For higher boiling species it may be necessary to use a higher trap temperature This page offers some additional options for the HS 40 110 trap Preferences Run Config Setup Connect Carrier Gas Helium Calibrate Sensors Units psi Inj vol calc flow rate 2 00 ccm Calibrate Oven Trap Setup Internal Standard Number of Injections 160 Maintenance Alarm Reset Counter e a OK Cancel Figure 52 HS 40 110 Trap Status Tab Config Tab 139 Operation Calibrate Oven This button provides direct access to the oven calibration dialog Trap Setup This button allows you to select the trap heating slow or fast rate and a value for the maximum temperature NOTE The speed of Trap temperature rise and the maximum allowable Trap temperature can be selected and set on the Trap Setup Tools gt Preferences gt Config tab gt Trap Setup You can choose either F
181. ion HS 40 110 Trap Only NOTE The Trap is added to the HS in order to offer a pre concentration of almost all the HS vapor produced in the sample vials by the preceding thermostatting Figure 58 is a logic flow diagram that shows the steps in sample preparation up to the Desorption Injection analysis carried out by a Headspace autosampler equipped with a Trap When an HS method is started the first sample vial is loaded into the thermostatting oven 15 position oven up to 12 vials can be loaded simultaneously 1 Vial thermostatting The system starts with the vial thermostatting at a temperature and for a time known to give the largest vapor volume of the compounds of interest 2 Vial Pressurization Next the needle is lowered into the headspace of the vial and the vial is pressurized with carrier gas at a pressure and for a time set in the method Vial Pressure Pressurization Time 3 Pressure Decay With the needle still in the vial the 155 Operation 156 carrier flow to the vial is interrupted Lack of external pressure forces the already pressurized headspace vapor to escape on a reverse flow through the needle then the Trap back to front and vent through the Purge outlet With the Trap cold default 40 C the compounds in the vapor are adsorbed in the Trap The system will repeat steps 2 and 3 Pressurization Pressure Decay for the number of cycles maximum 4 cycles set in the method The cor
182. ion for headspace that is before trap load Timed Events Messages Messages Description No events to delete You tried to delete from an empty timed event list Read only You can t change events during a run Event list is full You can t add events to a full 32 timed event list Duplicate event You can t add an event at the same time as another existing event Event add error An error in adding an event Table 20 Times Events Messages 330 Troubleshooting Instrument Motor Messages Messages Description Pneumatic PSI Too You need shop air for internal standard Low Check air supply for proper delivery pressure Magazine Motor Check for jammed vial otherwise call Stalled PerkinElmer Service Elevator Motor Check for jammed vial otherwise call Stalled PerkinElmer Service Oven Motor Check for jammed vial otherwise call Stalled PerkinElmer Service Needle Motor Check for jammed vial otherwise call Stalled PerkinElmer Service Vial Missing Check for missing vial otherwise call PerkinElmer Service Table 21 Instrument Motor Messages 331 Troubleshooting 332 Appendices 8 lt gt Appendices Appendix A Customer Service Contact PerkinElmer for columns supplies accessories and replacement parts PerkinElmer offers a full selection of high quality chromatography data handling products and gas chromat
183. is not damaged in any way To decap the vials 1 Hold the vial well away from your face Depending on the nature of the sample it may be necessary to decap the vials in a fume hood 2 Grip the cap with the cap removal tool P N N9301270 and twist your wrist 3 The cap will come off easily if it has been crimped correctly If the materials being sampled are hazardous in any way you must treat the collected samples and the vials that contained them as hazardous waste Used vials and seals may contain small amounts of the substances that were analyzed and may thus constitute a chemical or biological hazard Refer to your local safety regulations for proper disposal procedures 274 Routine Maintenance Installing the Transfer Line Cap The transfer line cap is used to protect the fused silica column when the transfer line is not connected to the GC Connect the cap to the transfer line once the heated transfer line has been removed from the GC The cap simply screws into the knurled nut of the transfer line When you connect the transfer line to the GC remove the cap and store it in a safe place away from volatile organic compounds Zeroing the Carrier Gas PPC Module The PPC module must be calibrated when you change the type of carrier gas being used To calibrate the module 1 Open the Tools menu and select Preferences Select the Config tab 2 Use the drop down box to select the type of carrier gas being use
184. itor save your method If you are using the Status tab you must enter all the method parameters and save the new method 9 Run an analysis to test that your devices are connected properly and your events are programmed correctly Example To turn relay 1 on for 1 minute 30 seconds after the current analysis has started you would enter an event time of 30 sec Relay Number 1 and Action would be On You would now enter a second event an event time of 90 sec Relay Number 1 and Action would be Off Accessories The following timing diagram shows various devices being activated during each analysis A device can also be activated for more than one analysis as shown by relay 3 Analysis time 2 00 min NO NC ON ON Start Duration Relay 1 OFF _OFF 0 50 1 00 1 2 3 4 5 6 min ON ON Relay 2 OFF _OFF 0 00 0 05 1 2 3 4 5 6 min ON ON Relay 3 OFF OFF 1 50 1 2 3 4 5 6 min c Cc Cc Cc S S S D 5 D 5 2 2 2 D E Figure 60 Timed Event Diagram NOTE Timed events are not included in the PII calculation BCD Interface The Binary Coded Decimals BCD interface is supplied on the options board The BCD interface is used to transfer the sample vial numbers to an external instrument such as an integrator The BCD interface has two configuration parameters BCD Data Logic and BCD Data Format 165 Accessories BCD Data Logic The BCD interface data channel contact
185. k for the empty position Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses Fault Checksum error to continue press any key Cause An instrument error has been detected during initialization Action A message appears on the display indicating where the error was detected Please take a note of the error message and contact your PerkinElmer service engineer ATTENTION Carrier Gas Shut Off There are cases where you are instructed to either switch off the Headspace or the HS 40 110 trap or and shut off the carrier gas supply to it However in certain cases as e Headspace units with direct or on column connection configurations e In HS 40 110 trap the Isolation Flow You should not switch the HS unit off PPC or the carrier gas supply to it or in an HS TRAP unit the carrier gas should not be shut off as the Isolation Flow that protects the analytical column will be stopped Therefore in cases as above you should not attempt maintenance or troubleshooting in the Headspace or HS 40 110 trap unit unless you have ensured the following in the GC 1 Ifthe detector is a flame one FID NPD etc the flame should be off 2 Ifthe detector is an MS the transfer line if present 306 Troubleshooting should be cool The ion source should be cool 3 GC oven injector and detector in the HS analytica
186. l P Applications of Gas Chromatographic Headspace Analysis Applied Chromatography No 20E PerkinElmer 1978 e Kolb B Applied Headspace Gas Chromatography Heyden amp Son Ltd 1980 e Kolb B Auer M Pospisil P Multiple Headspace Extraction a Procedure for Quantitative Analysis of Volatile Compounds in Solid Samples Applied Chromatography No 35E PerkinElmer 1981 e Kolb B Multiple Headspace Extraction A Procedure for Eliminating the Influence of the Sample Matfix in Quantitative Headspace Gas Chromatography Chromatographia Vol 15 No 9 587 594 1982 e Kolb B Pospisil P Applications of Gas Chromatographic 342 Appendices HeadspaceAnalysis Applied Chromatography No 33E PerkinElmer 1984 Kolb B Analysis of Food Contaminants by Headspace Gas Chromatography in Gilbert J Analysis of Food Contaminants Elsevier Ltd London New York 1984 Kolb B Auer M Pospisil P Quantitative Headspace Analysis of Solid Samples a Classification of Various Sample Types Chromatographia 19 113 1984 Kolb B Headspace Gaschromatographie mit Kapillar Trennsdulen Praktische instrumentelleAnalytik LaborPraxis Vogel Wurzburg 1986 Bibliography Braithwaite A and Smith F J Chromatographic Methods Fifth Edition Glasgow Blackie Academic and Professional an imprint of Chapman and Hall 1996 Kolb Bruno and Ettre Leslie S Static Headspace Gas Chromatography Theory and
187. l column channel should be cool Following the above steps will protect you in case you are busy with the HS TRAP maintenance or troubleshooting and you forget that the GC is still at a high temperature which will damage the column and possibly the transfer line if the carrier gas is cut off Troubleshooting Procedures Problem Leak test failed Cause The needle is coated with abraded sealing material Action Abraded sealing material from the vial septa may stick to the needle and can cause the needle to seal incorrectly during pressurization and withdrawal Clean the needle as outlined in the section on Cleaning the Jet Needle in the Routine Maintenance chapter Ensure that the oven temperature and the needle temperature do not exceed the septa maximum see page 179 Cause The needle has not been installed correctly Action Remove the needle and ensure it has been installed correctly See Removing and Replacing the Needle in the Routine Maintenance chapter Cause The needle seal assemblies have degraded Action Open the upper and lower needle seal assemblies and replace the o rings Check the seals for signs of wear Replace them if necessary See Changing the O Rings in the Routine Maintenance chapter Cause The transfer line has not been installed correctly at the needle or at the GC injector Action Check the connections at the sampling unit and ensure all nuts and ferrules have been installed correctly Do not
188. laced as described in Installing the Heated Transfer Line in the Installation and Setup Chapter 1 A Braithwaite and F J Smith Chromatographic Methods Fifth Edition Glasgow 1996 p27 309 Troubleshooting Cause A poor connection between the transfer line and the analytical column can cause peak broadening Action Ensure that the connecting ends of the column and the transfer line should be cut cleanly using a wafer silica cutting tool See Figure 10 in the Installation chapter of this manual Action The union or connector assembly should be an inert zero dead volume fitting recommended for butt connected capillary fused silica tubing Action If you are using the zero dilution liner ensure that it has been installed correctly See Installing the Zero Dilution Liner in the Accessories chapter It is possible that during installation of the liner pieces of fused silica have broken off the transfer line and dropped into the injector Clean the injector as necessary Cause Activity of the analytical column itself can cause band broadening Action Replace the GC capillary column with one that is more closely suited to your application Refer to the GC manual for instructions Cause The sample has overloaded the GC column Action Use split sampling to reduce the sample volume sample that reaches the GC column Adjust the injected split flow to deliver the correct sample volume onto the GC column Samp
189. lapping thermostatting if you have the 15 vial oven option installed on the HS 40 110 only 196 Method Development Analysis Time J fai Nh pe WAM Thermostatting Time Sample 1 Sample Injection iit r Sample 2 IMIN JAW k Sample 3 iT min NAMA AMN JWL kl L Sample 4 gt Pll Figure 75 Overlapping Thermostatting NOTE In special cases you may need to work under non equilibrium conditions You can set this value to 0 0 to 9 9 min in steps of 0 1 min 10 to 99 min in steps of 1 min and 100 to 990 min in steps of 10 min If you are using MHE mode Headspace only set the thermostatting time so that it is equal to the GC cycle time Injection Volume Headspace Only The injection volume uL is based on the column flow rate and the injection time It corresponds to the flow rate measured at the end of the column under normal atmospheric pressure and temperature conditions The calculation of the injection time for the entered volume is based on the assumption that the vial pressure remains constant during sampling and no other gas is supplied to the column This parameter defines the sample injection volume Valid range 0 to 99 uL 100 to 990 1000 to 10000 uL in steps of 1 10 and 100 uL 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 Perkinelmer P N N1011210 p 118 197 Method Development
190. ld be greater than 80 kPa If chromatographic conditions demand a column pressure of 90 kPa the above criterion is met 90 gt 80 The scale below shows the relationship between vial pressure and thermostatting temperature in samples with a water matrix Vial pressure in samples with water matrix 0 20 40 60 80 100 120 kPa 3 psi 6 psi 9 psi 12 psi 15 psi 17 psi 4050 60 70 80 85 90 95 100 110 C Thermostatting temperature Figure 74 Relationship Between Vial Pressure and Thermostatting Temperature in Samples with a Water Matrix Injection Time Headspace Only The carrier gas supply line and the pressurized gas in the vial expand onto the column resulting in a flow of the headspace gas from the vial to the column Since both the pressure in the vial and the transfer time can be set the transferred volume of the headspace gas can be accurately controlled A separate gas supply is not required for pressurization the vial is pressurized to the carrier inlet pressure The sample injection time can be set to any value from 0 00 to 9 9 min in steps of 0 01min and 0 1 min The value that you set will depend on your application You may need to determine the actual setting experimentally using known standards 195 Method Development Thermostatting Time Headspace and HS 40 110 Trap The time needed for equilibration depends on the diffusion of the volatile sample components from the sample and then back into the
191. le Carryover Sample carry over is rare in HS and may be avoided with proper care and maintenance of you instrument Contamination can also be avoided by ensuring that your method is suitable for the compounds that you are analyzing Cause The needle or the transfer line is not hot enough and the sample is condensing Action Set the temperature of the needle and the transfer line to at least 10 C higher than the vial oven 310 Troubleshooting Cause The needle purge flow is below the acceptable range Action Check the needle purge flow and ensure the flow rate at the purge vent is between 10 20 mL min If the flow is below 10 or greater than 20 mL min contact your PerkinElmer service engineer Cause The GC injector is not being flushed completely Action In split sampling carrier gas continuously purges the split splitless injector to avoid back diffusion and sample carryover When operating with PPC control a minimum flow of approximately 2 mL min split flow should be supplied by the GC s pneumatic modules to purge the GC carrier gas lines Keeping this flow smaller than the septum purge flow ensures that no dilution of the injected headspace sample takes place in the injector A higher flow from the GC pneumatics can be applied to dilute the injected sample if necessary Cause If your are using the direct connect configuration or an on column connection and the injection time or the injection volume is too
192. lems During the Trap Clean and the following procedure of Trap Test to check if the trap is actually clean no sample vial is involved The GC is also involved and a run is started only in Trap Test Before attempting a Trap Clean or Trap Test ensure that e There is adequate flow of carrier gas through the trap before a Trap heating cycle begins First in the Option tab choose Trap Clean from the Operating Mode drop down menu Then with a flowmeter check flows at the Needle Purge outlet 12 18ml min and the Trap Dry Purge outlet 47 53ml min If not correct re adjust e Before starting the Trap Test ensure that the GC has the proper GC method loaded and is READY Cleaning the Trap The Trap Clean option allows you to clean the trap See Figure 121 CAUTION Be sure to stay below the minimum operating temperature of your installed trap adsorbent material NOTE The GC is not involved during the Trap Cleaning 1 Inthe HS screen select the Option tab 2 To condition the trap in the Option tab select Trap Clean from the Operating Mode drop down menu 3 Also you can carry out the trap clean operation from the Method Editor In the Method Editor screen select the Option tab 4 Inthe Status page select the Temp button and set the trap Temperature to 280 C or higher if required 282 Routine Maintenance 5 Select the Timing button on this Status page and set the Trap Hold time to 30 min or l
193. marks of E I duPont de Nemours and Company Inc Contents Contents TAT EOCUICTOM ies sisescrsccnstevadastdacnabaianndewsacadiadenmns 11 Introduction scenar aaeeea tes 13 TurboMatrix Headspace cee eseeseeseceseeseeeneeees 13 HS40 110 Trap since sete aaneen 14 About this Manual 0 00 eeesseceseeeeceseeeeeeaeceeeeeeeees 15 Unpacking the Instrument cee eeeeeeeeeseeeneeeeeeees 16 Symbols Used on the Instrument eee eee eeeeeeee 20 Safety Information 0 0 eeeeseeseeseceseceseeeeeeaeenseeees 20 Electrical Safety csi cccdecssehledcte dete dibtoeel lets cee ese 22 Electromagnetic Compatibility EMC 0 0 25 Mechanical Hazard 25 Chemicals ereere nie iin TE EE ARE 26 Compressed GaSe Srini eoin ios 27 Extreme Temperatures seseseeeseeseeesrrsressrerersserese 29 Waste Disposal meriiri nont 30 WEEE Instructions for PerkinElmer Products 31 Sample Vials eee eicetadea Senate Bae 32 Cleaning and Decontamination ce eeeeseeneeeeeeees 33 Decontamination 0 0 0 eeeeeeesseeseeeseceseeeeeeaeeeseeees 33 Cleaning the Instrument 0 0 0 eee ceeeeeeeeeeeeneeees 34 Installation ss scnieienecsnzedecchocoseaeisennisnencseecdeieretnene 35 Introd licttonissits ic iseisctt eneren cette pee taltethaleteat 37 Pre Installation Checklist 38 Laboratory Requirements 0 0 0 eeceseeeeeeeeeeseeeeeeeeeees 40 Operating Environment cee eeeseceseceeeeeeeees 40 Space Requirements for the Instrument 41 El
194. mension Function Carr In 1 8 stainless steel compression fitting Carrier gas moves the sample through the system The carrier gas connected to the HS also supplies the GC Maximum delivery pressure is 100 psig 690 kPa 90 620 kPa psig is recommended Dry Air 1 8 brass compression fitting Dry air is to drive the automated vial handling components on the HS 110 and HS 40 110 trap Maximum delivery pressure is 100 psig 690 kPa 90 620 kPa psig is recommended Cryo In Cryofocusing Inlet Maximum delivery pressure is 100 psig 690 kPa 90 620 kPa psig is recommended Cryo Out Water Trap Cryofocusing Outlet Carrier Gas for the Water Trap accessory 78 Table 10 HS Gas Connections Installation HS 40 110 Trap Connections The HS 40 110 trap may require three gas connections attach the catrier gas any gas internal standard and the dry air supply The following table shows the required gases for the HS 40 110 trap See the following photograph of the back of the instrument to find the location of the separate gas hook ups TRAP Model Gases Remarks and Options TurboMatrix 40 Trap He or N2 Carrier Gas TurboMatrix 40 Trap 1 He or N2 1 Carrier Gas and Int Std IS 2 Dry Air 2 for the air Actuator of IS valve TurboMatrix 110 1 He or N2 1 Carrier Gas Trap w or w o Int 2 Dry Air 2 and or Std IS crane IS NOTE It is
195. ment 193 Nitrogen Supply 48 Principles 172 Temperature 193 Time 114 Time Pre 205 Time Pre Post 204 Timing Diagram 173 Water Adsorption Trap 174 Customer Service 335 Cylinder Safety Practices 28 Storage 28 Valve Protection Cap 28 D Data BCD Logic 166 Date Setting 147 Date Setting 147 Decapping Vials 274 Delete Method 134 Description Cryofocusing 172 Headspace Analysis 185 High Pressure Sampling 208 Dimensions Instrument 41 Direct Connection 101 224 Display Brightenss 146 Language Options 146 Touch Screen 103 Troubleshooting 309 Double Injections 195 Dry Air Index Connection 77 Delivery Pressure 77 Inlet Port 78 Specifications 48 E ECD Requirements 75 Economy Mode 144 295 Electrical Protection 22 Surge 45 Elevator Crane Stalled Fault 300 Motor Stalled Fault 298 Needle Stalled Fault 299 Oven Stalled Fault 298 Emulation HS 40 138 Equilibration Status Message 295 Time 196 Error Unrecoverable 297 327 Error Condition 295 Event Programming Timed 163 Timed Relays 54 Event Relays Show 138 Exit Method Editor 135 External Devices 163 Extreme Temperatures 29 F Fault Carrier Pressure Too Low 297 Checksum 306 Conditions 297 Crane Motor Stalled 300 Elevator Motor Stalled 298 Magazine Full 303 Magazine Motor Stalled 298 Needle Motor Stalled 299 No Vials in First Last 302 347 Index Oven Motor Stalled 298 Pneumatic Pressure Too Low 297 Sensor Failure 301 Vial in Load Position 305 Vial
