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Chapter 1 TRACE GC Ultra Configuration

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1. How To K Meeting FID Specifications One uL of the test solution is injected at 20 ug ml in hexane of C12H26 C14H30 and C16H34 A real time plot will be visible under the home page without the Mass Spec TIC A representative chromatogram is shown below in Qual Browser Sei a Jl AEE sali ll el ee E ziel gl e a s GES Si Si Sot eg 10 0416 99 02 22 32 RT 0 00 9 50 Ra hargo of 1 oe E Mass Range no file pannel Bd Mors Range E no fie 1 e S Zen E Mass Range no file J jo zi 2 Mass Range no file 905 19K Mass Range no file J 804 704 2 oo A so Z ai J RT 4 75 RT 6 00 305 RT 3 35 AA 3585935 MA 3589938 J AA 3520699 AH 2628313 MH 2537825 gd AH 2040164 SN 86 SN 57 207 SN 41 104 NE ce ir TEE TT Tt TTT TTT 0 1 2 6 F 8 Time min 1 uL of the FID test solution is injected in the split splitless inlet with an injection time of 1 0 minute The FID gas flows were set to hydrogen at 30 ml min air at 350 ml min and makeup at 30 ml min nitrogen The FID detector base temperature was set to 250 C and the inlet to 230 C The range was put on 1 The spec calls for area counts gt 3 500 000 for each component The ratio of C12H16 C16H34 must be 1 0 0 1 If the column was installed correctly and the injection time is set to 1 0 minute or less a sharp front and back for the solvent peak should be seen The peak shapes should be symmetrical 4
2. Glossary linear velocity liquid chromatography negative ion on column injection on column injector 5 124 positive ion X point of the solvent during desolvation while the vent valve is open A high carrier gas flow rate sweeps the more volatile solvent out the vent valve while the analytes remain coated on the pre column The vent valve is then closed and the oven temperature programmed up to vaporize the analytes for transfer into the analytical column See also injection mode temperature programmable injector and on column injector The rate of movement of the carrier gas through the GC column measured in cm sec See also flow rate and flow control A form of elution chromatography in which a sample partitions between a stationary phase of large surface area and a liquid mobile phase that percolates over the stationary phase As components elute from the chromatographic column they flow into a detector and generate a signal The characteristic time each component elutes from the liquid chromatograph and enters the detector is called the component s retention time An atom radical molecule or molecular moiety that has gained one or more electrons acquiring an electrically negative charge The charge state becomes 1 2 3 etc depending upon the number or electrons acquired See also positive ion and ion polarity Sample injection directly inside the capillary column rather than in a liner locat
3. 4816 KB Breda 31 076 587 8722 P R China Thermo Finnigan China Suite 912 916 Ping An Mansion No 28 Jin Rong Street Xicheng District Beijing 100032 86 010 6621 0839 Spain Thermo Finnigan SA Acer 30 32 Edificio Sertram Planta 2 Modulo 3 ES 08038 Barcelona 34 093 223 0918 Spain Thermo Finnigan SA Avenida de Valdelaparra 27 Edificio Alcor Planta 2a ES 28108 Alcobendas Madrid 34 091 657 4930 Sweden Thermo Finnigan AB Pyramidbacken 3 S 141 75 Kungens Kurva Huddinge 46 08 680 0101 United Kingdom Thermo Finnigan Ltd Paradise Hemel Hempstead Herts HP2 4TG 44 01 442 233 555 Notes The country code is enclosed in square brackets The city code or area code is enclosed in parenthesis For countries other than the U S A when you are dialing from within the specified country dial the 0 of the city code For countries other than Italy when you are dialing from outside the country do not dial the 0 of the city code Copyright 2002 Thermo Finnigan a member of the Thermo Electron family of companies All rights reserved Printed in Italy X Contents Chapter 1 TRACE GC Ultra Configuration E 7 Introductio BEE 8 To open this view 8 General E 10 IEN SEN 11 Detectors and Data Pages ricecon reee Eea E R E EE EES E ec aetna 13 Aux E 15 Road Map Home Page Status Tabs scc cscsciscuasscescteotevetedscesvnseaueungnecovedanev
4. Packed sl Figure 3 9 PPKD Page View Related topics e Setting Up Parameters for PPKD PPKD Page Parameters Inlet Group Box Temperature check box This is the temperature setting for the purged packed column PPKD inlet and textbox The allowable entry range is 30 400 C This temperature is usually selected to be 20 above the evaporation temperature for all components of interest in the analysis sample Optimum temperature for an analytical method varies with the method and sample requirements The entry also has a check box for on off values so that the temperature setting may be turned off without affecting the setpoint usually used for troubleshooting purposes 3 60 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Constant Septum Purge check box Stop Purge Time text box Surge Pressure text box Surge Duration text box Wide Bore mode Packed mode Thermo Finnigan Purge Group Box This entry allows the septum purge flow to be turned off for a specified amount of time after injection Allowable entries is On or Off If you select On using a needle to penetrate to a normal injection depth then you will see little sample loss If the constant septum purge box is unchecked specify the time after injection that the septum purge flow is turned off Keep the flow off for the minimum time amounts so those septum bleed products are not transferred onto the analytical column
5. Flow Time Ramp On Yes No Off Mode Type Clear Enter AW 0 9 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu X Information Keys Method Storage and Automation Keys Thermo Finnigan Status Info Diag Run Log Load Store Method Seq Edit Active Run Table Clock Table Auto Sampler Valves Seq Control Look for specific instructions for operating each key in the TRACE GC Ultra Operating Manual Chapter 2 Flow Calculator Column Flow Calculator allows you to make changes in non DPFC pneumatics which affect carrier gas flow and velocity Additionally you may e Change the column length id inner diameter temperature or inlet pressure by moving any of the Column Parameters slider bars will change the calculated values for flow velocity and hold up time Changing outlet pressure or carrier gas type will also result in recalculation of the carrier flow and velocity but they are set on different parts of the screen because they are less likely to be varied during method development than the other column parameters e Change the Carrier Gas Parameters slider bars for either flow or linear velocity will calculate the inlet pressure needed to give that flow rate or velocity keeping the other column parameters constant e See the Flow linear velocity and hold up time simultaneously when a column parameter changes While all calculations are solved directly
6. Gas Parameters group box Slide the slider bar to the desired column length in meters Slide the bar to the columns inside diameter in millimeters Slide the bar to the oven temperature you want to use C Slide the bar to the pressure amount to supply to the column head k 2 25 TRACE Gas Chromatograph Setup User s Manual TRACE Menu 1 Atm Vacuum Other Outlet Pressure Gas type Flow Velocity Holdup time Quick tips 2 26 Column outlet pressure group box Atmospheric pressure Select this if your TRACE is connected to a mass spectrometer Select this if you want to adjust column outlet pressure above or below atmospheric 0 43 5 psi Slide the bar to the desired pressure amount the column flow will push against at the column exit Carrier gas parameters group box Select the type of gas you are using for column flow Actual flow calculated based on items listed in Column Parameter box This is the speed in which the flow travels to the column Time for non retained peak to travel through the column Hold up time is measured to determine the average linear velocity Using slider bar and buttons Slider Bars Click here to display the main topic for this procedure You might hear the slider bar referred to as a scroll bar But whereas scroll bars typically scroll vertically slider bar scroll horizontally Use the slider bar to adjust the displayed values dom 98 e Grab click and ho
7. Right PTV Right Carrier Left FPD Right TCD Run Table m Detector r Signal IT Flame On Range 1 e M Base Temperature C 250 E Anala Filter V FPD Temperature C 150 PMT Voltage Low e Flow ml min I Air e T H2 a I Makeup 2 Figure 3 16 FPD Page View Related topics e Setting Up Parameters for FPD FPD Parameters Detector Group Box Flame On Select this control to turn the detector ignition and detector gases on Base Temperature Select to set the detector base body temperature For an FPD set at 250 C FPD Temperature Sets the detector cell temperature A typical operating temperature is 180 C PMT Voltage Sets the value for the dynode voltage to apply to the photo multiplier table Values are high and low Low set the voltage to 800 V and high sets the voltage to 900 V 3 88 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Air H2 Makeup Range Analog Filter Thermo Finnigan Flow mL min Group Box Adjusts the air supply to the detector Typical values are 200 mL min Adjusts the hydrogen gas supply to the detector Typical value is 150 mL min Adjusts the makeup gas to the detector Preferred gas type is Nitrogen and a typical setting is 30 mL min Signal Group Box Changes the electrometer gain Valid selections are 1 10 and 100 With 1 yielding the most sensitivity Electronic filte