196. mination Seals are available in four types Your choice of seal will depend upon your application See Sample Vials and Seals on page 337 for part numbers NOTE Do not exceed the maximum septa temperature when thermostatting samples NOTE The sample needle temperature can not exceed the maximum temperature of the septa Butyl Rubber Septa for temperatures up to a maximum of 100 C very weak interference peaks with FID low permeability PTFE Coated Butyl Rubber Septa for temperatures up to a maximum of 100 C very weak interference peaks with FID lowest permeability Aluminum Coated Silicone Septa for temperatures up to a maximum of 120 C very weak interference peaks with FID very low permeability 179 Accessories NOTE Do not use the aluminum coated silicone septa for needle temperatures exceeding 120 C PTFE Coated Silicone Septa for temperatures up to a maximum of 210 C weak interference peaks with FID very low permeability Headspace Control Software The Control Software is designed to run under Microsoft Windows The software provides the means to operate the instrument though a PC You can also create methods and sequences and log information about the status of the HS The Control Software runs in combination with TotalChrom It is easy to install and use and allows you to e Control your HS e Create and test new headspace methods e Create sequences based on stored methods e View g
197. minimum possible number of joints for carrier gas lines If necessary pass a stream of clean inert gas through the tubing while baking it in an oven at a temperature high enough to remove any trace organic solvents Never clean the tubing or fittings with organic solvents Use compression fittings to make tubing connections Do not use soldered joints Carrier Gas Carrier gas can be a major source of contamination Contamination can originate from the gas itself or from the tubing used to deliver the gas Use only carrier gases with a purity of 99 995 or better Only top quality gases are suitable typical laboratory supplies are usually not pure enough Gas purity can be improved when filters are included in supply lines Hydrocarbon oxygen and moisture filters are recommended for carrier gas lines When oxygen filters and moisture filters are used together install them in the gas line in the following order gas cylinder hydrocarbon 75 Installation filter moisture filter oxygen filter and HS This sequence prevents any hydrocarbons present in the gas stream from reaching the oxygen filter To minimize carrier gas impurities and reduce instrument contamination we recommended installing a charcoal filter in the carrier gas line close to the inlet of the HS Most filters are disposable Replace them when a new cylinder is installed or as soon as contamination is suspected m lt H
198. mpling time and no other gas is supplied to the column This would be the case with a direct connection or splitless configuration GC Cycle Time The GC cycle time is the minimum time between a sample injection and the time at which the GC is ready for the next injection This time will be determined from the GC analysis time and the time required to return the GC to its ready state The Cycle Time value must be greater than or equal to the GC run time plus the GC oven equilibration time and the GC oven cool down time The HS will use this value to calculate when to begin the thermostatting time If you are running an HS 40 or an HS 110 the cycle time will be used to determine at which time the vials should be loaded into the oven in order to run vials successively without wasted time in between injections For normal Headspace applications the cycle time is short but with Trap operation the cycle time is much longer Make certain to enter a longer cycle time when using a trap otherwise you will see an apparent block on entering the GC cycle time 113 Operation The cycle time can be set to any value between 0 1 and 999 minutes The default time is 5 minutes NOTE Laboratory temperatures can strongly influence the GC oven cool down time and can vary The GC cycle time setting should take into account the longest oven cool down time expected during the analytical sequence Withdrawal Time Headspace only The length of time after
199. n The New Method tab opens The New Method tab is identical to the Status tab It contains four tabs that will allow you to set up various analysis parameters For a Headspace only unit Press the Timing tab Enter values for the Pressurization time the Inject time the Withdrawal time Headspace only and the Cycle time Headspace Trap A PII time will be calculated after you have entered values for each parameter If the cryofocusing option Headspace is installed enter the pre cryofocusing time and the post cryofocusing times Headspace only On the Temperature tab press the Needle box to activate the option and then press the Plus or Minus keys to enter the desired value Enter the Transfer Line and thermostatting temperatures in the same manner If the cryofocusing option Headspace is installed enter the cryofocusing temperature Headspace only See Cryofocusing Temperature Headspace Only on page 193 for details Press the Options tab and enable any options that are required to complete your method Select the desired operating mode If you are using MHE mode you must set certain parameters accordingly See MHE Theory and Calculations Headspace Only on page 229 for details If you have PPC installed press the PPC tab and Carrier pressure If you are using high pressure injections enter the desired value for this option A default method name is entered You can change the method name by pressing the default name
200. n performing a leak test Slide the transfer line down so that the PTFE sleeve is within 1 2 mm of the sleeve nut and then tighten the mounting screws on the collar Pull the sliding insulation tube from the transfer line all the way down so that it touches the needle unit in order to protect the fused silica tube connections and to keep the area heated Plug the electrical connector into the receptacle below the retaining collar The connector is polarized so that it will only fit one way Do not force the connection 73 Composite Zero Dilution Split Injector Liner for Headspace Interfacing Installation Instructions 1 Operation 1 Cool the oven and injector Remove the column and the existing injector liner Check the outer and inner liner components of the composite liner for contamination or damage and replace as necessary Insert the inner liner into the outer liner Install the composite liner into the injector using a standard O ring The inner liner should be upper most The outer liner should be pushed fully into the injector Replace the injector head and secure with the spanner Thread a length of 0 32 mm i d deactivated fused silica tubing through the transfer line and attach to the HS sampling head The other end of the tubing should be thread through the septum in the HS septum nut Cut the tubing so that 62 mm is left protruding from the septum 57 mm from the edge of the septum nut this length
201. n a visit by a PerkinElmer service engineer the visit will not be covered by the instrument warranty Also excluded from your instrument warranty agreement is damaged caused by e corrosion by the sample e overheating of the sample causing blockage of tubing e undue stress on parts constructed of glass lined stainless steel tubing deactivated tube Failure to observe the precautions described in this manual will not be covered by the warranty 336 Appendix C Appendices Supplies Accessories and Replacement Parts Sample Vials and Seals The safety closures consists of a crimp cap a star spring and a septum See Sample Vials on page 175 for details Headspace Vial 20 mm clear vials approximately 22 mL Caps and septa are not included Box of 1000 crimped top sample vials Box of 1000 screw top sample vials B0104236 N9306078 Butyl Rubber Septa for temperatures up to a maximum of 100 C very weak interference peaks with FID low permeability Pack of 100 Seals B0159356 Pack of 1000 Seals B0159357 PTFE Coated Butyl Rubber Septa Red for temperatures up to a maximum of 100 C very weak interference peaks with FID lowest permeability Pack of 100 Seals B0104239 Pack of 1000 Seals B0104240 Pack of 1000 Seals pre assembled ready to use B4000025 Aluminum Coated Silicone Septa for temperatures up to a maximum of 120 C very weak interference peaks
202. n progress Dry Purging The trap is being purged with helium Economy Mode The instrument is in the economy mode The heaters have been switched off and the carrier gas flow has been reduced to the minimum Fatal Error A fatal error is a malfunction from which the instrument cannot recover without user intervention The instrument may need to be switched off and then turned on again If the fatal error reoccurs you will need to contact your PerkinElmer Service Representative Ready The instrument is ready to begin an analysis Fault A fault is occurring Trap Cond Heat The instrument is in trap condition mode and the trap is being heated to the set point Trap Cond Hold The instrument is in trap condition mode and the trap is being held at the set temperature Trap Heat The trap is being heated to its high temperature Trap Hold The trap is being held at its high temperature Waiting for GC The HS 40 110 trap is waiting for a GC ready signal before the cold trap is heated Table 15 Instrument Status Messages 328 Troubleshooting Status Error Messages Error Messages Description Slow pressure decay vial x Vial pressure decayed more slowly than expected sample volume Fast pressure decay Vial pressure decayed more quickly than vial x expected a leaky septum Bad pressure decay Vial pressure decayed in an inappropriate vial x fashion but it is hard to qualify Table 16 Tur
203. n tab The methods and desired vial range will be displayed Press Stop then rotate the magazine to gain access to the vial location and insert a sample vial Press the Start button on the display to start analyses Cause Your method specifies multiple analyses on a vial and you have removed the specified vial after the first analysis was started Action Press Stop and then place the vial into the HS Press Start to resume your analysis 301 Troubleshooting Cause If there has been a power failure it is possible that a vial has been dropped by the crane arm Action Action Turn the instrument off and disconnect the power cord from the AC mains Remove the vial and replace it in the magazine If the vial has fallen into the instrument contact your PerkinElmer service engineer Fault No Vials in First and or Last Positions Cause The first and or last vials from the specified range have not been placed on the magazine Action Action Press Stop and rotate the magazine to gain access to the vial location and insert a sample vial and clear the fault Press the Start button on the display to start the analyses Press Stop Open the Run tab and adjust the vial range so that only vials that have already been placed on the magazine are included in the vial range Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the anal
204. nalyses PPC Tab Programmed Pneumatic Control PPC is the electronic control of pressures for inlet and auxiliary gases The PPC module is standard in the Headspace with Trap version The PPC control modules regulate pressures using electronically 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 121 123 216 Method Development driven variable flow restrictor The control modules also contain pressure transducers to provide feedback for complete monitoring A PPC controller board drives the variable restrictors on the control modules by comparing actual pressures with set points determined from user entered values You can set the carrier gas pressure from the PPC tab a Headspace only version Carrier Pressure Set the pressure required for the GC column and the analysis temperature program You will set the carrier pressure on this tab even if the PPC module is not installed on your instrument There are a number of considerations when you are setting the carrier gas pressure If you have connected the HS at the GC injector and you are using split injection then the carrier must be set so that the HS carrier pressure is approximately 5 psig higher than the GC column head pressure b Headspace Trap version Column Set the pressure required for the GC column and the analysis temperature program Set also Vial pressurization and Desorb pressu
205. nalyzed the thermostatting time and the injection time plus the status of the run are displayed If the sequence has been completed then the time at which it was completed is also displayed 130 Operation Run Status Log _jLog Report Oven Status Estimated Run Time 22112 STANDBY 10 29 11 Start Rotate Tools w Figure 48 Oven Status Tab The information is overwritten when a new sequence is started Decay HS40 110 Trap only If you set up your pressure decay properly the time for the complete headspace vapor to be decayed out of the vial on to the trap and the pressure in the vial is not consistent with your setup an error message will be generated and displayed in this log provided that the Monitor Vial Integrity is chosen For example in the next screen is a fast pressure decay for vial 15 There could also be a slow pressure decay for the vial that decays slower than the set decay time 131 Run Status Log Log Repor Oven Status Runt acy oul 9 Anns N9523 Instrument Serial HS00000000000 Instrument Mame heather Method default Vial Thermo Inject Status Pressure decay OK vial 13 13 09 53 34 09 55 34 Done Extended Therm Trap Nul Ready Pressure decay OK vial 14 14 09 56 17 09 59 34 xThermo Extended Therm Trap Not Ready Fast pressure decay vial 15 15 10 00 12 10 03 34 xTherma Run Stopped STANDBY Ea VE ESE Roe Too Figure 49 Pressure Decay Log Scre
206. nd enable the High Pressure Injection option A check mark must appear in the box Open the PPC tab and press the injection pressure to enable it Use the and keys to enter the desired value Problem Cannot enter pre and post cryofocusing times on the Timing tab Cause The cryofocusing accessory is not enabled on the Options tab Action Switch to the option tab and enable the cryofocusing option A check mark must appear in the box Open the Timing tab and press the pre cryofocusing to enable it Use the and keys to enter the desired value Peak Broadening or Splitting The chromatographic peaks represent the distribution of molecules in a band as it elutes from the column the overall broadness being conveniently measured in terms of the width of the peak A number of independent factors such as temperature and column retention processes contribute to the dispersion of molecules in a band and band broadening Classical chromatography theory considers that the separation process takes place by a succession of equilibrium steps the more steps in a column the greater the column efficiency with less band broadening occurring Peak broadening and splitting are undesirable and can lead to inaccurate quantitation or misidentification Cause Activity in the transfer line can cause peak broadening Action If this occurs the section of capillary column or the deactivated fused silica in the transfer line should be rep
207. nect them from the line power supply before you alter or make any new electrical connections WARNING 43 Installation Installation Category This instrument is able to withstand transient over voltage according to Installation Category II as defined in IEC 1010 1 Power Consumption Approximately 1000 watts for the HS the AutoSystem XL Clarus 500 GC will consume 2400 watts Add 250 W for the computer and 100 W for a printer Power Specifications All electrical supplies must be smooth and free of transients greater than 40 volts peak to peak and must meet and remain within the following tolerances HS 100V 10 50 60 Hz 41 8 A 120V 10 50 60 Hz 41 8A 220V 10 50 60 Hz 1 4 A 230 240V 410 50 60 Hz 1 4A Auto 120 VAC 10 50 60 Hz 1 System 230 VAC 10 50 60 Hz 1 Power Outlets HS A minimum of one dedicated 120 VAC outlet at 15 amps or a 230 V outlet at 6 amps Auto A minimum requirement of one System dedicated 120 VAC outlet at 20 A or or one 230 VAC outlet at 10 A or Clarus greater 400 500 or 600 Table 8 Power Requirements Additional equipment such as computers and printers should be connected as per their specifications Instruments and peripherals should not be connected to or near circuits with large inductive or large and variable loads i e large motors discharge lamps photocopy systems radio transmitters etc
208. ng If you heat the trap to high temperatures take care that the analytes do not degrade at these high temperature For example if the halogenated hydrocarbons are present in the sample the temperature should not exceed 325 C When the trap is heated to 325 C trimethyl benzenes are released quantitatively For higher boiling species it may be necessary to use a higher trap temperature Trap Breaks Inside the Trap Assembly If the trap breaks inside the trap assembly you will need to contact your PerkinElmer Service engineer Replacing the Dry Purge Assembly If you have noticed that the Dry Purge Assembly has been damaged you will need to replace it before you return it to the trap assembly 1 Take the new dry purge assembly P N N6700112 out of its packing 2 The dry purge assembly has two stainless steel lines which must be attached to the instrument correctly 280 Routine Maintenance The longer stainless steel line goes to the bottom compression fitting to the trap vent See the following photo The shorter stainless steel line goes to the upper compression fitting to the V9 valve See the following photo e T b A r A u 2 Cj 1 d di i Upper Line Lower Line Figure 120 281 Routine Maintenance Trap Maintenance Introduction for Conditioning the Trap You will need to condition the trap if you have just installed a new trap or if you are encountering carry over prob
209. ng Pre Injection 222 Time 113 Volume 113 197 Injector GC Adapter 68 Packed Column 227 Input Signal Ready In 53 Start In 54 Stop In 54 Input Signals RS 232 54 Input Output Port 49 Installation by a Service Engineer 37 by Experienced User 37 Carrier Gas Filters 75 Checklist 37 Direct Connection 71 GC Connections 46 49 HS 37 HS to Any GC 56 HS to AutoSystem XL GC 55 HS to HP6890 GC 57 On Column Connection 72 Pre installation Checklist 38 Transfer Line 58 Transfer Line at GC 68 Transfer Line Cap 275 Transfer Line Needle Unit 62 65 Tubing Requirements 75 Instrument Conditions 297 Contamination 312 Index Dimensions 41 Input Signals 53 Introduction 13 Layout 98 Operation 97 Output Signals 51 Safety Information 21 Shutdown 160 Storage 40 Unpacking 16 Weight 42 Interface Binary Coded Decimal BCD 165 Input Output 49 Touch Screen 103 Interference Earth Loops 45 Introduction Headspace Analysis 185 User s Manual 13 J Jet Needle Cleaning 246 Llower Seal 249 Replacing 243 245 Types 243 Upper Seal 247 K Key Clicks 145 L Laboratory Carrier Gas Cleanliness 237 Cleanliness 236 Environment 40 Safety 27 Language Options 146 Layout Touch Screen Interface 103 Layout Instrument 98 Leak Test 135 349 Index Failed 307 Sampling System 86 261 Leak Test Time 295 Leak Testing 86 Line Cord Connector 241 Liner Zero Dilution 168 Liquid Nitrogen Extreme Temperatures 29 Supply 48 Log Tab Log Repor
210. ng the cryofocusing system should be used as a guideline for the pre cryofocusing time in the headspace method The total cryofocusing time comprises the pre before and during sample injection focus time inject time and post after injection cryofocusing times The pre cryofocusing time must be sufficiently longer to ensure that the headspace has reached the required low temperature before an injection begins Typically this would be at least two minutes before the injection time begins depending on the pressure flow of the cooling gas During the pre cryofocusing time the GC oven should be less than 45 C to ensure adequate cooling of the trap The pre cryofocusing time can be measured using the Cryo Test on the Test and Diagnostics option on the Tools menu To establish the pre cryofocusing time 1 Enable the Cryofocusing option and water trap if it is installed on the Options tab NOTE Check that the GC is cooled and in the ready state 2 On the Temperature tab enter the desired cryo temperature This is the temperature the head of the column will be cooled to 3 Select the Tools menu and then select Test On the pop up menu select Cryo Test 4 Press OK to begin the test The HS begins to cool the head of the column It also begins to measure the time until the set temperature has been reached 5 Once the set temperature has been reached the test is stopped The displayed time is the pre cryofocusing time
211. normally be very short however it should be at least equal to the injection time withdrawal time You can set this value to 0 0 to 9 9 min in steps of 0 1 min or 10 to 99 min in steps of 1 minute The time taken for chromatography of the sample is determined by the GC method You must enter a value for the GC Cycle Time into the HS The Option Tab The Options tab provides access to the headspace method options There are some options that you may need for some methods but may not need for others You can enable vial venting the shaker cryofocusing and high pressure injection from this tab In the case of the headspace trap instrument add IS internal standard outlet split and dry purge The high pressure injection option is only available if you have the PPC option installed The cryofocusing option is only available if it has been installed on both the HS and the GC column oven 206 Method Development You also select the operating mode and the injection mode from this tab Injection Mode Headspace Only The volume of the injected sample can be entered as an injection Time or an injection Volume The injection volume uL is based on your entry for the column flow rate The injection volume corresponds to the flow rate measured at the end of the column under normal atmospheric pressure and temperature conditions for Headspace only if you select injection volume as your mode of injection specify the column flow rate
212. ns a pressurization period of 1 3 minutes is recommended The pressurization time needs to be long enough to ensure homogeneity of the gas phase in the vial The pressurization time should be at least two minutes for good reproducibility and three minutes for optimum reproducibility For some applications where a short pressurization time is used to increase productivity expect deterioration in performance Vial Pressurization Carrier Pressure Headspace Only In order to obtain good reproducibility it is important that the column head pressure be greater than the pressure in the sample vial At the beginning of the pressurization phase when the needle moves down into the vial pressure is released Part of the pressure built up between the injection port and the column head is released to the atmosphere through the hole located laterally at the lower part of the needle Thus if the difference in pressure between column head and vial is too small part of the sample in the vial headspace will be 194 Method Development taken up in the carrier gas flow prior to the actual injection resulting in an undesirable double injection In order to prevent such double injections the column head pressure should be greater than the vial pressure Carrier Pressure in PPC tab at the preselected thermostatting temperature by at least a factor of 1 2 20 kPa 100 kPa 1 bar Example At a vial pressure of 50 kPa the column head pressure shou
213. ns to the GC injector The column must be disconnected from the HS sampling head before and the GC column re connected to the injector Direct Connection In the direct connection configuration the transfer line and the analytical column are directly connected together using a butt connector inside the GC oven Two types of butt connectors are available press fit connectors which can only be used once and standard low dead volume unions which can be reused Transfer Line ea Injector Column Connector Figure 93 Splitless Sampling Direct Connection On Column Connection To perform on column sampling a 0 25 mm i d or 0 32 mm i d capillary column can be connected directly to the HS needle area Approximately 1 5 m of the capillary column is unwound from its holding cage and inserted from the GC oven directly up through the GC injector and heated transfer line to the HS needle area During operation the temperature of the heated transfer line should not be allowed to exceed the maximum recommended temperature for the column stationary phase 224 Method Development Splitless Sampling with the HS 40 110 Trap HS 40 110 Trap Theory The HS 40 110 trap uses a focusing trap Pulsed Headspace Extraction or Trap as its sampling operating mode This approach uses a single or user specified number of pressurization and Trap Load steps to extract a high percentage of the headspace from the s
214. nsfer line to the sampling head have degraded and are leaking Action Disconnect the transfer line from the sampling head and replace all the nuts and ferrules Also replace the deactivated tube adapter Reconnect the transfer line and the sampling head as outlined in nstalling the Heated Transfer Line at the HS Needle Unit in the Installation chapter Increase the flow of carrier gas through the transfer line and set the transfer line temperature to 210 C Allow the transfer line to purge overnight Cause There is leak in the sampling system Action Action Action Action Action Disconnect the fused silica transfer line from the GC and ensure there is flow through the transfer line Connect a flow meter to the end of the fused silica transfer line and then set the HS carrier pressure to 20 psi 138kPa ensure there is a steady flow Perform a leak test as outlined in Leak Testing the Sample Injection System section in the Installation chapter Connect the HS to the GC and leak test the GC HS system Check all of the connections with a helium Leak Hunter or concentrated ethanol and water solution Once you have checked and tightened all of the connections then run the leak test again Heat the GC oven to the highest temperature used in the current method Allow the GC oven to cool and then tighten the column connection fittings Check the rear panel gas connections Ensure the carrier gas is securely c
215. nstall the HS Transfer HS Transfer GC Column Line into GC split Line connected via direct From GC injector port union inside oven to HS to column NOTE If liquid autosampler is installed These options can be connected the transfer line must be installed outside side panel mounting kit of the autosampler path rear panel of GC injector port Figure 7 Headspace Setup 60 Installation Yes No Split Operation Through the Injector Port OrrColumn Direct Operation Operation NOTE If liquid autosampler is installed the These options can be connected transfer line must be installed outside of side panel mounting kit the autosampler path rear panel of GC injector port This connection is typicalhy not recommended for the HS 40 110 Trap setup 4n advanced understanding of chromatography pressures and Aows are required if you use this setup The ZDL Zero Dilution Lines is desirable Figure 8 HS40 110 Trap Setup 61 Installation Installing the Heated Transfer Line at the HS Needle Unit TurboMatrix Headspace Only To install the heated transfer line at the HS needle unit 1 Cut the white PTFE sleeve that extends from the transfer line so that it is nearly flush with the outer shell of the transfer line Ensure that the sliding insulation tube is in the transfer line header 2 Place the electrical connector through the retaining collar Sliding Insulation Lug 2
216. nstructions provided here are for the experienced user You will require the following tools and accessories e Flathead screwdriver e Phillips screwdriver e 1 4 and 1 8 inch wrench e 1 16 inch and 3 8 inch wrench e 2mm Allen Key e Pneumatic leak detection device or concentrated ethanol and water solution Do not use soap solutions to detect leaks Warning Concentrated ethanol is flammable e Multimeter 37 Installation e Bubble flow meter Pre Installation Checklist Contact your safety engineer industrial hygienist environmental engineer or safety manager before you install or use this instrument to determine if there are any other considerations in addition to the information listed below Before the instrument arrives 1 Check your laboratory environment and ensure that the temperature and humidity settings are within the acceptable operating range for the HS See Operating Environment later in this chapter 2 Read Safety Information later in this chapter and ensure that you have complied with the requirements for each section 3 If you are using the PC software you must have a computer capable of running the software If you are running TotalChrom the HS control software can be run from the same computer 4 Obtain the required gas supplies See the section on Gas Supply Specifications later in this chapter Ensure that you have the required carrier gas filters 5 Ensure that you have the specified
217. nt and or loss of sample materials or data resulting from the use of sample vials caps and septa not supplied by PerkinElmer may occur The subsequent service visit to remedy the situation caused by the choice to use these non PerkinElmer sample vials caps and septa is not included under your warranty or service contract agreement Your Service Engineer can discuss the benefits of using only PerkinElmer sample vials caps and septa PerkinElmer sample vials and patented safety closures are carefully selected They are under permanent quality control If you use vials and closures from other manufacturers the instrument may not function correctly if a vial should rupture you risk injury from glass splinters and possible damage to the instrument WARNING Using sample vials caps and septa other than those supplied by PerkinElmer can result in damage to the instrument and or injury to the user if they attempt to remove the broken glass vials e Itis possible that a few vials in a batch are not within tolerance If in doubt we recommend that you check the sample vials using the vial gauge Part No BO15 1737 provided with the instrument e Observe the maximum filling volume of 15 mL for liquid samples when using 22 mL sample vials e Check the safety closure for reliable tightness after sealing the sample vial e Use only felt tip pens to mark sample vials Adhesive labels may jam in the oven 32 Introduction
218. ntation must be consulted to determine the nature of the potential hazard and any actions which have been taken gt BR O Safety Information Do not attempt to make adjustments replacements or repairs to this instrument except as described in the accompanying user documentation WARNING NOTE This equipment requires no specified inspection or preventive maintenance to ensure the continuous functioning of its safety features 20 Introduction Please read this section carefully before beginning operation of the HS and pay particular attention to any advice it contains concerning potential hazards that may arise from the use of the instrument This manual contains information and warnings that must be followed by the user to ensure safe operation Possible hazards that could harm the user or result in damage to the instrument are clearly stated throughout this manual The advice is intended to supplement not supersede the normal safety code of behavior prevailing in your country Warning Toxic Fumes Fume Ventilation System Without adequate ventilation potential toxic vapors can build up in the laboratory your laboratory must have a reliable fume ventilation system before you use this instrument WARNING Warning Explosive Atmosphere This instrument is not designed for operation in an explosive atmosphere WARNING This equipment must be used in a manner specified by this manual
219. o 50 cm 4 The transfer line is connected to the GC injector using a stainless steel adapter Part No B0505266 and a septum 5 Place the septum into the adapter See Figure 18 71 Installation 7 8 NOTE Sto 9 10 11 12 Carefully push the fused silica column through the adapter piercing the septum Connect the adapter to the end of the transfer line Remove the septum nut from the GC injector port re the septum nut in a safe location for later use Feed the fused silica tubing through the GC injector Loosen the threaded collar from the stainless steel adapter and using the threads on the adapter as a handle screw the adapter into the injector port Replace the threaded collar of the transfer line onto the stainless steel adapter use the universal connector Inside the GC oven connect the fused silica of the headspace transfer line to the other end of the column connecting union P N N9302149 Leak test the system See the procedure Leak Testing later in this chapter On Column Connection Recommended for the HS 40 110 trap In the on column configuration you will take the capillary column out through 1 2 72 the injector and connect it to the sampling head Turn off the GC and allow the injector to cool Inside the GC oven disconnect the GC column from the injector Unravel approximately 1 meter of the capillary column Remove the nut and fitting Score and bre
220. o spare traps on hand in case of breakage NOTE Turn off the unit and Column Isolation will be automatically applied CAUTION Do not over tighten the fittings Only tighten the trap fittings enough to prevent leakage The quartz tube is fragile NOTE When installing the trap in the instrument for the first time or you must take the trap assembly apart you must do an alignment procedure See the next procedure Trap Breaks Inside the Trap Assembly for the steps on aligning the trap If you are just removing an old trap and replacing it with a new trap you do not need to do an alignment procedure 276 Routine Maintenance To remove the trap 1 Turn off and allow the system to cool The vial oven and the trap enclosure may be very hot Allow 20 30 minutes for these parts to cool WARNING 2 Remove the looks cover by opening it and taking the cover off the hinges by lifting it straight up Turn off the HS40 110 trap or start the column isolation flow This will enable gas flow to continue to the GC but the trap will be blocked off 3 Remove the large thumb screw and put it in a secure location 4 Pull out the dry purge assembly P N N6700112 See the following photo Figure 115 5 Carefully loosen the nut in the back of the trap assembly Turn it 1 4 to 1 2 turn only since if you loosen 277 Routine Maintenance it too much the O ring inside will be out of alignment and difficult to
221. o the explosive nature of hydrogen NEVER use hydrogen gas as a carrier gas in any GC headspace system WARNING Filtered helium or nitrogen with a minimum purity of 99 995 or better will be required Use only approved gas lines to install the gas supply system for the HS You must use the same carrier gas for the HS that is required for the GC analysis Carrier gas for an HS GC system performing trace analysis or using either a mass spectrometer or an electrolytic conductivity detector 46 Installation ELCD must have a minimum purity of 99 999 and must be properly filtered Always use either copper or stainless steel tubing which is free of grease oil and organic material for all gases delivered to the HS GC system The carrier gas connections require 1 8 tubing with 1 8 connectors CAUTION Never clean carrier gas tubing with organic solvents Any remaining traces of solvent will contaminate your system Use compression fittings to make any joints in the tubing Do not use soldered joints The flux used in solder may contain a strongly electrophilic compound If the HS is fitted with the cryofocusing accessory a supply of an inert gas i e nitrogen and a Dewar vessel containing liquid nitrogen is required Observe proper handling procedures for compressed gas cylinders See Compressed Gases on page 27 WARNING Check the gas lines and connections regularly for leaks Gas purity improves w
222. ography supplies and columns through the PerkinElmer essentials catalog The PerkinElmer Virtual Store is an exciting addition to the analytical instruments suite of interactive resources The Virtual Store is easy to use and provides an electronic catalog with detailed product descriptions With one click orders can be sent via e mail Come and browse the store at www perkinelmer com Customer Service Supplies Accessories and Replacement Parts Address PerkinElmer Instruments 710 Bridgeport Avenue Shelton CT 06484 4794 U S A Telephone US and Canada 800 762 4000 only 8 a m to 5 p m EST Your order will be shipped promptly usually within 24 hours Telephone Worldwide Call your local PerkinElmer sales or service office or call PerkinElmer in Shelton CT USA 800 762 4000 Internet http www perkinelmer com e mail essentials perkinelmer com Applications Notes and 800 762 4000 and http Technical Bulletins www perkinelmer com Table 22 Contacting PerkinElmer 335 Appendices Appendix B Warranty Exclusions and Limitations The following consumable items are excluded from your instrument warranty agreement e Fused Silica Transfer Line e Ferrules e O rings e Filters e Trap e Fuses Any attempts to perform installation or maintenance operations that are not detailed in this manual are at the user s own risk WARNING If user attempted service results i
223. olant gas and associated delivery system are not an issue as this gas does not come into contact with the sample Hydrogen If you are using hydrogen for GC detectors only ensure that all hydrogen lines and connections are leak free When using a hydrogen tank install an in line hydrogen flame arrestor P N 0009 0038 between the tank regulator and the delivery tubing 48 Table 9 Gas Supply Specifications Installation Electrical Connections Electrical connections between the HS and the GC are made at the HS input output port shown in Figure 1 This port is located on the back of the instrument There are the following six options for connecting the HS to a GC 1 HS to AutoSystem XL or Clarus 500 GC with TotalChrom LINK Interface HS to AutoSystem XL GC or Clarus 500 and PE Nelson 900 Series Intelligent Interface HS to AutoSystem XL GC or Clarus 500 and Network Chromatographic Interface NCI HS to a GC other than an AutoSystem XL or Clarus 500 and the HP 6890 HS to the HP 6890 If the HS is PC controlled the PC must be connected to the HS The HS Input Output Port Communication consists of a number of relay contact signals provided by the HS which can be read by the external device and a relay contact signal provided by the external device which is read by the HS Figure J shows the signal connections to the Input Output Port 49 Installation GROUND GROUND GROUND START IN
224. omatogram is assigned to a particular sample vial This is due to the fact that synchronization between the HS and such instrumentation is usually provided by the Inject signal from the HS which starts the GC See BCD Interface on page 165 If processing of a vial is started by the HS but is stopped for example by a missing vial a GC run is not performed for this vial because an Inject signal is not generated The next GC run is produced only when the sample from the following vial has been injected onto the GC There will be gaps in the GC runs corresponding to samples that were not successfully transferred to the GC 51 Installation Although the position of these gaps can be determined from the Log tab some data handling systems automatically increment the sample number reported with the chromatogram This can be misleading The fail output signal consists of a relay contact closure between pins 7 and 8 Fail Out See Figure 1 The Fail Out signal is generated instead if the Start signal in the event of a missing vial This signals to an external device that the expected sample will not be transferred and that there will be a gap in the chromatographic data Under these circumstances the Fail signal can be connected to the external device in parallel with the Inject signal so that either signal can start the run This results in blank runs being generated for tubes that fail but synchronization of the HS and the other instrumenta
225. on after position one the thermostatting time will be increased by n times the initial thermostatting time where n is the sample number In progressive mode the thermostatting time of the nth sample is n times the value chosen for the 1st sample For example Sample 1 is thermostatted for the value entered Sample 2 is thermostatted for twice the entered value Sample 3 for three times the entered value and so on Thermostatting lilt Time T WW eN Samplet shi I Sample 2 Thermostatting ll Time T 2xT JM i hih T 3xT WN Sample 3 T nxT Figure 90 Thermostatting Time Using Progressive Mode Number of Injections This parameter defines the number of extraction steps in multiple headspace extraction methods Valid settings are 1 to 9 injections 214 Method Development If you take two consecutive aliquots from the headspace of the same vial although the partition coefficient K remains constant the peak area obtained for the second aliquot may be smaller than the area obtained in the first analysis If you continue taking successive aliquots from the vial s headspace the total amount of the analyte present will further decline eventually becoming totally exhausted Thus the sum of the amounts of the analyte removed in the individual extractions will be equal to the total amount of analyte present in the original sample This is what we call the multiple headspace extraction method Its advantage is