8. TRACE Gas Chromatograph Setup User s Manual 2 31 TRACE Menu 2 32 Type Boiling Point Density Mol Weight Type x If you are using an DPFC system pressure programming can be used to help control vapor volume With the Pressure Pulse technique pressure is briefly increased at the time of injection then returned to the setpoint best for column flow rate during the rest of the run Advantages for this technique include Optimizing conditions for sample transfer to the column e Facilitating larger injection volumes e Reducing sensitive components residence time inside the inlet e Solvent parameters group box Solvent parameters group box Select the solvent type you wish to use Choosing a specific type automatically sets preferred values in all the other fields However you still may make adjustments If any of your adjustments exceed the recommended allowance for the liner then Xcalibur displays an error message Values you see listed in Type are for the most common solvents that have densities at 20 C Select Other to calculate expansion volumes for other solvents not listed here Then you may enter the appropriate values for the rest of the Solvent Parameters boiling point molecular weight and density This is shown on the screen for reference although it is not used in the calculations Because the approximation for vapor volume does not really apply near the solvent boiling point calculations are n
9. onto the analytical column Typical entries are 0 2 1 0 minutes with allowable entries from 0 99 99 minutes Surge Group Box This control is enabled when you select wide bore w surge or packed w surge as the injection mode This injection mode allows a higher inlet pressure to be applied during injection This serves to reduce the volume of the vapor cloud created when injected sample is vaporized and may improve separated analytes resolution Allowable entries are 0 250 or 0 700 kPa depending on the carrier flow module you have installed TRACE Gas Chromatograph Setup User s Manual 3 65 Instrument Setup Surge Duration text box 3 66 Injection Evaporation Transfer Cleaning Sub ambient Evaporation Phase Ramped Pressure Cleaning Phase X Enter a time duration for the inlet pressure to be set at the surge pressure setting This entry should be only the time necessary to ensure the injected sample transfers to the analytical column so that the column flow is slightly affected Injection Phase group box Use this control for the injection s ramped pressure Available only with PTV Splitless or PTV Large Volume mode The injector temperature is automatically set to be lower than the solvent s boiling point all you have to do is specify the time the injector temperature must be maintained This group of controls allows you to specify solvent evaporation controls pressure PTV Splitless and PTV Larg
10. other method editor pages see the note below This box is available only after selecting LVOCI left inlet Check this box only if you plan to use a LVCI to run the Large Volume Program Checking this box disables the initial oven temperature controls in instrument stup This is because Large Volume Assistant Program sets the temperature automatically If you want to activate the initial oven temperature control on te Oven page located in instrument setup then uncheck this box TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE GC Ultra Configuration X 1 4 Detectors and Data Page Thermo Finnigan Right Left Use this dialog tab to configure the detectors you will use with your TRACE GC Ultra If you disconnect your detector from your GC remember to reconfigure your TRACE here and from the TRACE GC Ultra front panel Detectors chosen here display instrument setup pages and list in the Detector Events located in the Run Table page TRACE GC 2000 Configuration x General LO Inlets amp Detectors and Data dh Ausiliary and Oven options m Detectors Options Left Right FID Z V Detector Gas Flow Control Aula None Line Frequency 50Hz e 60Hz m Data Channel Definitions Data Source Channel Name Scan Rate Hz Channel 1 Se Channel 1 fio D Channel 2 None DI Channel 2 fio 7 Channel 3 None DI Channel 3 fio 7 Get Annulla ie Figu
11. pressure is programmed as a method development or optimization tool On a Split Splitless SSL Injector the septum purge gas flows out this vent into the atmosphere The purge vent may have a purge valve on it which allows the purge flow to be regulated Use the ramps to increase the oven temperature at a specific rate in C minutes to a final value in C Using multiple ramps allows for finer control of the component separation A graph is generated during GC temperature method development to display the temperature versus time plot that is being created or edited This is the rate of change of the temperature when increasing the temperature from one value to the next This rate is described in degrees Celsius per minute C min The ramp begins at the previous step s final temperature value and proceeds to the current step s final temperature at the specified rate A measure of the ability of a chromatographic column to separate components during a chromatographic experiment Chromatographic resolution between two adjacent peaks is defined as the distance between the centers of the peaks divided by their average peak width measured at 10 of the peak height A resolution of 1 00 indicates baseline separation The total time that a component is in the chromatographic column This is measured from the time of injection until elution If the maximum signal from an analyte is detected 5 minutes and 14 seconds after injection then
12. 1 5 ml min using the dimensions of the test column at 50 C The outlet is set to 1 Atm and the inside diameter to 0 25 mm with the length at 30 meters The inlet pressure slide bar is increased to achieve a flow rate of 1 5 ml min This value is 16 37 psi or about 2 3 psi above atmospheric pressure Column parameters Column outlet pressure Length m 30 0 G 1 Atm C Vacuum C Other D w EI Inside diameter mm 0 250 Hl Temperature C 50 Al IW gt Gas type Outlet pressure psi 14 69 EH Carier gas parameters Inlet pressure gauge psi 1627 Flow ml min ET a Velocity cm sec Holdup time ect Ready ae sam Z e A Astan X C Xcalibur Data Fj Microsoft Office E Data Test Mix BY Microsoft Word f Untitled Inst li Qual Browser 0 VBA 5 19PM Now you can determine the length of the transfer line for the FID Set the column outlet for the splitter to 1 Atm and the inlet pressure to 3 psi The oven temperature remains at 50 C The i d was set to 0 1 mm Reduce the splitter length to a value such that a flow rate of 1 2 of 1 5 ml min is shown or TRACE Gas Chromatograph Setup User s Manual 4 103 How To A 0 747 ml min The length should be 0 2 meters or 20 cm The dimensions for the FID splitter transfer line are 0 1 mm x 20 cm Now calculate the length for the transfer line to the Mass Spec Column parameters p Column outlet pressure Length m 0
13. 112 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To X 4 5 Simultaneous Analysis on the lon Trap and the FID Thermo Finnigan Configuration Close Xcalibur and open the Configuration icon Select the TRACE GC Ultra and then configure The configuration may be uploaded directly from the GC or entered Go to the Detector and Data Tab and select Channel 1 for the Right FID with a scan rate of 10 Hz Select Done and close Configuration Open Xcalibur and proceed to Instrument Set up By specifying a Channel for the detector you invoke acquisition in every run B General O inlets amp Detectors and Data dh Auxiliary r Detectors Let Options Right FID hl I Detector Gas Flow Control Auxiliary None E Line Frequency 50Hz 60Hz m Data Channel Definitions Data Source Channel Name Scan Rate Hz Channel 1 Det A X Channel 1 10 S Channel 2 None x Channel 2 10 Z Channel 3 None sl Channel 3 10 Z When you select NONE for the Detector channel no acquisition of a GC detector will occur Press OK to save the changes Then open Xcalibur Instrument Method Set Up Go to Instrument Set Up from the Home Page and select new method Enter the FID parameters listed below test meth Instrument Setup Eile IRACE Help TRACE Gas Chromatograph Setup User s Manual 4 113 How To By entering a tem
14. 2 3 4 Open the Instrument Setup window Click on the TRACE GC Ultra panel button Select the OCI tab For secondary cooling enter a value equivalent to the sample injection time If you have auxiliary purge controls available and the optional hardware is installed then select column purge to continuously purge the inlet during injection If constant purge is not selected then enter a Stop Purge Time value that is greater than the sample injection time TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan 3 6 HOTOC Page This page is the method editor for the high oven cold on column inlet To display this page Click on the HOTOC page from the Instrument Setup view Oven Left nlet HOTOC Left Carrier Right Inlet SSL Right Carrier Left Det FID m Inlet Duration min 0 00 Figure 3 6 HOTOC Page View Related topics e Setting Up Parameters for an HOTOC HOTOC Page Parameters Inlet Group Box This group box is intentionally left blank for future developments HOTOC Group Box HOTOC Temperature Activates the secondary cooling valve and prevents the GC from going into check box and textbox READY mode until the entered temperature value you enter in this box is achieved Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 51 Instrument Setup XK Duration textbox Enter the amount of time the secondary cooling remains on once the GC advances to
15. 2 Ze 1 tm C Vacuum Other HI Al Outlet pressure psi 14 69 Inside diameter mm 0 100 ail H IR A EEN en m Carrier gas parameters al H gt Gas type Helium zl Inlet pressure gauge psi 3 00 Flow ml min 0 747 A Al Velocity cm sec 155 49 Holdup time sec 0 1 e Leaving the oven temperature at 50 C and the i d at 0 1 mm set the outlet of the splitter to vacuum With 3 psi at the inlet increase the length until a flow of 0 8 ml min is shown The dimensions for the Mass Spec splitter transfer line should be 0 1 mm x 0 6 meters 60cm At these conditions the flow should be split evenly between the Mass Spec and the FID Column Flow Calculator x Column parameters ee p Column outlet pressure Length m 0 6 C 1Atm Vacuum C Other EE 2 Outlet pressure psi 0 00 Inside diameter mm 0 100 K H i mi E Temperature C 50 m Carrier gas parameters laa gt Gas type Helium zl Inlet pressure gauge psi 3 00 Flow ml min 0 802 PE DI Velocity cm sec 229 76 Holdup time ect 0 3 pes Installing the Post Column Splitter Insert the effluent end of the analytical column into the union with a ferrule and insert the two transfer line sections into the other end of the union with the two hole ferrule Note that there is flow of carrier out each transfer line 4 104 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To Thermo Fi
16. Browser Browser For Help press F1 num 06 03 2002 9 19 Figure 3 1 Roadmap Home Page Using the TRACE Tabs After you have configured the TRACE and options you are ready to set the controls to run your method 3 36 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan Related Topics How To Installing the Desolvation Column and Connecting the Tee Characterizing Columns Post Column Splitting of the GCQ with the Flame Ionization Detector Operating an FID with Xcalibur Software Simultaneous Analysis on the Ion Trap and the FID TRACE Gas Chromatograph Setup User s Manual 3 37 Instrument Setup K 3 2 Oven Page This page is the method editor for setting up parameters in the GC run To display this page Click on the Oven page from the Instrument Setup view Oven Left Inlet OCI Left Carrier Right Inlet PTY Right Carrier Left Det FID X Right Det TCD Run Table 50 25 0 TE O S TnL SS O S GL TSU LA I DL IC LSS 000 020 040 060 O80 100 120 140 160 180 200 220 240 260 280 300 m Ramps T Post Run Conditions r Oven Rate Temp Hold Time T Enable C C min C minutes Terese fan KR nable Liyo Initial 40 1 00 D nitial Time min Gem Max Temp C 350 Ramp 1 bon 50 1 00 Prep Run g Pressure Left kPa fi ae min 10 00 i Equilibration Pressure Right kPa 10 Tre mink faso m Ac
17. ON at the first display for the Right Detector The flame will ignite and the signal value displayed will go up You will hear a soft pop A shiny wrench may be held next to one of the exhaust holes at the top of the detector body and a condensation of water will be seen from the flame Setting up the Method In Xcalibur under Instrument Setup enter the values shown below for the method 4 108 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan K How To EA FID_TEST Instrument Setup Bisi E File TRACE Help Distal ai de J Oven Left LVOCI Left Carrier Right SSL Right Carrier Right FID Run Table m Detector M Flame On ee d I Base Temperature C IT en T Analog Filter A i Go Ignition Threshold p 0 2 D amp I Flameout Retry SC el Flow ml min M ar M H2 M Makeup Ready The Mass Spec will not be run but you should set the temperatures to appropriate values for the ion source and the transfer line Also put in a 5 minute filament delay as a precautionary measure The oven program is set to 50 C 1 0 min 20 C min 200 C 1 0 min The split splitless injector is set with a split flow of 60 ml min in the splitless mode with a 1 minute inject time at 230 C Setting up a Sequence in Xcalibur for Acquisition of the FID Only Write a sequence for injection of the test mix When activating the sequence to run open the dialog box
18. Pressure Program graph Pressure text box Gas Saver Flow text box Gas Saver Time text box Ramps arrow buttons Initial Flow text box Initial Hold Time text box Ramp Rate text boxes Thermo Finnigan The graph represents a pressure program for the carrier gas Itis a flat line if a constant pressure program is selected The axes represent time for the x axis and either flow in mls min or pressure in kPa for the y axis Enter the inlet pressure for the analytical run in this text box Vacuum Compensation check box Check this box to compensate for a vacuum at the end of the analytical column This is usually the case where the detector is a mass spectrometer When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure Gas Saver check box and group box This group box contains gas saver controls which reduce carrier gas consumption especially when a large split flow is used The gas saver options are set to come on at some point well after the injection to conserve gas Checking the box will activate the other two features of gas saver The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run The time after the injection when gas saver flow will be activated Programmed Flow Mode Use the Carrier page programmed flow option to set up a programmed
19. TRACE GC 2000 Configuration 4 x J General LO Inlets Detectors and Data P Auxiliary and Oven options r Oven option P UltraFast Module Present m Aux Temperature Zones I Aux 1 Present IT Aux 2 Present Annulla Figure 1 5 Auxiliary Page Aux Temperature Zones Group Box e Check the Aux 1 Present control if you have one of these devices attached Aux1 Valve Oven or MS Transfer Line e Check the Aux 2 Present if you have one of these devices attached Aux 2 Jet Separator and Open Split Aux Pressure Zones Group Box e Check Aux 1 3 Present controls if you will use auxiliary pressure zones during your data acquisition Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 1 15 TRACE GC Ultra Configuration UltraFast Module Auxiliary Interface Valve Oven transfer line jet separator X Oven Option Group Box Check the Ultra Fast Module Present box if the UltraFast Module UFM device is installed inside the GC See also UltraFast Module The UFM is a GC device allows the direct heating of the analytical capillary column properly installed inside the GC oven The UFM device integrates a GC capillary column with the components for its temperature control Compared to conventional air circulating oven this device features faster temperature programming An optional piece of equipment that must be used as the interface between the GC and MS if carrier gas
20. Typical entries are 0 2 1 0 minutes with allowable entries from 0 99 99 minutes Surge Group Box This control is enabled when you select wide bore w surge or packed w surge as the injection mode This injection mode allows a higher inlet pressure to be applied during injection This serves to reduce the volume of the vapor cloud created when injected sample is vaporized and may improve separated analytes resolution Allowable entries are 0 250 or 0 700 kPa depending on the carrier flow module you have installed Enter a time duration for the inlet pressure to be set at the surge pressure setting This entry should be only the time necessary to ensure the injected sample transfers to the analytical column so that the column flow is slightly affected Mode The PPKD inlet operates in both packed mode and wide bore capillary column mode If you select wide bore the carrier flow module operates like conventional capillary modes and uses the column evaluation K factor to calculate flow from pressure applied to the inlet This mode is appropriate for capillary column e length equal or greater than 30 m and operating at column flow rates less than 5 mL min When a column s length is less than 30 m the flow resistance is so small that the packed mode with its closed loop flow control is more accurate If packed mode is selected for the PPKD inlet to operate in then the column flow control is in a closed loop This means that the carrier
21. analyzing high concentration or neat samples or in instances where sensitivity is less important The split vent remains open all the time This method yields the sharpest peaks if the split gas is properly mixed The split vent is closed during the injection to drive most of the sample into the column The solvent effect is required to refocus the analytes especially more volatile compounds You can achieve the solvent effect by keeping the analytical column or guard column slightly below the solvent s boiling point Splitless times of 1 minute are typical Activates controls listed in the Purge group box Injection technique used when it is necessary to eliminate the solvent before the sample enters the column This is mainly for large volume injections when components have a lower volatility than the solvent This item does not list if the Solvent Valve control was selected in for PTV in the Inlet Configuration dialog Displays when the Solvent Valve control is selected or the PTV in the Inlet Configuration dialog Activates Purge controls CT Modes All CT injection modes are constant temperature isothermal modes you operate at set temperatures and time increments Selecting CT modes disables all controls in the Injections Phases group box Constant temperature isothermal split valve Isothermal temperatures operate at a single temperature during the entire analysis Constant temperature isothermal splitless valve The split