226. on carts designed for compressed gas cylinders Do not move cylinders without the valve protection cap in place e Always secure cylinders before removing the cylinder valve protection cap and before connecting the regulator and adapter tubing e Use only the specified regulator for the carrier gas cylinders e Never plug obstruct or tamper with safety relief devices e Wear safety glasses and ear protection when working with compressed gases When using hydrogen or methane special care must be taken to avoid the build up of explosive gas mixtures in the GC oven or interior of HS system e Ensure that all hydrogen line couplings are leak free and do not allow hydrogen to be vented inside the oven Do not use H with HS systems pressure venting makes this very dangerous WARNING Regulators for Compressed Gases Use only approved regulators for gas supply lines and observe the following e Use only the specified regulator for carrier and calibration gas 28 Introduction Confirm regulator type and material with your specialty gas supplier e Mark each regulator with its intended service and never use a regulator for more than one service Do not change gas service or adapt equipment without consulting your gas supplier e Ensure regulator construction materials are compatible with the gas and that the cylinder pressure gauge will withstand the cylinder pressure e Never use the regulator as a shut off valv
227. on the Option tab see page 114 The Inject Pressure is applied to the sampling needle and the column head pressure from start of the pressurization time until the end of the withdrawal time and or the end of the vial venting time if vial venting has been selected 118 Operation HS 40 110 Trap Status Tab Temp The Temperature tab on the Status tab for the HS 40 110 trap offers an additional option of inputting the trap temperatures Trap Low Temperature This is the temperature to be used for the absorption of the analytes during trap loading It should be low enough in order to trap the components of interest but not too low Temperatures that are too low could cause moisture condensation in the trap itself The default value is 40 C The range of acceptable values is 0 to 100 C in increments of 1 C The minimum attainable temperature is approximately 2 C above the ambient temperature Trap High Temperature This is the temperature to be used for the trapped components of vaporization and their subsequent injection into the column It should be high enough to ensure fast complete vaporization of the sample The default value is 280 C The range of acceptable values is 0 to 400 C in increments of 1 C NOTE The default Trap Maximum Temperature is 400 C This value depends on the trap material The name of the method that is currently loaded on the Run tab is also displayed The settings displayed here are from
228. onger 6 Touch Start to begin the trap conditioning procedure NOTE If running in sequence mode be sure to start the active method not the sequence the sequence will activate the saved method During the Trap Hold 30 minutes the vaporized Trap contaminants and moisture will elute via the needle purge outlet or on to the column During cleaning the Isolation Flow of 10 ml min will isolate the transfer line and analytical column from the Trap effluents The GC is not involved in the trap cleaning No GC run is started it could even be off NOTE It is recommended that you clean or install a new trap if you see carryover in your blanks run after this test 283 Routine Maintenance Trap Clean Eao n aeS 10mL min a AU z 10mL min 4 Isolate sv8 Carrier sv1 50mL min lt Leak Test SsVia Figure 121 Cleaning the trap Trap Test After a Trap cleaning the system should be checked with a blank run under the GC method to ensure that no ghost peaks or baseline disturbances are observed This is the Trap Test procedure During the Trap Test the system HSTRAP GC simulates the Trap Desorption and Injection step of the HS Trap At the same time the GC runs its method cycle 284 Routine Maintenance Monitoring of the baseline reveals whether the Trap cleaning is successful or that replacement of the Trap is necessary During this test
229. onnected and that the Troubleshooting delivery pressure is set to 90 psig 620kPa Cause The lower opening on the needle is plugged Action Clean the needle See Cleaning the Jet Needle in the Routine Maintenance chapter Action Replace the needle See Removing and Replacing the Needle in the Routine Maintenance chapter Cause The needle seal assemblies have degraded Action Open the upper and lower needle seal assemblies and replace the o rings Check the seals for signs of wear Replace them if necessary See Changing the Upper Needle Seal Assembly and Changing the Lower Seal Assembly in the Routine Maintenance chapter Cause The needle has not been installed correctly Action Ensure the needle holes are pointing towards the transfer line See Removing and Replacing the Needle in the Routine Maintenance chapter Cause The transfer line has not been installed correctly at the needle or at the GC injector Action Check the connections at the sampling unit and ensure all nuts and ferrules have been installed correctly Do not over tighten any fittings NOTE The deactivated tube adapter tube is a glass lined stainless steel tube Over tightening the fittings may result in damaging the tube or the fittings Action Check the connections at the GC injector Action Ensure both ends of the fused silica transfer line have been cut cleanly See Figure 10 Cause The thermostatting temperature is too high and the
230. or Stalled Cause An obstruction has caused the needle to halt Action Turn the HS off and disconnect the power cord from the AC mains Remove the obstruction and reconnect the line cord Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized correctly You must update the vial range on the Run tab to exclude the vials that have already been run and press the Start button to continue your analyses Cause The o ring seals have degraded Action Replace the o rings as outlined in the section on Changing the O rings in the Routine Maintenance chapter Cause The needle cannot penetrate the septa of the sample vial Action You are using septa or caps that are not for use on automated headspace sampler Use only PerkinElmer vials caps and septa Cause The needle is dirty Action Abraded sealing material from the vial septa may stick to the needle and can cause the needle to seal incorrectly during pressurization and withdrawal Clean the needle as outlined in the section on Cleaning the Jet Needle in the Routine Maintenance chapter Cause The needle motor has overheated Action The sampling head is not being cooled efficiently Ensure the front access door is closed when the HS is in operation Action Turn off the HS and allow 10 to 15 minutes for the driver motor to cool down This fault may 299 Troubleshooting be an indication t
231. or more details on the shaker option as well as considerations when setting the duration of thermostatting time when the shaker is used The shaker only starts an automatic shaking program when a headspace method which utilizes the shaker is started In MHE mode the optional shaker must be switched off Shaking is not possible during MHE analyses since the needle remains inserted in the vial during all of the analyses NOTE See additional options that are available in the section Status Tab Option Tab for the HS 40 110 Trap on page 122 The Status Tab PPC Tab Programmed Pneumatic Control PPC is the electronic control of the carrier gas pressure You can set the carrier gas pressure from the PPC tab then the PPC control module regulates pressure to that set point Column Pressure This is the carrier gas pressure for the HS system The carrier gas is used to pressurize the vials and then carry the sample through the transfer line to the GC injector or column You will set the carrier pressure on this tab even if the PPC module is not installed on your instrument 117 Operation Run Status Log Column 20 0 psi Set Point Actual TestL_Env5_2 CJC Temp Timing Option eppc STANDBY hinuurgfu Stat Rotate Tools w Figure 38 PPC Tab Inject Pressure This option is available and the pressure set if the system is PPC equipped and high pressure injection has been selected
232. or the HS if you are performing any of the following e Pressure programming e Constant flow or constant linear carrier gas velocity over an oven temperature program e Flow programming e High pressure sampling During headspace injection the split flow added to the GC injector dilutes the headspace sample For example an HS transfer line flow 222 Method Development of 25 mL min and a GC split flow of 25 mL min results in a 1 1 dilution or split of the original headspace sample concentration Since additional carrier gas is supplied from the HS the actual flow through the GC split vent must be measured by an external flow meter The flow through the split vent should be equal Actual Split Flow Transfer Line Flow Column Flow Split Set point Equation 3 Splitless Sampling In the splitless sampling technique the sampling head pressure is used to pressurize the vial and to supply the GC column flow This technique is recommended for the HS 40 110 trap but could also be used just with the headspace For reproducible analytical results the sampling head pressure must be greater than the headspace pressure in the vial During pressurization the pressure in the vial equals the sampling head pressure During injection the sample vapor flows to the column The rate of the pressure decrease in the sample vial depends on the carrier gas flow Any GC injector can be used for splitless sampling The injector is used only to prov
233. ove calibration is run with a calibration vial identical in content solvent and sample volume with the vials to be analyzed When this procedure is started the system thermostats this vial for a preset Thermostatting time of 2 minutes Thermostatting temperature and subsequent Pressurization Pressure and Time are carried out under the values set in the method The Pressure Decay in the Calibration lasts two minutes preset by the system At the end of this process the system will display for you the pressure decay curve On choosing Calibrate Decay Time loading the calibration vial and pressing the Start button the following screen appears and this process begins Calibrate Decay Time Pressure psi Uo We Meh ee a Time min Calibration Vial 1 Time 2 0 Decay Time 1 0 min STANDBY Oct 24 n C C Close Figure 78 End of the Calibrate Decay Time function This is a correct Pressure Decay The calibration curve is linear with a good slope It reaches minimum pressure at around 1 4min A safe Decay time in the method would be 1 6min 200 Method Development The Pressure Decay curve should be a linear function with a proper slope to the vial lowest pressure after decay ends The Decay time should be set at a value safely beyond the pressure curve minimum but not too long as this will unnecessarily prolong the overall vial handling time The Decay Time range of values is 0 1 99 9 min in steps of
234. over tighten any fittings NOTE The adapter tube is a glass lined stainless steel tube Over 307 Troubleshooting tightening the fittings may result in damaging the tube or the fittings CAUTION Ensure that the transfer line does not touch the needle This could cause bending and scratching Action Check the connections at the GC injector Action Ensure both ends of the fused silica transfer line have been cut cleanly See Figure 13 in the Installation chapter Cause The gas connections on the rear panels have not been made correctly Action Check and tighten all gas fittings on the rear panel Problem Cannot select another method on the Run tab Cause Single method operation has been selected on the Preference s Run Tab Action If you need to edit the method you must disable single method operation Refer to the section on Preferences Tab in the Operation chapter Problem Cannot edit a method from the Run tab The Method Editor is greyed out Cause Single method operation has been selected on the Preference s Run Tab Action If you need to edit the method you must disable single method operation Refer to the section on Preferences Tab in the Operation chapter Problem Cannot enter an injection pressure for the high pressure injection on the PPC tab Cause The high pressure option is not enabled on the Options tab 308 Troubleshooting Action Switch to the Option tab a
235. p tab 2 Press the Password Protection check box A check mark will appear in the box to enable the option 3 To create a password touch the gray bar to the right of Password Protection The password window will then appear 4 Touch the new entry box and the Alpha Numeric Entry window appears 5 Enter the desired password using letters Alpha tab and or numbers Num tab The blue shift key changes letters to from upper case Touch OK 6 Touch to confirm entry box Repeat the password entry Touch OK 7 Press OK to close the Preferences tab This confirms your selection If you press Cancel then the settings on this tab revert to the default settings Priority Vials This feature can be used only if the vial under counting has a magazine position of 10 or higher This feature can also be used to insert vials into an analysis sequence that has already been started Once the vials have been placed in the priority vial position and the priority command is issued the priority vials are inserted into the analysis sequence The analysis of the priority vials does not affect any ongoing thermostatting of vials or analysis This parameter reserves sample magazine locations for a priority run You can select 39 40 40 or None On the HS 110 you can select 109 110 110 or None The priority vial option is not available on the HS 16 NOTE If two priority vials are selected the higher numbered position will be analyzed
236. pass over the trap to purge the trap of water The amount of time needed for the dry purge 203 Method Development will vary depending on the type of sample you are running and the HS Trap Cycles number The higher the number of Trap re loadings the higher the HS oven temp and the more moisture your sample has the higher the moisture will condense Note If the FID extinguishes during your analysis you will have to increase the dry purge time Desorb Time HS 40 110 Trap Only Desorb time is the time for the sample to be desorbed from the HS 40 110 trap to the transfer line column GC Typically for a 10 ml sample 0 5 min is plenty of time Pre Post Cryofocusing Time Headspace Only These optional parameters appear only if the cryofocusing accessory is installed and the option has been enabled The pre cryofocusing time takes place before the sample injection Pre Cryofocusing Time Cryofocusing Time Withdrawal deja Vent HS Analysis Time Time to Reach Cryofocusing Set Temperature GC Analysis Time New Analysis Time minutes Figure 81 Setting the Pre and Post Cryofocusing Time NOTE The reference point for the cryofocusing times is always the end of the injection time The system parameters pre and post cryofocusing time are used to optimize the cryofocusing duration before and after sample injection 204 Method Development The cryofocusing duration determined when optimizi
237. pen knurled sleeve pulled all the way to the front 268 Routine Maintenance To start a Valve Leak Test 1 Set the carrier pressure at 45 psi in the Column field of the Option tab 2 Open the Tools drop down menu select Maintenance and then select Valve Leak Test 3 Next touch the OK button in Start the Leak Test now window This part of the plumbing is now a closed pressurized system The pressure displayed on the PPC tab must not drop by more than 1 psi over a period of 40 seconds On test completion the system displays the Leak Test Results screen 4 If the first Valve Leak Test fails repeat the test 3 more times If these additional tests come out successfully pass ignore the first one However if these tests fail a leak is detected Check all of the connections between SV 1a and the inlets to SV1 and SV9 with a helium Leak Hunter or a concentrated ethanol and water 50 50 solution The most suspect parts in this area are SV1 or SV9 or the filter connections However most of this plumbing area is not accessible to the operator A PerkinElmer service engineer should be called in For more details see the Leak Troubleshooting section in the Troubleshooting chapter of this manual On completion of this check return the system to Standby and set the Transfer line temperature to its method value Magazine Maintenance Removing and Replacing the Magazine The magazine on the HS 40 and the HS 1
238. perature P1 1 2 x Headspace Pressure 20 kPa Equation 2 P1 should be at least 30 50 kPa 4 7 psi higher than Pac to account for the pressure drop caused by the split The split vent flow should be at least 2 mL min For a graph on equilibrium pressure for aqueous samples as a function of thermostatting temperature see Figure 74 The equilibrium pressure can also be measured directly from a thermostatted vial using the vial pressure gauge P N B0501377 The following diagram indicates the pressures in the sample vial sampling head and column head in the system with split operation E l gt Ss e ip N Headspace Pressure ie Progsyre P4 Column Head Pressure Pac Figure 92 System Pressure During Split Operation Example Setting P1 and Pac for split operation Aqueous sample is to be thermostatted at 80 C A P1 of 17 psi 120 kPa is required for split operation and a column head pressure of 10 psi 70 kPa is required 220 Method Development 1 Set P1 to 17 psi 120 kPa 2 Adjust the split flow on the GC until you reach 9 psi 60 kPa 3 Adjust Pec until you reach the required pressure of 10 psi 70 kPa In order to connect your HS to a split splitless or PSS injector you must be familiar with the operation of your GC The instructions provided below are specific to the AutoSystem XL or the Clarus 500 Refer to your AutoSystem XL User s Manual P N 09936073 or the Clarus 500 User
239. placed in the same orientation as when it was removed i e the same side must be facing up Retain the seal removal tool in the seal assembly Routine Maintenance Needle Unit Lower Assembly oe M3 Hole 6 gt o rings Thumbscrew a ar i Tool Lower Seal Figure 98 Changing the Lower Seal Assembly Metal Disc with Holes Spigot Key 0 12 Ensure that the needle seal assembly is correctly seated before securing it with the metal disc Tighten the metal disk by hand enough to hold the seal assembly in place Use the spigot key to turn the metal disk counter clockwise 13 Close the front panels and reconnect the instrument to the electrical supply 14 Power up the instrument and turn on gases 15 Perform a leak test to ensure the instrument is leak tight 251 Routine Maintenance Changing the O Rings Normally it is not necessary to replace the whole needle seal assembly In most cases it is only the o rings that need to be changed A special o ring tool B0147449 is supplied for removing and inserting the o rings O Ring Tool O Ring m 0 Seal Assembly Figure 99 Changing the O Ring Seals To replace the o ring NOTE 252 1 Remove the needle seal assembly See Changing the Upper Needle Seal Assembly on page 247 or Changing the Lower Seal Assembly on page 249 Insert the narrow end of the o ring tool into the o ring Carefully press the tool to the side and remove the o r
240. printer is required in order to obtain printed reports e A mouse or another pointing device supported by Windows e A serial port for direct connection to your instrument using the communication cable kit P N M0417035 The serial port to which the HS is connected cannot be shared with another serial device You may require additional serial ports for an NCI a mass spectrometer and other serial devices NOTE The communication cable is a null modem cable e ACD ROM drive for installing the control software Refer to the Control Software Manual for details on the installation and operation of the control software 181 Accessories HS 40 110 Trap Accessories The HS 40 110 trap offers some options and accessories The Integrated Trap This feature is available on the TurboMatrix 40 Trap and TurboMatrix110 Trap options as a factory installed accessory only It cannot be fitted at the same time as the cryo trap IS Addition This feature is available on the TurboMatrix 40 Trap and TurboMatrix 110 trap options as a factory installed accessory or as a field installed upgrade on systems where the trap has been preciously installed Vial Integrity Testing This feature is standard on the trap based systems for the TurboMatrix 40 Trap and TurboMatrix 110 Trap options Vial Temperature Calibration This feature is standard for the HS16 HS40 and HS110 options 182 Method Development 5 lt gt Method Development