22. box and enter a value mL min in the Split Flow text box 5 Enter a value in the Splitless time text box If you want to use constant septum purge click in the Constant Septum Purge check box Otherwise enter the time in minutes in the Stop Purge Time text box 6 Enter values in the Surge Pressure and Surge Duration text boxes 3 48 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 5 OCI Page Thermo Finnigan This is the method editor for the on column inlet To display this page Click on the OCI page from the Instrument Setup view Oven Left Inlet OCI Left Carrier Right Inlet SSL Right Carrier Left Det FID Righi Inlet Sec Cooling Time min 1 00 Figure 3 5 On Column Page View Related topics e Setting Up Parameters for an OCI OCI Page Parameters Sec Cooling Time text box The amount of time the secondary cooling stays on after the start of injection This begins when the TRACE GC Ultra display panel displays READY The value you enter in this text box is the time duration for secondary cooling after selecting Run Start For example if you enter a one in this text box then secondary cooling and the secondary valve turn on when the GC begins READY mode and remains on for one minute after the GC run has started TRACE Gas Chromatograph Setup User s Manual 3 49 Instrument Setup 3 50 Setting Up Parameters for an OCI l
23. change in pressure that the ramp is intended to reach TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Ramp Pressure text boxes Ramp Hold Time text boxes Gas Saver Flow text box Gas Saver Time text box Thermo Finnigan The pressure to be applied during injection and at the beginning of the ramp The time to maintain the value in the ramp pressure field Vacuum Compensation check box Check this box to compensate for a vacuum at the end of the analytical column This is usually the case where the detector is a mass spectrometer When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure Gas Saver check box and group box This group box contains gas saver controls which reduce carrier gas consumption especially when a large split flow is used The gas saver options are set to come on at some point well after the injection to conserve gas Checking the box will activate the other two features of gas saver The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run The time after the injection when gas saver flow will be activated Setting Up Parameters for Constant Flow Mode Use the following procedure to set up parameters for the constant flow option 1 Open the Instrument Setup window 2 Select the Carri
24. flow rates in excess of 4 mL min through the GC column are required for the chromatographic separation This is true when GC columns with inner diameters of 0 53 mm or larger are used There are two Auxiliary Interfaces available for use with the TRACE GC Ultra a jet separator and an open split This is an independent heat zone other than the analytical oven where valves are kept at a temperature to prevent analyte from condensing inside them Valves are often used in GC analysis for introducing sample into the analytical column sampling valve or for enhancing the analytes separation from other compounds in the sample matrix column switching valve Some gas analyses require the use of two or more columns The first column would be used to hold some compounds while allowing others to pass on to a second column for back flushing to vent or for subsequent analysis Valves are mainly used in gas samples analysis although liquid pressurized gas samples may be analyzed using a liquid sampling valve It is critical for the valve or valves to be heated and to be in a purged in a closed environment such as an oven which prevents atmospheric gases from leaking into them This would apply to the gas sample analysis for the components that are in air such as oxygen or nitrogen A heated tube that the GC column effluent passes through to enter the ion source of the MS detector An optional Auxiliary Interface available for use with the GCQ data syste
25. made for a normal GC detector which is usually at atmospheric or slightly higher pressure Gas Saver check box and group box This group box contains gas saver controls which reduce carrier gas consumption especially when a large split flow is used The gas saver options are set to come on at some point well after the injection to conserve gas Checking the box will activate the other two features of gas saver The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run The time after the injection when gas saver flow will be activated Programmed Pressure Mode Click on the Carrier tab of the GC Setup view and then click on Programmed Pressure in the Flow Mode list box Use the Carrier page programmed pressure option to program the pressures to the carrier The parameters are The controls in the Ramps group box depend on the Flow Mode you choose Use the up down control to add or subtract the number of ramps to use in the pressure or flow program For pressure programs this is the rate of change in kPa per minute that the inlet pressure increased or decreased Click the down arrow to add another ramp level Click the up arrow to delete the last ramp displayed The initial pressure for the inlet and column at the start of the analytical run The amount of time the pressure is held at the beginning of the run before the first ramp The rate of
26. method of identification In gas chromatography the components are primarily separated by differences in volatility and structure Some components and samples are not TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Glossary GC MS head pressure hold time initial injection mode injector ion polarity ion source Large Volume Injection Thermo Finnigan suitable for gas chromatographic analysis due to their physical and chemical properties Analysizing organic compounds by gas chromatography with a mass spectometer The mass spectrometer detects analyte concentration found and the analytes identity by comparing the analytes to a library of known spectra The pressure of carrier gas in the injector of the GC The head pressure creates a specific flow of the carrier gas through the GC column See also flow rate and linear velocity The time in minutes to maintain the temperature specified in the Final Value control box Referred to as Holdup time in the Flow Calculator This refers to an unretained component s at column termperature T elution time This is a measure of time that the sample components spend in the mobile phase Hold up time is measured to determie the average linear velocity This is the initial temperature of the GC during injection and at the beginning of the run Type of injection used to introduce a sample mixture onto the GC column Types of injection modes include S
27. program 8 Check the Vacuum Compensation box to compensate for a vacuum at the end of the analytical column When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure 9 Check the Gas Saver box to activate gas saver controls Checking the box will activate the other two features of gas saver Gas Saver Flow mL minute The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run Gas Saver Time minutes The time after the injection when gas saver flow will be activated 3 76 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan 3 12 ECD Page This page is the method editor for the electron capture detector To display this page Click on the ECD page from the Instrument Setup view Oven UFM Left SSL Left Carer Right PTV Right Carrier Left ECD Right FID Run Table m Detector I Base Temperature C 20 I ECD Temperature C 20 Reference Current n 10 Pulse Amplitude MI 50 Pulse Width usec zl 1 0 Flow ml min I Makeup 20 Figure 3 12 ECD Page View Related topics e Setting Up Parameters for ECD ECD Parameters Detector group box Base Temperature This is the ECD detectors base body temperature in degrees Celsius 300 to 350 C ECD Temperature The temperature of the Elec
28. rate mL min Common carrier gases are helium hydrogen and nitrogen Hydrogen offers the best chromatographic properties optimum resolution at the highest flow rates However because hydrogen is flammable helium is often used as a safer alternative for a carrier gas See also chromatography constant flow linear velocity flow rate and resolution A process in which a chemical mixture carried by mobile phase gas or liquid is separated into its individual components as a result of differential distribution of the analytes as they flow around or over a stationary phase liquid or solid See also liquid chromatography_and gas chromatography The flow of mobile phase of carrier gas through the chromatographic column Column flow is usually reported as a linear velocity cm sec or as a flow rate mL min See also linear velocity and flow rate The type of flow control available on gas chromatographs to regulate the flow of carrier gas through the GC column Flow rates are specified in units of mL min In the Constant Flow mode the flow rate of the carrier gas is maintained at a designated setting for the duration of the GC run The head pressure of the carrier gas in the injector is electronically adjusted during the oven temperature program to compensate for changes in the gas viscosity and thereby maintain the desired flow rate The computer hardware and software used to control the instrument and to record analyze an