241. proximately 30 minutes for the needle assembly and transfer line to cool down 2 Once the system has cooled switch off the instrument 3 Disconnect the instrument from the electrical supply 249 Routine Maintenance NOTE 250 4 Pull gently on the magnetic door release of the front panel to open the door 5 Remove the needle holder and the needle as outlined in Removing and Replacing the Needle Headspace Only on page 243 6 Screw the seal removal tool into the threaded hole M3 of the lower needle seal assembly You will need to hold the removal tool as it will rotate once you begin to loosen the metal disc 7 Place the spigot key into one of the holes in the metal disc 8 Turn the metal disk clockwise right to left when facing the instrument to undo it as far as necessary to allow the lower seal assembly to be released 9 Using the seal removal tool gently pull out the needle seal assembly Take note of the orientation of the seal assembly You must retain this orientation 10 Check the seal assembly and replace the o rings as outlined in Changing the O Rings on page 252 There are two o rings in the lower needle seal assembly Do not touch the new o rings with your fingers Use forceps or tweezers to remove the o ring from its bag and place it on the seal assembly If you touch the o ring for any reason throw it out and use a clean one 11 Replace the seal assembly Ensure the seal assembly is re
242. r entry for the column flow rate The injection volume corresponds to the flow rate measured at the end of the column under normal atmospheric pressure and temperature conditions If you select injection Volume as your mode of injection specify the column flow rate Tools gt Preferences gt Config Tab and the desired injection volume The HS will automatically calculate the corresponding injection time If you select Time as the injection mode the HS will determine the injected volume from the time you have entered on the timing tab and the column flow rate Vial Venting To enable automatic venting of the vial set to a venting time This parameter enables vial venting of the sample vial The vial is vented after the withdrawal time If you have enabled vial venting then you must set a vent time This will be the length of time during which the vial is vented to atmosphere Venting occurs immediately after the withdrawal time has elapsed Default should be 0 3 min 18 seconds Venting is used to allow for the safe handling of spent vials after analysis High Pressure Sampling If you are using the high pressure injection option you will set the injection pressure here You must first enable the option on the Option tab This option is available if you have PPC installed You can enable it on the PPC tab as Inject psi For more information see the section Principles of High Pressure Sampling in the Method Development chapter of thi
243. ransfer line temperature to 210 C Allow the transfer line to purge overnight Poor Sample Recovery or Reduced Sensitivity If you cannot obtain the desired detection limits you must first eliminate the GC as the source of the problem Inject a representative sample at the desired concentration directly into the GC and ensure that you can obtain the desired response If you cannot obtained the desired response then refer to your GC user s manual or contact your PerkinElmer service engineer If the GC is fine then you must troubleshoot the HS and the transfer line Cause The needle or the transfer line are not hot enough and the sample is condensing Action Set the temperature of the needle and the transfer line to at least 10 C higher than the thermostatting temperature Cause The sample has not reached equilibrium before the sample injection was made Action The pressurization time needs to be long enough to ensure homogeneity of the gas phase in the vial The pressurization time should be at least 2 minutes for good reproducibility and 3 minutes for optimum reproducibility For some applications where a short pressurization time is used to increase productivity expect 315 Troubleshooting 316 deterioration in performance You may see an increase in RSD from 1 to 3 to greater than 5 RSD A pressure gauge P N B0501377 is available for measuring the sample vial pressure Cause The fittings connecting the tra
244. rap Dry Purge flow rate instead of the recommended 50 ml min Isolation Flow is low A misadjusted column Isolation Flow will also decrease sensitivity and cause the Pre Injection effect If the Isolation Flow is less than required it will not isolate the HS transfer line GC column from the vial trap system Instead during the Trap Load step the flow from the pressurized vial to the trap will also branch to the transfer line GC column carrying with it part of the HS vapor This will result in an early peak Pre Injection and the Desorption Analysis peak will be smaller loss of sensitivity with poor repeatability as the trap HS vapor content is now less than that in a regular trap loading The next curve indicates a leak in the system or that the Isolation Flow is incorrectly adjusted or both 322 Troubleshooting x _ 60 0 g a 300 a a 00 0 04 08 12 16 2 Time min Calibration Vial Pi Time 20 Decay Time 1 0 min STANDBY 12 27 14 Sian j E EJ Close Figure 129 Action A good rule here is to adjust the Isolation Flow to a value equal to the GC column flow plus 5 10 ml min A total value of 12 15 ml min seem to be adequate for all types of columns and analytical conditions In the next figure the Pre Injection effect is shown 323 Troubleshooting gt ParkinElmor rrn yea Biwai atl No cr Ireufficiert Eolation Flow Pw inpoton zm a Figure 130 Troubleshooting
245. raphical status and instrument control e Log events that may affect analysis results e Create printed method or sequence reports A computer is not required to run the HS If however you have a large number of varied applications then the PC control software is recommended If you do opt to use the HS Control Software your computer must be capable of running the PC Software and TotalChrom If a TurboMass detector is also a component of the system then the computer that is supplied with the mass spectrometer can be used to run HS control You require the following hardware and software to connect your computer directly to the HS and run the control software NOTE Additional hardware may be required if you are running your data handling system from the same computer Refer to the documentation supplied with your data handling system for details The minimum hardware configuration requirements are 180 Accessories Windows 2000 2003 Servers e Processor Intel Pentium 933 MHz e Memory 256 MB RAM Windows 2000 Clients e Processor Intel Pentium 933 MHz e Memory 256 MB RAM Windows XP Clients e Processor Intel Pentium 933 MHz e Memory 256 MB RAM e Workstation The operating system requirements are e Windows 2000 with Service Pack 3 Window XP with Service Pack 1 The minimum hardware configuration requirements are e Windows 2000 or XP e Processor Intel Pentium 933 MHz e Memory 256 MB RAM e A Windows compatible
246. raphy in Gilbert J Analysis of Food Contaminants Elsevier Ltd London New York 1984 Kolb B Auer M Pospisil P Quantitative Headspace Analysis of Solid Samples a Classification of Various Sample Types Chromatographia 19 113 1984 Kolb B Headspace Gaschromatographie mit Kapillar Trennsdulen Praktische instrumentelleAnalytik LaborPraxis Vogel Wiirzburg 1986 341 Appendices Laboratory Safety Practice e Bretherik L Bretheriks Handbook of Reactive Chemical Hazards 4th ed Butterworth amp Co Ltd London 1990 e Bretherik L Hazards in the Chemical Laboratory 3rd ed Royal Society of Chemistry London 1981 e Furr K ed CRC Handbook of Laboratory Safety 3rd ed The Chemical Rubber Co Press Florida 1990 e Data Sheets provided by chemical manufacturers e g USX Material Safety Data Sheets MSDS FRG DIN Sicherheitsdatenbldtter GB Hazard Data Sheets e Prudent Practices for Handling Hazardous Chemicals in Laboratories National Research Council National Academic Press Washington D C USA 1981 e Sax N ed Dangerous Properties of Industrial Materials 7th ed Van Nostrand Reinhold New York 1989 Multiple Headspace Extraction The theoretical principles of Multiple Headspace Extraction are presented in the following publications e Hachenberg H Schmidt A P Gas Chromatographic Headspace Analysis Heyden amp Son Ltd 1977 e Kolb B Auer M Pospisi
247. ratures are at set point and that the headspace is ready 1 Extend the pressurization time to approximately 20 minutes Load a vial containing a sample into the magazine and start a run You do not need to save this method You must be in the Status tab or the HS will attempt to run the method or sequence on the Run tab 2 Wait until the thermostatting time has elapsed Press the Run key on the GC at the start of the pressurization time 3 Should a chromatogram appear during the pressurization time the setting for injection pressure is too low Repeat this procedure at a higher injection pressure until the pre injection of the sample is eliminated This option is available if you have PPC installed You can enable it on the PPC tab See Cryofocusing Accessory on page 172 for a detailed description of this option and some operating guidelines Split Sampling Headspace Only Split sampling is recommended for most headspace applications using capillary columns Using this technique the sample is delivered more efficiently through the transfer line A pressure drop of 5 to 7 psi 35 to 50 kPa can be generated across the transfer line 218 Method Development depending on the split flow This can be useful when operating short capillary columns or wide bore capillary columns at a limited head pressure while the headspace vial equilibrium pressure is high Typically when changing from splitless sampling to split sampling
248. re 243 Platinum Iridium 243 Replacing 243 245 Stainless Steel 243 Temperature 110 191 Types 243 Upper Seal Assembly 247 Widebore 243 Needle Purge Gas Flow checking 85 New Method Command 134 Next Thermostat 295 Nitrogen Cryofocusing Accessory 48 Liquid 29 Number of Injections 117 214 O On Column Connection 72 102 224 Open Command 134 Operation 97 Cryofocusing Accessory 172 MHE 117 213 Multiple Method 106 138 150 Pre selected Single Method 138 Single Method 105 137 149 Split Setting Carrier Gas Pressure 100 Splitless Setting Carrier Gas Pressure 101 Index Starting 149 Warnings and Safety Practices 21 Options Board 163 Config Tab 138 High Pressure Sampling 208 Injection Mode 115 207 Number of Injections 117 214 Shaker 117 215 Thermostatting Mode 212 Vial Venting 116 Water Trap 116 212 Options Board Binary Coded Decimal BCD 165 Timed Event Relays 163 Options Tab 115 206 O Ring Changing 252 Changing Lower Needle 249 Changing Upper Needle 247 Scored Scratched 249 Tool 252 Outlets AC 44 Output Signal BCD 53 Fail 51 Output Signals Ready Out 51 Start Inject 51 Oven Status 130 132 Overlapping Thermostatting 196 222 P Packed Column Sampling 227 Password Protection 141 Peak Broadening or Splitting 309 Period from Injection to Injection 114 351 Index PerkinElmer Customer Service 335 Essentials Catalog 335 Service 235 Virtual Store 335 PII Time 114 Pneuma
249. re must be firmly crimped to the neck of the vial so that it cannot rotate freely but it should not be deformed in any way 6 If the vial is not sealed properly remove the cap using the cap removal tool P N N9301270 or the electronic hand decapper P N N9302595 and reseal the vial If the vial still cannot be sealed properly you may need to adjust the hand crimper See Adjusting the Hand Crimper on page 271 for more information Screw Top Sample Vials If not properly secured and sealed the screw cap vials may leak In order to prevent this from occurring please insure that the septa is seated securely in the cap prior to tightening In addition the vial cap should be securely screwed down with the cap and vial threads properly aligned Accessories Screw and Crimp Cap Vials Unsafe high pressure formed in the vial during thermostatting may be due to the use of a solvent with a boiling point that is too low for the application Operator error or inexperience may also contribute to unsafe thermostatting conditions For example if an aqueous sample is thermostatted to 80 C the internal water vapor pressure is only 47 kPa If however the sample is thermostatted at 180 C the internal pressure would be as high as 10 kPa with a high risk of vial explosion The internal pressure in the vial presses the septum disk against a star spring crimp top only and the aluminum cap which has a small curved slot At pressures abo
250. re using any cleaning or decontamination methods except those specified by PerkinElmer users should check with PerkinElmer that the proposed method will not damage the equipment Cleaning In general the instrument needs very little maintenance You can clean the outside with a damp cloth with non aggressive cleaning liquid Other items that may need periodic cleaning 236 Routine Maintenance Decontamination If the instrument or an accessory requires decontamination before repair maintenance warranty or trade in purposes at PerkinElmer the responsible body should read the procedure and complete the certificate which is available on the PerkinElmer public website http las perkinelmer com OneSource decontamination htm Follow the Decontamination of Instrumentation and Associated Sub assemblies procedure and complete the Certificate of Decontamination The certificate is used to certify the decontamination process was completed before equipment can be returned to PerkinElmer Carrier Gas The carrier gas is a major potential source of contamination Contamination can originate from the gas itself or from the tubing used to carry the gas Always use high purity gases 99 999 NOTE Appropriate filters should be placed in the carrier gas line close to the inlet of the HS to minimize the level of impurities in the carrier gas Ensure that gas lines containing filters are protected from excess pressure as described in
251. re values If you are using a Direct or On column connection then you are also supplying the GC carrier gas and you must consider the type of column and the GC temperature program when you are setting the catrier pressure You may need to connect a flow meter to the end of the column to accurately measure the column flow rates High Pressure Sampling The high pressure sampling technique is necessary if the vial pressure exceeds the column head pressure The standard balanced pressure sampling technique requires the column head pressure to be higher than the internal vapor pressure in the thermostatted sample vial 217 Method Development When using wide bore capillary columns 0 53 mm i d or high thermostatting temperatures it is possible that the internal pressure in the vial generated by the partial vapor pressures of the sample components can exceed the column head pressure The differential pressure between column head pressure and vial pressure becomes negative In such cases the sample expands onto the separating column as soon as the sampling needle moves down into the vial at the start of the pressurization phase causing double peaking and split peaks in the chromatogram The high pressure sampling technique permits sampling in such cases without these secondary effects The maximum injection pressure must not exceed 73 psi 500 kPa The minimum pressure can be determined as follows NOTE Confirm that your tempe
252. reated the desired sequence To delete an entry from the sequence select the entry in the list and press the Delete button To change the vial range you must add a new entry with the revised vial range and then delete the old entry If you edit the methods called by your sequence the sequence will use the revised methods If you need to edit a method but do not want to affect your sequence then save the revised method with a different name 107 Operation 7 You can use up to 8 methods in your sequence If you need to use more than 8 methods you must use the PC control software optional NOTE You will not be able to edit any of the selected methods if method editing has been disabled from the Tools button 8 Press the green Start button to run the sequence The HS will configure itself based on the method parameters The instrument status will be Not Ready until the instrument reaches all of the set points at which time it will become Ready When the GC and the data handling system are ready a vial will be loaded into the oven The vial will be thermostatted and the analyses will continue as determined by the method If you are using the HS 40 or HS 110 with the 15 vial oven the first vial will be loaded and then vials are loaded as required based on the time established by overlapping thermostatting Status Tab Headspace and HS 40 110 Trap The HS Status tab consists of four views Temperature Timing Option and P
253. rect number of cycles is the minimum number which results in the removal of practically all of the analyte vapors This is determined by successively analyzing identical vials with the same method altering only the number of Pressurize Decay cycles The smallest cycle number resulting in the highest vapor transfer indicated by highest peak area is the most suitable Needle Withdrawal After the last cycle the needle is withdrawn from the vial and this one is returned to the magazine Dry Purging the Trap Next is the optional step of the Trap Dry Purging if removal of moisture or and certain volatiles is desired The system applies a forward carrier gas flow through the cold trap at low trap temperature set in method from front to back and out of the Trap Dry Purge outlet 50 ml min The analytes in the sample headspace vapor are now adsorbed thus pre concentrated in the dried Trap The Trap is ready for the analytes desorption After the Dry Purge step the system interrupts the Isolation Flow to transfer line and column The PPC pressure will then take over The system will then proceed to the Desorption step only if the GC is ready If not it will wait until the GC becomes Ready Desorption With the GC ready the system will proceed to desorption It will rapidly heat the trap to the High Temperature set in the method Simultaneously it will 10 Operation apply a low pressure for a short time Both parameters
254. rectly You must update the vial range on the Run tab to exclude the vials that have already been run and press the Start button to continue your analyses Cause A mechanical problem has occurred 300 Troubleshooting Action Contact your PerkinElmer service engineer Fault Sensor Failure Zone 1 2 3 or 4 Cause The sensor for the vial oven in zone has failed Action Contact your PerkinElmer service engineer Cause The sensor for the needle in zone 2 has failed Action Contact your PerkinElmer service engineer Cause The sensor for the heated transfer line in zone 3 has failed Action Turn the HS off and disconnect the power cord from the AC mains Ensure the electrical connector from the transfer line is securely connected to the HS connector See the section on Installing the Heated Transfer Line at the HS Needle Unit in the Installation and Setup chapter Reconnect the power cord and turn on the HS to see if the fault has cleared Action Contact your PerkinElmer service engineer Cause The sensor for the cryofocusing accessory or the sensor for the HS 40 110 trap HS 40 110 trap in zone 4 has failed Action Contact your PerkinElmer service engineer Fault Vial Missing Cause No vial was present when the Start button was pressed or an empty slot was encountered during automatic operation Action Ensure all of the slots in the specified vial range contain vials To check the vial range open the Ru
255. resent in the oven When you are loading the HS 110 you must leave the load and unload spots empty You must also leave one further location on the outside ring empty for the HS to unload any vials that may be present in the oven The HS will search the outer ring until it locates the empty position To reduce the initialization time leave location 1 empty This is the first location that the instrument will look for the empty position Press the rotate button to move the magazine one quadrant at a time to access vial locations under the loading port of the thermostatted oven If you are using the smaller 9 ml vials you must use the low volume vial adapters P N N612 0110 NOTE You can only load these low volume vials in the outer ring of the HS 110 magazine Sample vials recently unloaded from the oven can be very hot When automatic venting is switched off the sample vials are still under pressure when unloaded from the oven Ensure that sample vials are cool before venting them and disposing of the sample WARNING Single Method Operation on the HS Once you have set up the HS and entered a method for your application you are ready to begin analyzing your samples To start a run 1 Ensure the GC is ready 149 Operation 2 Open the Run tab If you have selected single method operation instructions will be displayed on the tab 3 If you are running a single method and the method has been pre selec