29. retention time for the first analyte and press OK The peak of 4 118 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To interest will be integrated Continue building your method as instructed in the on line Help tup Quan Ide n Untitled Ext Std Disa ei iskal This detector stream doesn t contain ang soul 6 Select the remaining analytes by retention time and press OK with their appropriate name FT 9 19 9 94 SME 1G Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 4 119 How To XK Report Writing After establishing a report template in Merlin the raw data files may be reprocessed in a batch and reports printed out A calibration curve may be viewed in Quan Browser 4 120 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan analyte carrier gas chromatography column flow constant flow data system Thermo Finnigan Chapter 5 Glossary Any chemical component to be analyzed Internal standards external standards target components quality control samples knowns and unknowns can all be considered analytes The mobile phase in gas chromatography The carrier gas carries the analyte mixture through the GC column where it is separated into its individual components The carrier gas flows through the GC column at a specific rate measured either as a linear velocity cm sec or as a flow
30. stationary phase condensation on the analytical column operate the detector at a higher temperature than the oven program Pay special attention to the analytical column s upper limit Use this to monitor the signal If the signal should drop below the Ignition Threshold it will turn on the ignition coil and attempt to light the FID Flameout Retry repeats up to three times Flameout Retry compares the ignition threshold value to the signal pA The point at which the FID attempts to re ignite The signal in picoamps for the GC to use to compare the current signal to determine if the FID flame is still lit If the signal pA is lower than the threshold the FID flame function indicates igniting When the flame ignites the signal pA increases above the ignition threshold and the ignition process stops If the signal pA does not increase above the ignition threshold value the flame function attempt to ignites the FID three times and then stops The flame function indicates out Flow mL min Group Box Checking any of the following controls enables gas flow from the DGFC to the detector Checking any of these boxes and downloading the method will turn on the particular gas even if the Flame On box is not checked Specify how much airflow 0 600 cc min to activate Acceptable values are On Off When the air is turned on enter the value of the air supplied to the detector to optimize the flame Typical flow is 350 mL min Specify how much Hydr
31. the initial temperature or the previous level s final ramp temperature e Clicking on the Down arrow automatically adds a ramp level after the last one listed e Clicking on the Up arrow deletes the highest level or the one being displayed on the bottom The initial temperature the column is set at the beginning of the temperature program The amount of time to maintain the initial temperature The rate of change of the temperature when increasing the temperature from one value to the next Described in degrees Centigrade per minute C min The ramp begins at the previous step s final temperature value and proceeds to the current step s final temperature at the specified rate The temperature the column is set at for the next ramp of the temperature program The time to maintain the temperature specified in the Final Value control box Oven Group Box Specify how long the GC should remain in the Ready to Inject mode before returning to Stand By If the GC Start button is not pressed within the prep run timeout period then the GC will return to Stand By mode This feature is a protective measure to keep the GC from being in the Ready to Inject mode too long For example this will prevent accumulation of contaminants on the analytical column when doing splitless injections Specify the maximum temperature for this run The UFM has a maximum temperature of 350 C Specify how much time the GC should wait after the initi
32. time of each component of the mixture determines when each component enters the detector On the GCQ the GC can be operated from the either the data system or the GC front panel A serial I O connection COM1 port between the GC and the data system allows the GC parameters to be set up and controlled directly by the data system through the Analysis window and the Instrument Setup window One of the most common instrumental analysis techniques in use When properly used it provides both qualitative what is it and quantitative how much information about individual components in a sample Gas chromatography involves separating the different components in a sample mixture from each other The separation is produced by injecting the sample into a carrier gas stream usually through an injector that passes through a GC column that is packed with a solid packing or coated with a liquid stationary phase The GC column is housed within a temperature programmable oven Varying the oven temperature during a GC run affects the resolution of components as well as their retention time Under reproducible temperature and carrier gas flow conditions the retention time of a component is descriptive of it The components in a mixture can then be identified by comparing their retention times with those of known standard components With a mass spectrometric detector the mass spectra of the components are also descriptive of the components offering another
33. vacuum at the end of the analytical column When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure Check the Gas Saver box to activate gas saver controls Checking the box will activate the other two features of gas saver Gas Saver Flow mL min The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run Gas Saver Time minutes The time after the injection when gas saver flow will be activated Related topics Setting Up Parameters for Programmed Pressure Mode Use the following procedure to set up parameters for the Programmed Pressure option 1 2 3 Open the Instrument Setup window Select the Carrier tab Select Programmed Pressure from the Flow Mode spin box 4 Check the Pressure box to enable flow to the inlet Thermo Finnigan When this box is not checked gas flow goes to the inlet and through any TRACE Gas Chromatograph Setup User s Manual 3 75 Instrument Setup XK installed column If the oven is taken to a high temperature the column may be damaged as well as any detectors or components attached to it 5 Type in values for the initial pressure and hold time for the analytical column 6 Use the Ramp control to add extra ramps to the program 7 Enter rate pressure and hold time values for each additional ramp in the
34. z Scan Fite zi des Plot Type IS zl z Delay min J Benoit Fiy scale ta onnon D Channel 1 will appear as selected type of file Press OK Ranges Automatic Processing Range Time Range minutes 1 T Fixed Scale Type Range Scan Filter Delay min Scale Raw File TIC 0 00 C Xcalbur e Channel 1 0 00 e xcaliburke oO i e D S D x o o S D x P Plot Properties Raw File c xcalbur data test mix with spliter O4069911 raw x Detector EE Seen Fitter z Plot Type Channel 1 7 z Z Delay min 0 00 pen seto POOLS Cancel Hep The TIC and FID chromatogram will be displayed Press the integration button on the tool bar and integrate the peaks in the TIC and FID chromatogram Also set the display labels to area Press the right mouse button with the mouse over the chromatogram for the FID and select Peak Detection settings to allow integration of the peaks The default integration is set for 10 of the highest peak With a FID the solvent is the highest peak so the Peak Identification has to be set to 0 1 TRACE Gas Chromatograph Setup User s Manual 4 115 How To PA Qual Browser 04069911 Raw Data 51 x File Edt View Display Grid Actions Tools Window Help 16 x sjel al IX lefa xl A elem Sal SE le EE gl Caxcalbun 0406931t 04206739 03 14 20 B TIC 04069911 E Channel 1 04069911 X
35. 0 260 280 3 00 gt Ramps T Post Run Conditions r Oven Rate Temp Hold Time 5 C min C minutes ees E T Enable Cryo Initial ao 1 00 il Time min Max Temp C 350 Ramp 1 fio o 50 1 00 Prep Run P Pressure Left kPa fi ied min 10 00 i Equilibration Pressure Right kPa 10 tre mink faso m Acquisition Time min Oven Run Time 3 00 C Specific Time fi 1 00 Figure 3 3 UFM Page View Related topics e Setting Up UFM Ramp Parameters UFM Page Parameters UFM Temperature Program Graph UFM Temperature Graphical representations of the column temperature program The axes are Program graph temperature in degrees Centigrade and time in minutes An isothermal run just gives a flat line Block Temperature Group Box Temperature Enter here the temperature of the auxiliary heating block 3 42 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Ramps arrow buttons Initial Temp text box Initial Hold Time text box Ramp Rate text boxes Ramp Temp text boxes Ramp Hold Time text boxes Prep Run Timeout Max Temp text box Equilibrium Time min text box Thermo Finnigan UFM Temperature Program Parameters Use the up down control to add or subtract the number of ramps to use in the column temperature program This is the rate in degrees Centigrade per minute C min the column is ramped up or down from
36. 0ET SN 94703 Channel 1 BP 0 00 Analog 100 04063911 RT 658 pro RT 928 AA 1599884 AA 1603412 AA 1557855 SN 634 zm Im BP 000 BP 000 BP 0 00 H 1 z 3 4 5 D T 8 H 10 H 2 D H 15 16 w 18 Time min 04069911 567 RT 9 29 AV 1 NL 4 18E5 io T c Full ms 50 00 450 00 100487 g 80 2 S 5 60 3 2 2 40 ZS 3 20 140 0 154 0 p 8 429 0 447 4 0 EST 50 100 150 200 250 300 350 400 450 mz Mass 275 44 Intensity 3 93e 005 Scan Filter none NUM 4 4 116 Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual How To Developing a Processing Method Separate processing methods are created for the Mass Spec and the GCdetector The following order must be followed to open a GC detectorchromatogram 1 Open Processing Set Up and select new method file Under Options verify that the chromatography is by GC Deel al datz FE Chromatox y Option 2 Set the Detector Type to Analog 3 Open a raw data file and enter a name for the first analyte Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 4 117 How To X Press OK Be sure that the Detector Type is still Analog The FID chromatogram will appear 4 Zoom in on the analyte peaks by pinning the cell with the chromatogramand dragging the mouse across the area to be enlarged uan Identification Untitled Ext Std 5 Enter the
37. Change Instruments Remove the Mass Spec from the list by a right mouse click on the word YES by Mass Spec Press OK Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 4 109 How To asm Seele gt m 3 FileName Comment instMeth sitio FID_TESTOIO1 testing FID with Xcalibur C AXcalibur methods FID_TEST FID_TESTO102 testing FID with Xcalibur C Xcalbur methods FID_TEST FID_TEST0103 testing FID with Xcalibur tert Est 7 Ready to Download methods FID_TEST E GCQ Mase Spectrometer Ready to Download TRACE GC 2000 Ready to Download GCO Mass Spectrometer Yes Ae Run Sequence The real time plot will appear on the home page for the FID 4 110 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To calibur D ata FID_TEST108 RAW Real Time Plot Sequence C Xcalibur methods FID_TEST sld Sample Name J Channel 1 Working On Seq Row 8 i alog Position 2 ID_TEST1 Raw File C Xcalibur Data FID_TEST108 RAW g Inst Method C Xcalibur methods FID_TEST Relative Abundance Time min Setting Up Qual Browser for the FID Analog Chromatogram Open the file If this were a dual Mass Spec and FID run you would have to select Channel 1 and set the Detector type to analog Chromatogram Ranges ooooooog Rengels Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 4 111
38. Ionization Detector FID simultaneously or independently Configuring Xcalibur and the TRACE GC Ultra First configure Xcalibur for all hardware that is installed on the TRACE GC Ultra In order to acquire from the FID a Channel will have to be selected for acquisition of the analog signal in the TRACE GC Ultra Configuration under the Detectors and Data Tab TRACE GC 2000 Configuration sl A General 9 inlets amp Detectors and Data d Aulia Detectors Lett None E Options Right FID bs M Detector Gas Flow Control Auriam None jA Line Frequency C 50Hz 60Hz r Data Channel Definitions Data Source Channel Name Scan Rate Hz Charnel 1 Dete D Channel 1 fio Di Channel 2 None D Channel 2 10 Channel 3 None D Channel 3 10 S Verify that the FID is configured on the keypad of the TRACE GC Ultra Unplug the Handshake HS cable from the back of the TRACE GC Ultra that connects to the Mass Spec Review the menu for the Right Detector and be sure that the gases are all configured correctly Standing in front of the GC the right detector position is on your right side Connecting the Gases Connect hydrogen air and a make up of helium or nitrogen to the bulkhead fittings on the back of the GC Set the pressure on the regulators at each tank to about 50 psi The DPFC must be checked by placing a plug in the column end of the detector and installing the brass flow adapter for measuring flows on the d
39. Large Volume Program Load Large Volume File 3 56 X with a specific name and close the LV program Launches the large volume program to automatically make a Large Volume File which calculates the appropriate oven temperature injection speed and pressure setting required for desolvation and analysis 3 Select Load Large Volume File to see a list of available methods Select the appropriate method The instrument parameters for the large volume injection insert into the GC and autosampler methods accordingly Actually downloads the file made during the Run Large Volume Program 4 Enter the desired oven program analytical column flow required other autosampler and mass spectrometer parameters 5 Enter a long filament delay for the first injection for 5 8 minutes The actual fore pressure to the mass spectrometer may be monitored during the filament delay Just look at the GCQ Plus Status page located on the home page for desolvation step optimization and filament delay time Operating Precautions for the LVOCI To conserve air consumption install a step down single stage regulator to use secondary coolant set at 10 psi or 70 kPa Stop all sequence runs not using secondary coolant and do not have a vial located in the tray This is because the GC begins using initial conditions when not using secondary coolant andwill stop the run when it does not detect a vial in the autosampler tray Set the GCQ Plus to the CI mode press th
40. Mase Range no file X Mass Range no file 1 2 Mass Flange no fie X Mass Range no file X Mass Range no file 2K Mass Range no file FID Test mit 2uL RT 0 00 18 50 1005 2 o Tit Relative Abundance RT 1 95 AA 816230506 SN 118120 BP 0 00 RT 6 58 AA 8046246 SN 700 BP 57 06 RT 9 28 AE Pf Peak Detection Settings r Peak Identification Percent of Highest Peak 0 1 Minimum Peak Ht S N 2 0 Peak Integration S N Threshold 05 Valley Detection Enabled Expected Width sec 0 0 KR Peak Ht 7 0 Tailing Factor fo T Apply to All Plots 10 Time min E NL wei 9 09E6 ell TIC MS 04069911 NL 1 3067 Channel 1 Analog 04069911 Astar Microsoft Office Shortcut Bay X 040699 sid Open Seque BY Microsoft Word Simuitane i j Qual Browser 04069 DBA 2254M The spectrum may be viewed as usual by adding another cell and setting it to view spectrum Then select a peak in the TIC and view the spectrum Qual Browser 04069911 Raw Data Jol File Edit View Display Grid Actions Tools Window Help la xl gjela ai PIX alaa eaa mee al Ee EE E E e bm Cie Maneet 04 06 98 03 14 20 FID Test mist Du RT 0 00 18 50 Prag Me E AA 13277898 PrE 7 me ms At DIE AA 3046246 SN 750 Suz BP 5708 08 osossant 5 BP 57 06 E 2 a eo T NL AA 541049331 AS
41. PD Page Note Use in Auxiliary right and left detector positions This page is the method editor for the nitrogen phosphorus detector To display this page Click on the NPD page from the Instrument Setup view VO AE OPAN A AE PLAE AE PE EAA AE AE TL AL AE EA LOL A AA AE E TO AE AE LL PE A AS AE A A A A AE A AA LC AE PC AE AE EAA AE AE E AA AE E AE AE AE E EE AE LET AE AE AE AE AE EAE AE AEA Oven UFM Left SSL Left Carier Right PTV Right Carrier LeftECD Right FID Run Table m Detector Signal I Flame On Range fi x IV Base Temperature C 35 T Analog Filter Ignition Threshold p 0 2 I Flameout Retry m Flow ml min IT Air 350 M H2 35 IT Makeup 30 Figure 3 14 NPD Page View Related topics e Setting Up Parameters for NPD The Nitrogen Phosphorus detector detects Nitrogen and or Phosphorus containing organic compounds The NPD source is a ceramic bead impregnated with alkali metal The source is mounted just above the jet with air makeup and a dilute concentration of hydrogen combined with the column effluent The source is heated to high temperature producing plasma around the bead which decomposes the sample Interaction with the thermionic source is thought to produce the ions attracted and detected by the collector A low hydrogen flow lt 4mls min is used which will not sustain a flame An NPD Nitrogen Phosphorus Detector is an alkali sensitized thermioni
42. PTV 1 In the Options group box select an injection mode and then check or uncheck the available controls listed in this group box Set the available controls listed in the Injection Phases group box Set the available controls listed in the Inlet group box Set the available controls listed in the Purge group box Set the available controls listed in the Surge group box For PTV mode or SSL inlets and all isothermal modes select Vapor Calculator from the TRACE menu bar to automatically calculate the expansion volumes Select Keypad from the TRACE menu bar for quick access to your TRACE GC Ultra keypad functions TRACE Gas Chromatograph Setup User s Manual 3 67 Instrument Setup 3 11 Carrier Page 3 68 This page is the method editor for setting the carrier gas for the TRACE GC Ultra inlet Carrier is gas used as the mobile phase in gas chromatography The carrier gas carries the analyte mixture through the GC column where it is separated into its individual components The carrier gas flows through the GC column at a specific rate measured either as a linear velocity cm sec or as a flow rate mL min Common carrier gases are helium hydrogen and nitrogen Hydrogen offers the best chromatographic properties optimum resolution at the highest flow rates However because hydrogen is flammable helium is often used as an alternative for a carrier gas To display this page Click on the Carrier page from the Instr