256. rformance the HS 40 110 trap requires a splitless sampling setup For the headspace and the HS 40 110 trap configurations you can make a direct splitless connection by installing the fused silica transfer line so that it bypasses the GC carrier gas inlet You can make this connection by using the universal column connection P N N930 2149 inside the oven In this configuration the carrier gas is supplied and controlled by the HS All vapor entering the transfer line enters the column See the procedure Installing the On Column Connection later in this chapter For the headspace and the HS 40 110 trap configurations you can make a direct connection from the GC capillary column to the sampling head Sample separation begins immediately and again the vapor entering the transfer line enters the GC column The first meter of the column is under isothermal control and will not be affected by temperature program See the procedure Installing the Heated Transfer Line at the GC for Direct Connection later in this chapter NOTE For the on column connection ensure that the transfer line temperature is high enough to elute your last component of interest Lastly for the headspace and the HS 40 110 trap to improve performance the procedure Composite Zero Dilution Split Injector Liner for Headspace Interfacing later in this chapter 59 Installation HS Transfer Line Split Operation Direct Operation OrrColumn Operation I
257. rogressive kiiin Operating Mode UE Inject Mode is disabled Trap Bj in Trap operation Trap Clean Trap Test dotauk E ET JTemp JTiming Option Jppc STANDBY Sen 26 _ Stan Rotate Tools zji Figure 45 HS 40 110 Trap Status Tab Option Tab Status Screen PPC Tab for the HS 40 110 Trap The PPC tab on the Status screen for the HS 40 110 trap has the following options for the trap The vial PSI box allows you to set the pressure value for the vial in the vial pressurization and the trap transfer step Column Pressure This is the pressure that the PPC will apply at the end of the desorb step as the carrier gas column head pressure during the analysis Its value depends on the column characteristics the GC oven temperature program and the analysis requirements It range of values is 0 60 psi or 0 1 psi Vial Pressure This is the pressure the PPC applies during the step of Vial Pressurization 40 5Opsi is a reasonable pressure value that will allow the system to transfer the maximum of the headspace vapor volume to the Trap with a minimum number of cycles Too high a pressure would subject the system to rather rigorous conditions that may lead to gas leaks The range of values is 0 60psi in increments of 0 1 psi Desorb Pressure Trap Only This is the pressure that the PPC applies to the Trap during the Desorption step 128 Operation The range of values is 0 60 psi in increments of 0 1 psi NOTE During the Trap Dry
258. rotect human health and utilize natural resources prudently and rationally Specific treatment of WEEE is indispensable in order to avoid the dispersion of pollutants into the recycled material or waste stream Such treatment is the most effective means of protecting the customer s environment Requirements for waste collection reuse recycling and recovery programs vary by regulatory authority at your location Contact your local responsible body e g your laboratory manager or authorized representative for information regarding applicable disposal regulations Contact PerkinElmer at the web site listed below for information specific to PerkinElmer products Web address http las perkinelmer com OneSource Environmental directives htm For Customer Care telephone numbers select Contact us on the web page Products from other manufacturers may also form a part of your PerkinElmer system These other producers are directly responsible for the collection and processing of their own waste products under the terms of the WEEE Directive Please contact these producers directly before discarding any of their products Consult the PerkinElmer web site above for producer names and web addresses 31 Introduction Sample Vials CAUTION Using sample vials caps and septa other than those supplied by PerkinElmer may result in improper operation of the TurboMatrix Headspace or Trap Headspace Sampler Damage to the instrume
259. runo Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 71 111 Operation accessory allows you to concentrate your sample at the head of the GC column by cooling the head of the column See Cryofocusing Accessory on page 172 for details You can set the temperature to any value between 180 and 10 C in steps of 1 C Timing Tab Headspace and HS 40 110 Trap You can view the timing values for the HS from the Timing tab The exact values that you enter here will be based on your application The HS timing parameters will also be affected by the GC method Once all of the correct timing values have been entered the period from injection to injection PII can be calculated Run Status Log Pressurize Cryo Focus Pre Post Withdraw 0 1 min Thermo Cycle Time a OS 13 0 min min Pil 13 0 Relays n ppcspec JTemp Timing JOption ppe INITIALIZING 14 40 38 BH Tools Figure 36 Timing Tab Thermostatting Time The thermostatting time should be the shortest time the sample has to be thermostatted The analytical result will not change if the thermostatting time is longer than the time needed for equilibration Excessively long thermostatting should be avoided however because some samples may be sensitive to prolonged heating You can set the thermostatting time to any value between 0 1 and 999 minutes The default value is 12 minutes
260. s Press Alpha to return to the alphabetic keypad 8 Press OK to enter the new method name and then press OK to save the method and return to the Status tab You can switch to the Actual screen to view the current needle temperature Needle Temperature The needle is heated so that the headspace sample does not condense in the needle during injection You must keep the needle warmer than the thermostatting temperature The needle temperature should be high enough to prevent condensation but not so high that the septum is burned with a needle that is too hot For best reproducibility set the needle and transfer temperatures to a value 5 10 C higher than the sample temperature You must also consider the GC oven and injector temperatures It is recommended to set the transfer line and inject needle temperature to a similar temperature Typically the injector is a higher temperature The needle temperature can be set to any value between 35 and 210 C in steps of 1 C If you set the temperature to 0 the heaters are turned off 110 Operation Transfer Line Temperature Set the temperature at or slightly above 5 10 C the HS oven thermostatting temperature You must also consider the GC oven and injector temperatures Please refer to the section above Needle Temperature for recommendations However you need to remember that in the heated transfer line the headspace gas is a mixture of air with trace concentrations of the
261. s Usually 10 C above the thermostatting temperature is sufficient To clean your jet needle 1 Remove the needle as outlined in Removing and Replacing the Needle Headspace Only on page 243 2 Clean the needle with a lint free cloth or tissue If necessary dampen the cloth slightly with methanol CAUTION Do not touch the lower half of the needle with your fingers 3 When you are wiping the needle ensure that you do not force any material into the holes located on the side of the needle 4 Blow filtered carrier gas through the needle 5 Replace the needle assembly 246 Routine Maintenance Changing the Upper Needle Seal Assembly Check the needle seal assemblies Part Number B0500833 every 1500 injections Replace the o rings and check the holders for damage The seal assemblies holders and o rings need to be replaced if they are scored or scratched on the top or bottom surfaces The graphite coated Viton o rings B0198110 should be changed every 1500 injections The special tools required to remove and replace the seals and o rings are supplied in the shipping kit provided with the instrument To change the upper needle seal assembly 1 Turn off all heated zones by setting the temperature to 0 Allow approximately 30 minutes for the needle assembly and transfer line to cool down Once the system has cooled switch off the instrument Disconnect the instrument from the electrical supply T
262. s guide Water Trap lIn cryofocusing water is removed from the sample prior to enrichment using the water adsorption trap Water from the sample is removed by adsorption onto a hygroscopic salt Operating Modes Select Constant mode if you want to use the same thermostatting time for all samples that are analyzed by this method Constant mode is the standard mode of operation When you select constant mode overlapping thermostatting is enabled if you have an HS 40 or HS 110 with the 15 vial oven In Progressive mode the thermostatting time for a series of samples increases automatically for each vial Sample 1 is thermostatted for the value entered Sample 2 is thermostatted for twice the entered value Sample 3 for three times the entered value and so on 116 Operation Select Multiple Headspace Extraction MHE mode if you want to perform multiple headspace extractions The MHE function uses from 2 to 9 extraction steps per sample vial and pressurizes injects and vents each vial between extractions Number of Injections This parameter defines the number of extraction steps in multiple headspace extraction methods Valid settings are 1 to 9 injections Shaker If installed and selected the shaker can decrease the time needed for equilibration by providing continuous mixing of the sample in the vial during the equilibration process See information on the Vial Shaker accessory in the Accessories chapter later this manual f
263. s with a constant volume The specified nominal volume is usually very close to the actual volume In many methods the actual vial volume must be known If the work at hand involves a new batch or a new supplier It is advisable to determine this value This can be done by completely filling a number of vials with water weighing them and then using the mean value for future calculations For quantitative analysis identical sample volumes are required Loading the Magazine The sample vial locations in the magazine are numbered 1 to 16 1 to 40 or 1 to 110 depending on the instrument See the Accessories chapter Sample Vial section for details of sealing sample vials All vial locations can be filled on the HS 16 magazine The vial will be lifted from its location into the oven When the analysis is completed the vial is lowered to its location 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 46 148 Operation On instruments with the 15 vial oven it is possible to turn the instrument off while vials are still in the oven When the instrument is turned on again it will attempt to unload the oven You must provide an empty spot in the outside ring of the magazine so that the HS can unload the oven When you are loading the HS 40 you can place vials in all positions except for one You must leave one spot open in order for the HS to unload any vials that may be p
264. s are set as follows 900 SERIES OR NCI PORT TURBOMATRIX ADDRESS AO BCD LSD 1 Z 4 a MSD 1C 2c AC A7 8c BO BCD 10C GRC B5 GND WIRING DIAGRAM Figure 61BCD Interface Data Channel Contacts The BCD data channels contacts 1 to 13 are set to negative logic Negative is the default Negative is the default If you wish to change from negative to positive logic in the software under Tools select Preference in this screen the connect the logic can be changed to positive The Vial Shaker Accessory The frequency scanning shaker accessory may be installed on the HS 40 or HS 110 The options board is required for the shaker option If you have an HS 40 the options board must be installed The options board is standard on the HS 110 The shaker can decrease the time needed for equilibration by providing continuous mixing of the sample in the vial during the equilibration process When applying the shaker it is important that 166 Accessories the sample be in resonance with the shaker frequency to obtain the desired mechanical mixing effect In the case of liquid samples the resonance frequency depends on the sample viscosity and its volume To overcome this problem the frequency scanning shaker varies its frequency automatically during equilibration through a broad frequency range so that each sample in the oven reaches its resonance frequency The shaker option is installed in the factory If you ord
265. s controlling the backflush flow through the water trap The water trap can be regenerated by maintaining the GC oven temperature at 120 C for several minutes before beginning the next analysis Sample Vials PerkinElmer 22 mL crimped top sample vials P N N9306079 100 vials or P N B0104236 1000 vials and PerkinElmer 22 mL screw top sample vials P N N9306075 100 vials or P N N9306078 1000 vials are carefully selected for HS operation They are maintained under stringent quality control standards NOTE Using any other vials from a different manufacturer is not covered under the warranty Please observe the following information e Itis possible that a few vials in a batch are not within tolerance If in doubt we recommend that you check the sample vials using the vial gauge P N B0151737 provided with the instrument Do not use unsuitable vials e Check the safety closure for reliable tightness after sealing the sample vial e Use only felt tip pens to mark sample vials Adhesive labels may jam in the oven e Sample vials recently unloaded from the thermostatted oven into the magazine can be very hot and may still be under pressure Cool and vent the sample vials before you open or dispose of them Using the Vial Gauge to Check Sample Vials In order to ensure rapid and reproducible thermostatting the vials fit exactly in the oven As vials are heated in the oven the glass expands slightly If you are not using suita
266. s into the connector and tighten the screws 4 Connect all of your devices Re insert the connector 6 Connect the instrument to AC power and turn it on NOTE Relays 1 4 are contact closures and Relay 5 and 6 are switched 24 volts 54 Installation Once all the devices are connected you will power them up and program the timing for each device through the HS touch screen or the control software Refer to Timed Events on page 163 for important details Connecting the HS to the AutoSystem XL or Clarus 500 GC To connect the HS to the AutoSytem XL GC or Clarus 500 GC 1 Connect the generic Ready Start Cable Assembly P N N1011206 between the Input Output socket on the HS and make the appropriate connections on the GC as shown in Figure 5 2 The HS requires a contact closure or equivalent to be applied between pin 9 Ready In and Ground pins 12 13 or 14 to receive a GC ready signal The HS provides a contact closure between pin 5 and pin 6 Start Out to start a GC run NOTE In the following illustration Pin 9 12 13 or 14 are Ready In and Pin 5 and 6 are Start N O out TurboMatrix I O Port 14 13 Banani 12 e e 7 READY OUTC 10 READY OUT NO 9 aaa 8 7 EXT START HI 6 e 5 io EXT START LO 4 gt 31 GC 2 1 Figure 4 Connecting the HS to the AutoSystem XL GC using the Ready
267. sample The equilibration time cannot be predicted Therefore in the case of an unknown sample particularly if no previous information is available the required equilibration time must be established empirically You can do this by preparing a number of vials with the same sample thermostatting them for different times and then using identical analysis conditions and plotting the resultant peak area against the thermostatting time Particularly useful for time consuming kinetic measurements Headspace only is the automated progressive mode of thermostatting For details see The Options Tab in the Operation chapter The equilibration time should be the shortest time the sample has to be thermostatted The analytical result will not change if the thermostatting time is longer than the time needed for equilibration However excessively long thermostatting should be avoided because some samples may be sensitive to prolonged heating The equilibration time may be fairly long in fact generally longer than the analysis time Starting the equilibration of the second sample only after the analysis of the first has been accomplished will result in an unnecessary loss of time and sample throughput To eliminate this unnecessary time delay for routine analyses you can thermostat each sample for the same time and start it while the preceding sample is still being analyzed This is the overlapping constant mode of thermostatting You can only use over
268. sample is degrading Sample loss can also be attributed to polymerization depolymerization or decomposition Action Ensure the thermostatting time and temperature are appropriate for your application In the heated transfer line the headspace gas is a 317 Troubleshooting mixture of air with trace concentrations of the analytes Setting a high temperature may cause sample decomposition by oxidation Set the thermostatting needle and transfer line temperature accordingly Cause The original samples have not been prepared correctly Action Ensure that the sample was prepared correctly Le if you are using a diluted liquid sample ensure that you have the correct dilution ratio Cause The vials have not been sealed correctly Action Action Action Ensure the caps have been assembled and crimped correctly If you can turn the cap after it has been crimped it will leak Remove the cap and dispose of it Install another seal See Sealing the Vials in the Accessories chapter If the cap cannot be crimped correctly adjust the hand crimper See Adjusting the Hand Crimper in the Routine Maintenance chapter If the pressure in the vial is excessive the seal will begin to vent and result in sample loss When you are creating methods ensure that you set thermostatting times and temperatures that are suitable for both your sample and the solvent See Sealing the Vials in the Accessories chapter Unsafe high pr
269. ses the pre before sample injection focusing time during injection and post after injection cryofocusing times Pre Cryofocusing Time I I i pocung Post Cryofocusing Time Cryofocusing Time Injection Withdrawal Vent HS Analysis Time Time to Reach Cryofocusing Set Temperature New Analysis lt gt GC Analysis Time Time minutes Figure 66 Setting the Pre and Post Cryofocusing Time 173 Accessories Cryofocusing with the Water Adsorption Trap In cryofocusing using the water adsorption trap water is removed from the sample prior to enrichment This is done by adsorption onto a hygroscopic salt The schematic below illustrates how this functions during the injection phase Transfer Line Cooling N2 Liquid Nitrogen Water Adsorption Trap Cryo Tube GC Oven Figure 67 Cryofocusing with the Water Adsorption Trap Gas flows through SV7 in the direction of SV1 when the needle is in the vial Gas flows through SV7 in direction of the T union and adsorption trap when the needle is out of the vial 174 Accessories The water trap is backflushed automatically at the end of the withdrawal and vent time and it continues until the next vial is pressurized When you enable the water trap on the Options tab the HS switches SV7 on and off thu
270. t 130 Run Log 129 Loss of Sample 315 M Magazine Cap Nut 269 Cleaning 269 270 Full Fault 303 Motor Stalled Fault 298 Removing 269 Maintenance Alarm 138 Cleaning Needle 246 Cleaning the Magazine 270 Cold Trap 276 282 Leak Test 261 Magazine 269 Needle Seal Assemblies 247 O Ring Seals 252 Routine 235 Trap 282 Manual Introduction 15 Other Manuals and Reference Material 15 Material Safety Data Sheets MSDS 26 274 Mechanical Hazard 25 Messages Fault Conditions 297 Status 295 327 Method 350 Activating 134 Cannot Edit 308 Delete 134 Editing Disabled 138 Editor Tool 133 Multiple Method Operation 106 138 150 Pre selected Method Operation 138 Saving 134 Selecting from Run Tab 308 Single Method Operation 105 137 149 Method Development 185 Cryofocusing Temperature 193 Editor Tool 133 Injection Mode 207 Injection Volume 197 Needle Temperature 191 Pre PostCryofocusing Time 204 Shaker 215 Split Sampling 218 Thermostatting Temperature 192 Thermostatting Time 196 Transfer Line Temperature 191 Withdrawal Time 198 MHE Calculator 136 Shaker 117 Thermostatting 117 213 Mode Economy 144 Handshake 146 Injection 115 207 MHE 117 213 Temperature 111 191 Thermostatting 212 MSDS 26 274 Multiple Method Operation 106 N Needle Adapter Sleeve 248 Cleaning 246 General Information 243 Installing Transfer Line at Needle Unit 62 65 Lower Seal Assembly 249 Maintenance 243 Microbo
271. t edit the methods in any way HS 40 Emulation If you are using an HS 110 you can configure it to operate as an HS 40 If you enable this command only vials from the outer ring will be loaded and the crane will not be used In HS 40 emulation the load and unload positions are not reserved You can place samples in these positions You can use this mode if you are using low volume vials with adaptors or if you have fewer than 40 samples to run Show Use this option to hide the Relay option on the Timing tab If you need to program timed events to control external devices ensure that the Relay option is enabled Config Tab Carrier Gas Select the type of carrier gas being used and the units to be displayed when a pressure value must be entered to complete a method Number of Injections You can set the number of injections to be made before an indicator is displayed to the user that maintenance is required Once the needle maintenance has been completed as outlined in The Sampling Needle on page 243 then you can reset the counter by pressing the Reset button Maintenance Alarm The needle needs to be maintained periodically After every 500 injections the needle holder should be 138 Operation removed to clean the needle from abraded sealing material It is only necessary to change the sampling needle when it is damaged or when you wish to change to another needle type See The Sampling Needle on page 243 for needle ma