43. Port Select the COM port in which your TRACE is connected A COM port is a 9 pin cable connection located on the back of your computer Network Address Enter the I P address to allow the LAN control of the GC through the Thermo data systems ADVANCED Select this button to set the LAN communication port used by the TCP IP ptotocol and timeout Options Group Box Pressure Units Specify the pressure unit measurement to use in your work sessions Pressure measurement units to select include kPa bar and psi 1 10 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan XK TRACE GC Ultra Configuration 1 3 Inlets Page Use this page to select the inlets installed on the top of your TRACE GC Ultra The inlet you select determines which options are available on this page and the instrument setup method editor pages TRACE GC 2000 Configuration x General Io Inlets Q Detectors and Data cp Auxiliary and Oven options Inlets Left EI sel Right SSL e Left Valves J Column Select Valve E SVE Valve DT Solvent Valve Active Inlet Right z IV Link to large volume assistant program Get Annulla Figure 1 3 Inlet Page Inlets Group Box Choose the inlet installed on the left or right side of your TRACE GC Ultra Left Inlets Choose one None SSL OCI HOTOC LVOCI PKD PPKD Right Inlets Choose one None SSL PTV PKD PPKD Left and Right Valves Group Box S
44. R split vent flow column flow Split ratio is usually expressed as a ratio relative to one For example for a split vent flow of 100 ml min and a column flow of 2 ml min SR split vent flow column flow column flow column flow 50 1 On the pressure flow calculator screen the split ratio is always based on the current value for column flow Entering a value for either split vent flow or split ratio and clicking on Calc Flow Ratio calculates the other Column Outlet Flow The Poiseuille equation gives the gas flow carrier rate through an open tubular GC column For a given set of experimental conditions column length and id carrier gas type temperature and outlet pressure this equation can be used to calculate the flow expected with a known inlet pressure or the pressure setting needed to give a desired flow rate F outlet flow in ml min measured at Tref and pref standard conditions 60pr 16h L pi po po po pref Tref T Eq 1 where r column inner radius cm TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu Thermo Finnigan L column length cm pi inlet pressure absolute dynes cm po outlet pressure absolute dynes cm pref reference pressure typically 1 atm T column oven temperature K Tref reference temperature typically 25 C 298 K h carrier gas viscosity at column temperature poise 60 conversion from seconds cgs uni
45. READY SVE Valve Group Box These controls display ONLY if you selected SVE Valve during Inlet configuration SVE Temperature check The solvent vapor exit valve is normally heated to a temperature above the box and textbox boiling point of the solvent being injected in order to prevent solvent condensation in the valve which may cause a flow change during injection Allowable values are 0 200 C or On Off SVE Duration text box This is the time that the SVE valve is open after injection to vent most of the solvent s large volume The LVI program usually calculates this parameter since the exact time to cut off is critical for the LVI injection to properly operate This time determines the volume of residual solvent that is allowed to enter the analytical column Setting Up Parameters for an HOTOC Click here to display the main topic for this procedure_ 1 Cool the area around the column where sample is introduced since the GC column oven generally heats to a temperature higher than the injected solvent boiling point Generally this temperature is set to a value below a solvents boiling point 2 Set the HOTOC Time Duration to the same amount of time as it takes for a sample injection 3 Ifthe SVE Valve is installed heat it to approximately 150 C Turn on the SVE Valve for the necessary time needed to vent the solvent Solvent vent valve turns on when GC READY begins After RUN START the SVE duration time turns off How
46. Specify how much airflow 60 100 uL min to activate When the air is turned on enter the value of the air supplied to the detector to optimize the flame Typical flow is 70 mL min Specify how much hydrogen air flow 2 4 cc min to activate Acceptable values are On Off When the H2 is turned on enter the hydrogen range 0 10 mL min to supply to the detector which optimizes the flame Typical flow is 3 mL min Specify how many minutes to delay the H2 flow within the detector Specify how much makeup gas 10 30 uL min to activate Nitrogen is recommended as the makeup gas to the NPD detector Makeup gas has less thermal capacity and tends to cool the plasma and bead less Makeup gas serves to sweep the column effluent into the detector energy field on plasma Makeup should be nitrogen since Helium tends to cool the source Typical makeup flow is 15 mL min Signal Group Box The range for the detector signal to be acquired Selections are 1 10 100 100 however the lowest setting 0 gives the most sensitivity A higher range TRACE Gas Chromatograph Setup User s Manual 3 83 Instrument Setup XK may be needed for high concentration samples Range represents the amount of current required in nano amps from the detector to offer a full scale output at the selected range Analog Filter Check this box to enable electronic filtering which reduces the response to high frequency baseline noise and signal Setting Up Parameter
47. Thermo ELECTRON CORPORATION TRACE GC Gas Chromatograph Setup User s Manual Published by Technical Publications Thermo Finnigan Italia S p A Strada Rivoltana 20090 Rodano Milan Italy Printing History Revision E printed March 2003 Xcalibur and TRACE GC Ultra are trademarks and or product names of Finnigan Corporation Microsoft is a registered trademark of Microsoft Corporation Technical information contained in this publication is for reference purposes only and is subject to change without notice Every effort has been made to supply complete and accurate information however Thermo Finnigan Corporation assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this manual or the information contained therein even if this information is properly followed and problems still arise This publication is not part of the Agreement of Sale between Thermo Finnigan Corporation and the purchaser of a Thermo Finnigan system In the event of any conflict between the provisions of this document and those contained in Thermo Finnigan Corporation s Terms and Conditions the provisions of the Terms and Conditions shall govern Reference to System Configuration and Specifications supersede all previous information and are subject to change without notice The GC MS and LC MS products of the Thermo Finnigan Division are produced under VISION 2000 accredited quality m
48. able difference between the block temperature and the filament temperature depends on the carrier gas you are using See the TRACE GC Ultra Operators Manual for suggested carrier gas values and the TCD See also TCD Recommended Filament Temperature and Voltages Enter an integer between 5 and 15 in 1 V increments Filament voltages are closely related to filament temperature values Typical values are 5 to 7 V See TCD Recommended Filament Temperature and Voltages TCD Recommended Filament Temperature and Voltages Table 3 1 Detector Temperature 100 C Table 3 2 Voltage v 5 6 7 8 9 10 Table 3 3 Filament Temperature 235 279 315 355 395 435 The detector s block temperature and filament temperatures voltages and carrier gas influence the analysis sensitivity and filament s average life time Limits the filament temperature when the detector operates in the constant voltage mode Enter an integer between 50 to 450 C See Recommended Filament Temperature and Voltages Flow mL min Group Box Makeup indicates the make up gas flow rate Enter an integer between 0 and 100 If the value is less than or equal to 10 mL min the filament power is TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan X Instrument Setup disabled Reference Set the appropriate reference gas flow Enter an integer from 1 to 100 If the value is less than or equal to 10 mL min the filament power is disabled Reference gas is used i
49. al conditions are met before going to standby TRACE Gas Chromatograph Setup User s Manual 3 43 Instrument Setup XK Acquisition Time min Group Box Use Oven Run Time Check this box for the Acquisition Time to be the same as the UFM device radio button Use Other Time button You can define the time for acquisition Enter a value in the text box and text box Setting Up UFM Ramp Parameters Set UFM ramp parameters 1 Open the Instrument Setup window 2 Display the UFM page by clicking on the TRACE panel button 3 Type in the temperature degrees Centigrade and time in minutes for the initial column parameters To add ramps to the column temperature program click on the down arrow of the up down control If you add too many ramps click on the up arrow to delete them Set block temperature parameter 1 Set the temperature of the column auxiliary heating 3 44 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 4 SSL Page Thermo Finnigan Split This page is the method editor for the Split Splitless inlet To display this page Click on the SSL page from the Instrument Setup view Oven Left Inlet OCI Left Carrier Right Inlet SSL Right Carrier Left Det FID Right Det FID Run T M Inlet IT Temperature C 200 V Split Flow ml min 50 Split Ratio 10 Splitless Time min l 1 00 m Purge M Constant Septum Purge Stop Pu