272. t stops Tighten the nut to hold the deactivated tube adapter in place Do not over tighten the nut as you may damage 65 Installation the ferrule or crack the glass in the deactivated tube adapter See Figure 9 9 Unravel approximately 1 meter of the fused silica tubing Insert the fused silica tubing from the GC end into the transfer line until approximately 5 cm of the line extends from the HS end of the transfer tubing 10 Slide the 1 16 sleeve nut and the graphite vespel ferrule onto the end of the fused silica tubing between the transfer line and the deactivated tube adapter Figure 13 Assembling the Fittings Ahead of the Deactivated Tube Adapter 11 Score and break the fused silica tubing to remove any graphite residue which may block the carrier gas flow CAUTION Do not break the column isolation flow connection This connection is very delicate take care not to break it 12 Push the fused silica tubing into the deactivated tube until it reaches the end Slide the ferrule and nut into position and tighten finger tight at the needle entry Tighten both nuts 13 Plug the other end of the fused silica tubing or column by forcing an injector septa on it Leak test the system before you finish assembling the transfer line See the Leak Testing procedure later in this chapter for details on performing a leak test 66 Installation 14 Slide the transfer tubing down so that the PTFE sleeve is within 1
273. tamination Disconnect the HS from the GC If the baseline signal drops to the normal detector background the HS is most likely the source of contamination Cause The carrier gas supply is a very common source of contamination in the headspace and the HS 40 110 trap Action Contaminants can be introduced through the gas itself cylinder regulators gas lines or carrier gas filters To establish whether or not this is the source of the problem change your tank of carrier gas the regulator and supply tubing If the problem persists contamination is likely entering from another source or the carrier gas is of poor quality 312 Troubleshooting Cause The needle or the transfer line are not hot enough and the sample is condensing Action Set the temperature of the needle and the transfer line to at least 10 C higher than the vial oven Cause The needle purge flow is below the acceptable range Action Check the needle purge flow and ensure the flow rate at the purge vent is 15 3 mL min See Checking the Needle purge Gas Flow in the Installation chapter of this manual If the flow is below 10 or greater than 20 mL min contact your PerkinElmer service engineer Cause The transfer line is contaminated Action Increase the flow of carrier gas through the transfer line set the transfer line temperature to its maximum 210 C temperature Allow the transfer line to purge overnight If you are using the on column conne
274. tched off but not disconnected from the AC outlet Wait at least one minute before opening the instrument after disconnecting it from the AC outlet Internal capacitors may remain charged for several seconds after the instrument has been switched off Do not operate the instrument with any covers or parts removed Servicing must be carried out only by a PerkinElmer Service Engineer or similarly qualified person Only persons trained and qualified in the use of the HS are authorized to carry out adjustments and maintenance described in this manual Line Cord Use only approved line cords with a protective ground conductor green or green yellow to ensure safe operation The line cord must be connected to a correctly installed AC power outlet with a protective ground earth terminal that conforms to the local safety code If the line cord plug has been installed by someone other than a PerkinElmer service representative ensure that it is wired correctly 23 Introduction Terminal Cord Lead Colors International USA Live Brown Black Neutral Blue White Protective Conductor Green Yellow Green earth ground Table 4 AC Line Cord Connections Servicing of incoming AC power line components in your laboratory must be performed by a licensed electrician Fuses Use only fuses with the required current rating and of the specified type for replacement For protection against fire hazard r
275. ted for the duration of the desorb time Dry Purge The trap is being purged with carrier gas to remove any air from it Ready The instrument is ready to begin an analysis Fault A fault is occurring Trap Cond Heat The instrument is in trap condition mode and the trap is being heated to the set point Trap Cond Hold The instrument is in trap condition mode and the trap is being held at the set temperature Trap Heat The trap is being heated to its high temperature Trap Hold The trap is being held at its high temperature Waiting for GC The primary desorption has been completed and the HS 40 110 trap is waiting for a GC ready signal before the cold trap is heated Table 14 Instrument Status Messages for Headspace and HS 40 110 Trap 296 Troubleshooting TurboMatrix Headspace and the HS 40 110 Trap Instrument Fault Conditions If there is more than one fault occurring at a time the instrument will cycle through them and display them one at time until they are corrected The following faults cause the instrument to stop immediately All heated zones are turned off and a message is shown on the display localizing the error Record the details of the failure before switching off the instrument Fatal error can only be remedied by switching the instrument off with the power switch waiting thirty seconds and switching it on again The instrument will then restart and attempt to initialize i
276. ted then you only need to enter the start and stop vials Press the Start vial entry box and then press the plus or minus button to select the desired start vial 4 Enter the desired end vial 5 Ifyou are running a single method then select vials and enter the start and stop vial number Choose the method to be used from the drop down box 6 The Start button should be green Press the Start button 7 The button will change to a red Stop button The Rotate button will also change to Priority The method can be stopped at any time by pressing the Stop button A confirmation pop up window will be displayed press Yes to confirm that you want to stop the run The analysis on the current vial is aborted and the vial will be unloaded and returned to the magazine The method will be interrupted and the instrument will revert to Standby Multiple Method Sequence Operation You can create a sequence of methods if you have varied applications Multiple method operation must be enabled on the Preferences tab You must also have created and tested all of the methods required for your sequence Your HS application may require the use of multiple method for analysis of multiple vials It is also possible to run a sequence of methods on a single vial if required To start multiple method operation 1 Select the Sequence option 2 Press the Start vial entry box and then press the plus or 150 Operation minus button to select the
277. that by extracting the whole amount of the analyte any effect of the sample matrix is eliminated and quantitative determination of the total amount present in the headspace vapor can only be calculated In practice you will not carry out the extractions indefinitely from a limited number of consecutive extractions the peak area corresponding to the total amount of analyte present is obtained by extrapolation based on mathematical relationships For the HS 40 110 trap Only The Operating Mode has the following choices in the drop down window in addition to the standard headspace modes e Trap Use the trap for concentrating the analytes onto the absorbent trap before injection into the GC column e Trap Clean without a vial uses high temperatures to vent the contaminants from the trap e Trap Test without a vial as a blank injection is made into the GC where the material from the trap only using the trap high temp is sent down the column for analysis Shaker The shaker can decrease the time needed for equilibration by providing continuous mixing of the sample in the vial during the equilibration process When applying the shaker it is important that the sample be in resonance with the shaker frequency to obtain the desired mechanical mixing effect In the case of liquid samples the 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 p 40 41 215 M
278. the door Loosen and remove the knurled needle nut Lift the needle holder out of the rack Loosen the securing nut and pull the needle out NAF YW Place the new needle in the needle holder nut The top of the needle will butt up against the bottom of the needle holder 7 Tighten the needle holder nut The nut must be finger tight 8 Clean the needle with a lint free cloth or tissue If necessary dampen the cloth slightly with methanol 9 Carefully slide the needle holder with the new needle back into the rack as far as the stop CAUTION Do not touch the lower half of the needle with your fingers 10 Rotate the needle so that the holes line up with the transfer line 245 Routine Maintenance 11 Securely hand tighten the knurled nut 12 Close the front panels and reconnect the instrument to the electrical supply 13 Turn off the column isolation flow by pressing Done on the touch screen Cleaning the Jet Needle Abraded sealing material from the vial septa may stick to the needle and can cause the needle to seal incorrectly during pressurization and withdrawal A needle coated with sealing material may also lead to unnecessary wear on the o rings contained in the needle seal assemblies The recommended interval for cleaning the needle will depend on the needle temperature and the type of septum being used The minimum interval should be 500 injections Avoid unnecessarily high needle temperature
279. the Leaks It has been found that the quickest way to find leaks is to systematically section off the instrument to isolate the leaking area and then to reassemble that section identified as having the leak one piece at a time until the one defective piece is identified and replaced Log Error Messages Fast pressure decay Cause Vial has a larger sample volume than the calibrated curve vial is incorrectly capped or a leak has developed in the instrument Action 1 Check sample volume use a new carefully sealed vial then check for system leaks 2 Recalibrate vial decay and check obtained curve with 324 Troubleshooting the provided guide Slow pressure decay Cause Vial has less sample than the calibrated curve or is at a higher pressure than the calibrated curve SV9 valve could have failed or the slide valve Dry Purge outlet is closed Action Recalibrate vial decay and check the new curve with the provided guide 1 Check slide valve pulled forward is open 2 If itis still failing call your PerkinElmer Service engineer to replace the SV9 gt Poerkinebner wrong lample volume or wrong rampis volume Figure 131 Pressure Decay in Vial with a Fixed Flow Venting Extended therm Trap Cause The trap was above the low trapping temperature when the sample should have been loaded onto the trap Action Increase the GC cycle time to allow the instrument time to cool the trap down prior to
280. the flow meter If the flow rate is less than 10 or greater than 15 contact your PerkinElmer service engineer Leak Testing the Headspace TurboMatrix Headspace Only If a leak is occurring and you cannot isolate the source you may want to separate the HS headspace from the GC and leak test each instrument separately Once each instrument is found to be leak tight you can then connect them and test them together The automated leak test will leak test the HS sampling system You must plug the end of the fused silica tubing or if the fused silica tubing is directly connected to the GC column then plug the end of the column To leak test the sample injection system 1 Switch off the gas chromatograph and let the instrument cool down Use a blanking plug to seal the column outlet Seal capillary columns with a new clean septum Set the carrier pressure to 45 psi See the section on Carrier Gas earlier in this chapter Open the Tools drop down menu and select Maintenance and then select Leak Test If the leak test fails you will get the following screen Go to step 8 for the procedure for a failed leak test NOTE The first screen on the following page shows a failed test red text indicates a failure and the second screen shows a passed test black text indicates a success 86 Installation Run Status Log d Dry Purge Trap Hold Initial Final Pressure Pressure psi psi Tests Gas Leak 33 16 2931
281. the next injection Alternatively if the user parameters allow it may be possible to adjust the thermostat and trap times desorb and hold so that the trap is at the appropriate temperature 325 Troubleshooting when required See the following figure the Log tab vial 14 GC not ready Cause GC did not come ready prior to the trap Desorb step The instrument will then wait until the GC becomes ready before the trap will fire Action Increase the GC cycle time Run Status Log Log Repor J Oven Status Run Log Jul 29 2003 09 52 53 a Instrument Senal HS 00000000000 Instrument Name heather Method default Vial Themo Inject Status Pressure decay OK vial 13 13 09 53 34 09 55 34 Done Extended Therm Trap Not Ready Pressure decay OK vial 14 14 09 56 17 09 59 34 xThermo Extended Therm Trap Not Ready Fast pressure de vial 15 15 10 00 12 10 03 34 xThermo Run Stopped STANDBY 10 05 12 DSt Rotate Toos v Figure 132 Action Log Tab Information on the vials already run 326 Troubleshooting Status Messages Error Messages Description TC MIN FAULT ZONE 4 Trap has gone below lowest allowed temperature Call your PerkinElmer Service Representative TC MAX FAULT ZONE 4 Trap has exceeded highest allowed temperature Call your PerkinElmer Service Representative HTR RATE FAIL ZONE 4 HEATER FAIL ZONE 4 Trap rise error rate of temperature change is
282. this method You can change the settings and then save the revised method 119 Operation Run Status Log Carrier 35 0 psi Transfer 750 gi Trap Oven Hi ar 70 C lof c Actual btexsplitles Temp Timing Option Ippe STANDBY Aug 14 __ Start Rotate Tools x Figure 39 HS 40 110 Trap Status Page Temp Tab 120 Operation Status Tab Timing Tab for the HS 40 110 Trap The Timing tab on the Status tab for the HS 40 110 trap offers some options for the trap Run Status Log Dry Purge Trap Hold eed 5 0 5 0 Setup min min y min saaa Pil _ 23 0 Relays man Col Blank_Te LJ LE JTemp Timing Option Jppe STANDBY 12 55 02 Stat Rotate Tools x Figure 40 HS 40 110 Trap Status Tab Timing Tab Dry Purge This option allows you to input the number of minutes required for the dry purge The dry purge allows for helium to purge the trap of water at the lowest trap temperature entered and at the desorb flow rate The amount of time needed for the dry purge will vary depending on the thermostatting temperature the type of sample you are running and the Headspace Trap Cycle time If the FID extinguishes during your analysis you will have to increase the dry purge time The Trap Dry Purge range of values is 0 1 99 min in steps of 0 1 min The Trap Dry Purge is carried out under a pressure equal to the used in the Desorb step The Desorb
283. tic Control Accessory 167 Pressure Fault 297 Pollution Degree IEC 1010 22 41 Poor Recovery 315 Port Carr In 78 Dry Air Inlet 78 Input Output 49 RS 232 54 Power Consumption 44 Powering up the Headspace Sampler 98 PPC Accessory 167 Calibrating Module 275 276 Carrier Pressure Control 118 128 Configuration 117 217 Pressure Control 118 128 Tab 117 217 Zero Module 275 276 Pre Post Cryofocusing Time 114 204 Pre Cryofocusing Time 205 Preferences Tab 107 136 Pre Injection Preventing 222 Pre Installation Checklist 38 Preparation Status Message 295 Pre selected Method 138 Pressure 132 Delivery for Carrier Gas 76 Delivery for Dry Air 77 Gauge 195 High Pressure Sampling 208 352 Setting Carrier Gas 100 Pressurization Phase 186 Time 112 122 Pressurize Time 295 Principles Cryofocusing 172 Headspace Analysis 185 Priority Vials 142 Progressive Thermostatting 116 214 Protection Electrical 22 PTFE Coated Butyl Rubber Septa 179 Coated Silicone Septa 180 R Ready In Signal 53 Out Signal 51 Ready Start Cable 55 HP6890 Cable Assembly 57 Reduced Sensitivity 315 Reference Material 15 Regulator Safety Practices 28 Regulator Safety Practices 28 Relays 163 Show 138 Timed Event 54 Removing Jet Needle 243 245 Magazine 269 Report Log 129 Reproducibility Test 239 Requirments AC Outlets 44 Power 44 Reset Command 136 Routine Maintenance 235 Cleaning Needle 246 Leak Test 261 Needle 243 Ne
284. time it closes the SV1 and SV9 to stop the carrier gas to the Trap the Sampling Head and the Needle 289 Routine Maintenance I gt PerkinElmer Manual flow controller is adjusted to give column flow rate 5m Lmin Flow away from column inlet stops air from entering column bolation valve controls operation and will open during oy oie PON Figure 126 Column Isolation Flow NOTE Although PPC pressure is shut off you will still measure a small flow 5 9 ml min at the Needle Purge and Trap Dry Purge outlets This is due to the Isolation Flow which entering the Sampling Head splits in to three branches i e to the Transfer Line GC column to Needle Purge and to the trap and its Trap Dry Purge outlet If you have an MS detector you will also observe an improvement in the vacuum as the column flow is now considerably decreased See the following figure This configuration will allow servicing and replacement of the trap the needle and the upper and lower needle sealing o rings 290 Routine Maintenance fd Isolation Flow protects Hier Line amp GC Column B VALVE STATE TABLE SV STATE la on 1 on 2 OFF 8 OFF 9 OFF SY1 amp SY99 are dosed No carrier gas to Trap and Sampling Head Needle to allow their mainterancereplace ment Figure 127 Before starting the maintenance cool down the area you intend to work in Oven Needle Trap Press the Start button to switch
285. tion is maintained 14 13 o 12 e 11 J 10 9 e To GC External Start 6 5 4 e 3 J 2 Pin 1 TurboMatrix I O Port Figure 2 Connecting the Fail Output Signal in Parallel with the Start Signal NOTE Depending on the configuration of the external instrumentation it may be more appropriate to connect the Fail signal elsewhere e g to a data handling system Many variations are possible Use of the Fail signal to start an external device and maintain synchronization depends on the device having completed its previous run and being in a state from which a blank run can be started 52 Installation BCD The number of the vial in the analysis position the rear most position on the carousel is available in BCD form Each digit is signaled by relay contact closures between the appropriate pins and Common Out See BCD Interface on page 165 NOTE The options board is required in order to use BCD signals This board is standard on HS 110 and Trap instruments Figure 3 BCD located at the back of the instrument HS Input Signals Ready In The HS can determine the status of external instrumentation using the Ready In signal A relay contact closure or equivalent within the external device connected between pin 9 Ready In and Ground pins 12 13 or 14 indicates to the HS that the GC is ready to start See Figure 1 The HS examines the status of the external device at several times d
286. tions 46 Tubing 46 Carryover 310 Changinf O Rings 252 Changing Fuse 241 Jet Needle 243 245 Lower Needle Seal 249 Upper Needle Seal 247 Checklist Installation 37 Pre Installation 38 Checksum Fault 306 Chemical Equilibrium 185 MSDS 26 Safety Information 26 274 Chromatography Broadening or Splitting Peaks 309 Circlip Pliers 272 Removing 272 Cleaning Jet Needle 246 Magazine 269 Cleanliness Laboratory 236 Closure Assembly 177 Cold Trap Conditioning Mode 282 Maintenance 276 282 Removing 277 Column Direct Connnection to HS 71 On Column Connnection to HS 72 Sampling with a Packed 227 Sampling with Wide Bore Capillary 226 346 Splitless Connnection to GC 71 Command Activate 134 Delete 134 Exit Method Editor 135 Method Editor 133 New Method 134 Open 134 Reset 136 Save Save As 134 Test 135 Composite Zero Dilution Liner 168 Compressed Gases Handling 28 Regulators 28 Safety Information 28 Conditioning Cold Trap 282 Trap 282 Config Tab 138 Connection AC Line 45 Carrier Gas 75 76 Direct 101 224 Dry Air 75 77 HS to Any GC 56 HS to AutoSystem XL 55 HS to GC 46 49 HS to HP 5890 6890 57 On Column 102 224 Pneumatic Ports 78 Tab 145 Constant Thermostatting 212 Contamination Carrier Gas 312 Sources 312 System 312 Transfer Line 313 Control Software 180 Crimper 176 Adjusting 271 Stop Pin 271 272 Cryo Test 135 Cryofocusing Accessory 172 Cannot Enter Pre Post Times 309 Cryo Test 205 Method Develop
287. ts branching of the decay flow to the Transfer Line GC column and maintains the flow down the column 187 Method Development Dry Purge Phase This phase allows you to input the number of minutes required for the dry purge The dry purge allows helium to pass over the trap to purge the trap of water The amount of time needed for the dry purge will vary depending on the type of sample you are running and the HS Trap Cycles number Desorb Phase The Desorb phase is the time for the sample to be desorbed from the HS 40 110 trap and focused onto the GC column The figure below is a generalized plumbing diagram 1 L Isolation Flow 6 3 2 way solenoid valve 4 Pressure transducer 5 3 way solenoid valve 6 Flow controller 7 Adsorbent trap 8 2 way solenoid valve 9 J vay solenoid valve 10 Fized restrictor 11 Fixed pressure regulator 12 Charceal filter 13 Pressure transducer 14 Solencid valve 15 PPC Pressure regulator 16 Pixed pressure regulator 17 fixed restrictor 18 Cartier gas supply 19 Sample vial 20 65 sampling head 21 Sampling needle 22 Chromatographic column zE Trap Dry Purge All solenoid valves are shown in their relaxed ricall states Figure 73 188 Method Development Creating a New Method To create a new method 1 Press the Tools button and then select Method Editor from the drop down box To create a new method press the New butto
288. tself If the error recurs please make note of the exact wording of the error message and contact your PerkinElmer service engineer Before you contact service ensure you have the following information e What you were doing when the error occurred e Any corrective action that you have taken e The exact wording of the error message and any numerical error codes e Additionally you should have this manual at hand Fault Pneumatic Psi Too Low Cause The supply of dry air used to drive the automated vial handling components has run out Action Replace the tank of dry air Open the tank and set the delivery pressure to 90 psig See the Gas Connections section in the Installation and Setup Chapter for details Fault Carrier Psi Too Low Cause The supply of carrier gas has run out Action Replace the tank of carrier gas Carrier gases require a minimum purity of 99 995 Open the tank and set the delivery pressure to 90 psig See the Gas Connections section in the Installation and Setup Chapter for details 297 Troubleshooting Fault Magazine Motor Stalled Cause An obstruction has caused the magazine to halt rotation Action Turn the HS off and disconnect the power cord from the AC mains Remove the obstruction and reconnect the line cord Turn on the HS The instrument will initialize the motors It will then return a Ready status if all of its systems have been initialized correctly You must update the vial r
289. ttendn tenia ess 212 Operating Modes Headspace Only 0 212 Number of Injections cccceeccesseceeeeeeneeeeteees 214 USSF casera ston ascii an e eee tans s 215 PPC Taboe shecta te costae Mest ne eea DE E a Ranai 216 Split Sampling Headspace Only 218 Splitless Sampling cece eeseceeeeeeeeeeeeneeeeeees 223 Splitless Sampling with the HS 40 110 Trap 8 gece hacen 225 HS 40 110 Trap Theory 0 cece eeeeeeeeeeereeeneee 225 Headspace Sampling 0 eee eeceseceseeeeeeneeeneeees 226 With Wide Bore Capillary Columns 226 Headspace Sampling 0 cece ceeceeeeeeeeeeeenseeeeees 227 Using a Packed Column and a Packed Column Injector ceeeeeeeeeeee 227 MHE Theory and Calculations Headspace Only oserei ano uni anness 229 Routine Maintenance s snsennsennesenrnnnnnnnnnn 233 Introductions isesi aeaee ae a thats 235 General Laboratory Cleanliness 236 Cleaning and Decontamination eee 236 Cams asda t r E EERE 236 Decontamination cccecceeeseesseeseeeeceaee 237 Cartier Gas Jaroor ten ae E ai eaei 237 Tubie onra iip aw eos 237 Sample Vials and Seals cee ceeeeeeeeeeeseeeeeeees 238 Important Carrier Gas Shut Off eee 238 Reproducibility Test Headspace eeeeeeeeeeee 239 Contents Changing the Fuse ccecsccsseceeceeseeeeseeenaeceaeeeees 241 The Sampling Needle ee eeeeseceeeeeeeereeereeeneens 243 Types of HS Needles 0 cece eee eseeseceneceseeeeeee
290. tude in the range 0 m to 12000 m When you remove the instrument from storage allow it to stand for at least a day under the approved operating conditions before putting it into operation 40 Installation Other The laboratory should be free of flammable explosive toxic or corrosive vapors Always provide adequate ventilation When analyzing hazardous compounds it may be necessary to arrange for venting the detector effluent into a fumehood Gas cylinders should be located outside of the laboratory whenever possible All gas cylinders should always be stored and operated in the vertical position and should be firmly clamped to a suitable surface Care must be taken not to kink or stress the gas delivery lines Installation Category The HS is able to withstand transient over voltage according to Installation Category II as defined in IEC 1010 1 Pollution Degree HS will operate safely in environments that contain non conducting foreign matter up to Pollution Degree 2 in IEC 1010 1 Table 6 Required Environmental Conditions Space Requirements for the Instrument You should leave sufficient room around the instruments to access all of the connections at the rear and reach the electrical supply points See Table 7 for the space requirements Dimensions HS 16 43 cm 17 wide x 61 cm 24 high x 58 23 deep HS 40 43 cm 17 wide x 61 cm 24 high x 61 24 deep
291. uL Cooling increases the partition coefficient of the volatile components in the stationary phase they thus pass through the column more slowly than the carrier gas while the air contained in the sample continues to flow at the same speed as the carrier gas In this way the components of interest are separated from the original large volume of air contained in the original sample and pre concentrated at the head of the column Principle of Operation In the cryofocusing technique a portion of the quartz capillary column is fed through a PTFE tube through which a coolant gas is passed in the opposite direction to the carrier gas in the column The coolant gas is cooled by passing it through a copper coil immersed in a Dewar vessel containing liquid nitrogen The gas flow is metered by a valve connected to the HS For efficient cooling during cryofocusing the temperature of the GC oven should be as low as possible 172 Accessories Pa Transfer Line HS PTFE Cryofocusing Tube Nitrogen GC Oven Figure 65 Cryofocusing Accessory The pre cryofocusing duration allows the head of the GC column to cool to the set cryofocusing temperature The post cryofocusing time maintains the head of the column at the low temp until the sample has been collected and unretained compounds have cleared the column These values are determined when optimizing the cryofocusing The total cryofocusing time compri
292. uld not replace the sampled vial on the magazine Action If you have placed a new vial into the location from which a vial was removed by the instrument you must remove it Press Stop and rotate the magazine to gain access to the magazine location and remove the vial Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses Cause If there has been a power failure it is possible that a vial has slipped from the crane arm Action Turn the HS off and disconnect the power cord from the AC mains Remove the vial from the unload position Turn on the HS You may need to update the vial range on the Run tab to exclude the vials that have already been run Press the Start button to continue your analyses Fault Magazine Full Cause You have placed vials in the load and unload position of the HS 110 or in the unload position of the HS 40 Action On instruments with the 15 vial oven it is 303 Troubleshooting possible to turn the instrument off while vials are still in the oven When the instrument is turned on again it will attempt to unload the oven You must provide an empty spot in the outside ring of the magazine so that the HS can unload the oven When you are loading the HS 40 you can place vials in all positions except for one You must leave one spot open in order for the HS to unload any vials that may be present
293. ure that you have the proper adapter kit and start ready cable to connect the HS to your GC and contact your PerkinElmer Service Representative for advice If you are using the cryofocusing accessory you need to obtain a supply of liquid nitrogen and a suitable Dewar vessel Review this manual and write down any questions that arise Contact your local PerkinElmer office to answer your questions or provide an alternate source of information 39 Installation Laboratory Requirements Operating Environment WARNING This instrument is not designed for operation in an explosive atmosphere General The site for the instrument must be Indoors as the HS is designed for indoor use only e Free of dust smoke and corrosive fumes e Smooth level and free from vibration Temperature Ambient temperature between 10 and 35 C 50 and 95 F Safe operation 5 to 40 C In addition the site for the instrument must be e Free of drafts e Out of direct sunlight e Away from radiators and heaters e Away from heating and air conditioning ducts as they will affect thermal stability Humidity 20 to 80 relative humidity non condensing Altitude Sea level 0 metres to 2000 m Storage You can store the instrument safely under the following conditions e Ambient temperature 20 to 60 C 4 to 140 F e Ambient relative humidity from 20 to 80 non condensing e Alti
294. uring a sequence including before a sample vial is loaded and before injection If a Ready signal is not received at these times the HS status message Ready To Inject appears and the HS waits until the Ready signal is received 53 Installation If overlapping thermostating is selected GC ready signal is examined only before sample injection Start In and Stop In The inputs are handshake signals that are currently not used by the instrument RS 232C Port This port operates at 9600 baud and is intended for computer communications It can be configured through the Preferences tab See Preferences Tab Headspace and HS 40 110 Trap on page 136 Refer to the HS Control Software manual for details on connecting your computer to the HS Timed Event Relays If you will be controlling external devices through the relays on the options board and timed events you must first connect the external devices to the HS and then program the events The relay contacts are rated to switch 10 W maximum Do not exceed 50 VDC or 0 5A External devices include external switching valves audible alarms very small motors etc Take care when you connect or disconnect the voltage outputs WARNING To connect external devices to the relay contacts 1 Turn off the HS and disconnect it from the line supply 2 Disconnect the I O connector 3 Connect your external devices to the appropriate connector contacts Insert the wire lead
295. uring servicing of the headspace and trapping system 225 Method Development even when the headspace instrument is turned off This feature is particularly useful when mass spectrometric MS detection is being used with the GC With the introduction of a trap some modifications have been made to method development The Method Editor has fields relating to the trap in each of the tab pages Temperature Times Option and Pneumatics See the Operations chapter of this guide for more details on modifying the Method Editor for the HS 40 110 trap Headspace Sampling With Wide Bore Capillary Columns Wide bore capillary columns with an I D of 0 53 mm generally do not have sufficient flow resistance for direct pneumatic headspace sampling The sampling pressure must exceed the headspace pressure in the vial after thermostatting to avoid uncontrolled pre injection If the column you are using requires a low inlet pressure while the headspace sampling pressure must be kept at a higher level you have two options When you are using a split splitless injector in the GC the required pressure drop can be established across the transfer line by setting a large split flow When you are using a packed column injector with no split function or a direct connection from the transfer line to the column the required pressure drop can be established across a flow restrictor attached to the outlet of the GC column A restrictor is recommended
296. urn off the gas supplies to the instrument In the case of direct or on column connections ensure that the flame is out and that your oven injectors and detectors are at room temperature Pull gently on the magnetic door release to open the door 247 Routine Maintenance Adapter Sleeve Tool Torsion Bar B013 5485 248 Knurled Nut _ gt Needle Holder gt with Needle Adapter Sleeve Needle Unit Upper Assembly Seal Assembly M3 Hole 4 Ea Upper Seal use O ring assembly tool to remove the upper seal o ring Figure 97 Changing the Upper Seal Assembly 6 10 Remove the needle holder and the needle as outlined in Removing and Replacing the Needle Headspace Only on page 243 Blow filtered carrier gas through the needle Screw the O ring assembly tool P N B013 1410 into the threaded hole M3 of the upper needle seal assembly Loosen the adapter sleeve with the adapter sleeve tool P N M041 5330 You will gain access to the adapter sleeve through a window in the needle unit drive assembly Use the tool to turn the adapter sleeve counterclockwise left to right facing instrument This lifts the adapter sleeve up and allows you to remove the seal assembly Using the seal removal tool gently pull out the needle seal assembly If the seal assembly cannot be removed then loosen adapter sleeve further NOTE NOTE Routine Maintenance 11 Replace the o ring
297. ve 500 kPa this slot is deformed and an artificial leak opens venting the internal pressure to atmosphere This safety closure requires flat septum disks and will not work with rubber stoppers l 1 Bruno Kolb and Leslie S Ettre Static Headspace Gas Chromatography Theory and Practice New York 1997 Perkinelmer P N N1011210 p 51 178 Accessories The most common source of sample loss or degradation is poorly sealed vials If your application requires sealing more than 10 vials on a daily basis you may want to consider the bench top or electric vial crimper to ensure your vials are sealed correctly Seals The seals are manufactured to high standards and made of carefully chosen materials Because of this the amount of residual volatile that may evaporate at higher sampling temperatures is minimized Ensure that the seals do not become contaminated once the bag is opened Your lab atmosphere may be loaded with many volatiles that can contaminate the seals and vials Don t touch the face of the seal that will contact the sample It is good practice to handle the seals with tweezers or forceps only Do not use your fingers For trace analysis best results will be obtained when the seals are preheated for up to 12 hours at sampling temperature In this case you must ensure that the seals don t touch each other and are well ventilated in a clean atmosphere Using a nitrogen atmosphere will decrease the possibility of conta
298. x contains protective circuitry Contact PerkinElmer Service before performing AC line tests Mechanical Hazard When working with the instrument please observe the following e Keep your hands clothing and other objects away from the moving parts of the instrument e Do not operate the instrument without the safety covers 25 Introduction e Do not touch any moving parts e Do not load or unload the magazine while it is in motion Chemicals Some chemicals used with this instrument may be hazardous or may become hazardous after completion of an analysis Do not store handle or work with any chemicals or hazardous materials unless you have received appropriate safety training and have read and understood all related Material Safety Data Sheets MSDS Use store and dispose of chemicals that you require for your analyses in accordance with the manufacturer s recommendations and local safety regulations You must comply with all federal state and local laws related to chemical storage handling and disposal MSDS sheets provide information on physical characteristics precautions first aid spill clean up and disposal procedures It is good practice to familiarize yourself with the information on the MSDS sheets before using any chemical substances You must work under a suitable hood when handling and mixing certain chemicals The room in which you work must have proper ventilation and a waste collection syst
299. xternal supply To avoid nuisance tripping of excess current protection devices do not supply power to the HS through fast acting circuit breakers In addition it is recommended that when you switch off the power to reset the HS that you wait at least 30 seconds before restoring the power This enables the thermistors to recover This information refers only to excess current protection devices Any tripping of devices that detect current running to ground for example earth leakage circuit breakers ELCBs residual current devices RCDs etc is due to a different mechanism Such occurrences must be investigated by a qualified person with expertise in electronics 45 Installation Connecting the HS to a Gas Chromatograph Connecting the HS to a gas chromatograph involves the following procedures 1 Connecting the gas supplies to the HS Making the electrical connections Installing the heated transfer line Connecting optional accessories Connect AC line cords Leak testing the system SOD eR uN Performing a test run to ensure all system components are operational The HS Gas Chromatograph configuration may vary slightly depending on the type of GC that you are using and on your application The HS is controlled from a computer PC or from its own touch screen keypad Control lines ready and start signals are provided to synchronize the HS the GC and the data acquisition system Gas Supply System Due t
300. y Make sure the following safety measures are observed when dealing with liquefied gases e Do not touch the liquefied gases e Always wear protective clothing gloves face mask safety glasses when handling liquefied gas e Secure the Dewar vessel so that it cannot tip over e Protect the Dewar vessel from any damage and from sources of heat The Dewar vessel must be fitted with a pressure relief valve e Cold vaporized nitrogen is heavier than air and can thus collect in low lying parts of the laboratory representing a suffocation risk Waste Disposal If the materials being sampled are hazardous in any way you must treat the collected samples and the vials that contained them as hazardous waste Used vials and seals may contain small amounts of the substances that were analyzed and may thus constitute a chemical or biological hazard Refer to your local safety regulations for proper disposal procedures 30 Introduction WEEE Instructions for PerkinElmer Products or A label with a crossed out wheeled bin symbol and a rectangular bar indicates that the product is covered by the Waste Electrical and Electronic Equipment WEEE Directive and is not to be disposed of as unsorted municipal waste Any products marked with this symbol must be collected separately according to the regulatory guidelines in your area The objectives of this program are to preserve protect and improve the quality of the environment p
301. yses Fault Vial Load Failure 302 Cause The HS could not load the vial from the magazine Action Action The vial has not been capped correctly Press Stop and rotate the magazine to gain access to the vial location Recap the vial and place it on the magazine Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses If the vial is stuck in the magazine remove it and clean the outside of the vial Ensure there is no adhesive material or residual sample on the outside of the vial before inserting it into the magazine Open the Preferences menu and select Reset The instrument will reset itself and clear the fault Press the Start button on the display to start the analyses Troubleshooting Action Do not use vials and seals that are not specifically identified for use with an automated headspace sampler Using other types of vials may result in unreliable analysis data or damage to the instrument Action If you are using the low volume 9mL vials you must install the low volume vial adapters P N N612 0110 in the magazine If you are using HS 110 you can only use the low volume vials and adapters in the outer ring Action The magazine is not rotating correctly It either overshoots or does not reach the target position Contact your PerkinElmer service engineer Fault Vial Unload Failure Cause The HS co

TurboMatrix Headspace Sampler and HS 40/110 Trap User's Guide

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