50. alyst may close this valve during the injection splitless time Enter the time in minutes for the septum purge valve to close after beginning the injection The Constant Septum Purge checkbox has to be unchecked for this option to be used This is usually set to the same time as TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Surge Pressure Surge Duration Thermo Finnigan the splitless time The pressure applied during the splitless time to produce a surge of flow in the inlet to speed transfer of the sample It may be used depending upon the analysis to sharpen peaks closer to the solvent s boiling point where cold trapping is ineffective and solvent effect is the main refocusing mechanism Try adding 8 psi or 55 157 kPa to the inlet and observe early peaks after the solvent to see if peak tailing is reduced The amount of time a pressure surge is administered after the injection Typically set to coincide with the splitless time gt GC Setup View Split Mode Setting Up SSL Parameters Setting Up Parameters for Split Mode Use the following procedure to specify the carrier gas flow rate and pressure for constant flow 1 Open the Instrument Setup window 2 Click on the TRACE GC Ultra panel button 3 Select the SSL tab 4 Choose Split from the Mode list box If you would like to set a temperature for the injector click in the temperature check box and enter a tem
51. ambient pressure usually taken as patm for this approximation Solvent boiling points molecular weights and densities can be found in references such as the Handbook of Chemistry and Physics CRC Press and the Merck Index Merck amp Co For more information refer to e Using Vapor Calculator Comparing Vapor Volume to Liner Volume 2 24 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu X 2 2 Using Flow Calculator Length Inside diameter Temperature Inlet pressure Thermo Finnigan Use the Column Flow Calculator to determine column pressure settings and flow rates through a capillary GC column when operating with manual pneumatics Column dimensions temperature inlet and outlet pressure and carrier gas type can be varied when calculating an outlet flow rate average linear velocity and holdup time Column Flow Calculator Page Column Flow Calculator xj r Column parameters Column outlet pressure Length m 30 0 1Atm Vacuum Other i E gt Outlet pressure kPa 101 3 Inside diameter mm 0 320 A F T RS E DI Temperate bt 100 m Carrier gas parameters Al E gt Gas type Helium zl Inlet pressure gauge kPa 101 3 Flow ml min 2 734 a 2 Velocity cm sec 45 58 Holdup time sec 65 8 e Figure 2 2 Column Flow Calculator Page Column parameters group box Each control listed in this box is affected by the choices made in the Carrier
52. ameters eegen eieiei eege cand seevecdoassocdestin derviao ase 42 Setting Up UFM Ramp Parameters eecceecccessceeseeceeeeceeneeceeeeenaessaeceeeeeeees 44 SSE age si8h E T E E T E EE 45 SSL Page Parameters isis cccesisdcislanecceiveicrsl inadcurtiacarniadesdinnecitiaeesliaeeeiions ecutive 45 Setting Up SSL Parameters cccsssscnscsssessosssesssccsssessoseccssnaesssccesscsssensesassesees 47 RENE 49 OGL Page Parameters iiss issaiidecisreochiamiencets pects E EE 49 Setting Up Parameters for an OCT ooo eee eecceeeeneceneeeseeeeeeeeeeeaeeseaeesaecnaeeneeenes 50 HOT EE 51 Setting Up Parameters for an HOTTON 52 LVOCI Page 53 Setting Up Parameters for an LVOCLI 0 ee eeceeceeeeeeceeeeeeeeeeesaecsaeceeeesaeeneeeeaes 54 Operating Precautions for the LVOCI o0 e cece eecceeesseceeeeceeneeceeeesaetenaeeeeeeeeees 56 Tips for Performing Large Volume Injections eee eeseesceeeeceseeeeeeeeeeneeeees 56 IN RRE 58 Setting Up Parameters for PKD ooo eee eee essecsneceeeeseeeeeeeeeeeaeeeaeceaeeeeeeeeeaeeeses 59 PPKD Pate ge Edge iserdnay des sosebauuasubeasensmbunuaeovadensebs 60 Setting Up Parameters for PPKD eee ese csecceecneceeeceseeseeeeeeeesaecsaecnaeenaeeneeeeaes 62 PEV EE 63 Setting Up Parameters for PTV croeer epaien oee e A Ea Nna RTS 67 Carrier Pafe eege tege n Nee E A E iia i a ie 68 Flow Mode list DOR io sscsesscteiectaats cevaced cnsteeds conssasbanaveite ss tate osno nr i a na 69 Setting Up Parameters for Constan
53. ample Optimum temperature for an analytical method varies with he method and sample requirements The entry also has a check box for on off values so that the temperature setting may be turned off without affectingthe setpoint usually used for troubleshooting purposes TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan Setting Up Parameters for PKD 1 Set up parameters for the temperature Typically you set the inlet temperature to approximately 20 C above the temperature necessary to volatilize a sample s components of interest ThePKD operates in a closed loop flow control manner This means that the carrier gas flow module measures the flow of gas to the inlet for direct flowcontrol Typical gas flow rates for 1 8 PKDs are 15 30 cc min Note Operating this inlet with micro packed or wide bore capillary columns make it necessary to optimize the carrier gas flow to match the installed column TRACE Gas Chromatograph Setup User s Manual 3 59 3 9 PPKD Page This is method editor for the purge packed column inlet To display this page Click on the PPKD page from the Instrument Setup view Oven UFM Left PKD Left Carrier Right PPKD Right Carrier Right FID Run Table m Inlet IV Temperature TC 35 m Purge IV Constant Septum Purge Stop Purge Time min 0 00 m Surge Surge Pressure kPa 3 Surge Duration min 0 00 Mode
54. anagement systems U S A Thermo Finnigan Corporation 355 River Oaks Parkway San Jose CA 95134 1991 1 408 965 6000 Thermo Finnigan Technical Support 3661 Interstate Park Road North Riviera Beach FL 33404 800 685 9535 561 844 5241 Fax 561 881 8431 Australia Thermo Finnigan P O Box 239 Rydalmere Unit 20 Metro Centre 38 46 South Street Rydalmere N S W 2116 61 02 9898 9000 Austria Thermo Finnigan GmbH Wehlistrasse 27b A 1200 Wein 43 01 333 50 34 0 info quest thermo at Belgium Thermo Finnigan BVBA Groenenbrogerlaan 84 B 2610 Wilrijk Antwerpen 32 03 825 0670 Canada Thermo Finnigan Canada 5716 Coopers Avenue Unit 1 Mississauga Ontario L4Z2E8 1 905 712 2258 France Thermo Finnigan France SA Parc Hightec Sud 12 Avenue des Tropiques Z A de Courtaboeuf BP141 F 91944 Les Ulis C dex 33 01 69 18 88 10 Germany Thermo Finnigan Analytische Systeme GmbH Boschring 12 D 63329 Egelsbach 49 06103 408 0 Italy Thermo Finnigan Italia S p A Strada Rivoltana I 20090 Rodano Milano 39 02 95059 1 Japan Thermo Finnigan K K Nishi Shinjuku Toyokuni Bldg 3F 2 5 8 Hatsudai Shibuya ku Tokyo 151 0061 81 03 3372 3001 Japan Thermo Finnigan K K Esaka Grand Building 2 3 1 Esaka cho Suita City Osaka 564 0063 81 06 6387 6681 Netherlands Thermo Finnigan BV Druivenstraat 33 NL
55. and Carrier Gases The DPFC module for the carrier gas should give a K value of about 1 879 with the outlet splitter installed to the FID and the Mass Spec when the standard test column is installed Rtx 5 0 25 mm x 30 meter 0 25 micron film Close the split and septum purge vent valves on the keypad of the GC and test by pressing the column evaluation button and selecting the right inlet If the value is lower then you have a leak If the value is higher like 14 or 22 you have a defective DPFC module The FID has a gas flow test for validation of the gas module calibration The FID module is a type AC This module provides control for the hydrogen air and make up flows A special adapter is enclosed to attach to the top of the FID for measuring the flows for this test Turn the heater off to the FID and allow it to cool Remove the chimney to the detector and install the adapter Using an electronic flow meter verify the following flows TRACE Gas Chromatograph Setup User s Manual 4 105 How To XK Test Low Flow Test High Flow Test Hydrogen 20 2 100 5 Air 60 6 300 15 Make up 10 1 5 50 3 If the flows are not within the specifications order a new module 4 106 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To X 4 4 Operating an FID with Xcalibur Software Thermo Finnigan Introduction Xcalibur software allows the user to acquire from the Mass Spec and the Flame
56. apture detector To display this page Click on the FID page from the Instrument Setup view POPC AE AE LO LLC AE AA AL AA AE AE EA AE AE OE AA AE AE E AL AE AE EE EA AE ETL AE E LL AE A LT LL LOL A A LOL ECL A AE LCL LOL LOL LL TIL AE AE AE AE AE EE AA AE ETC AEEA Oven UFM Left SSL Left Carrier Right PTV Right Carier LeftECD Right FID Run Table Detector Signal IT Flame On Range fi x V Base Temperature C 35 I Analog Filter Ignition Threshold p 0 2 I Flameout Retry m Flow ml min IT Air l 350 IT H 35 T Makeup 30 Figure 3 13 FID Page View Related topics e Setting Up Parameters for FID FID Parameters Detector Group Box Checking this box turns on the detector gases if not previously on and turns on the ignition coil to light the flame Unchecking this box shuts off the detector gases extinguishing the flame Performs several functions turns on detector gases increases hydrogen flow above the setpoint to 40 mL min decreases air below the setpoint to approximately 200 mL min turns the makeup gas off supplies current to the ignition coil TRACE Gas Chromatograph Setup User s Manual 3 79 Instrument Setup 3 80 Base Temperature Flameout Retry Ignition Threshold Air H2 Makeup Range nA Analog Filter X This is the temperature in degrees Celsius of the detector base body Enter values 250 to 350 To prevent
57. ature Enter an integer between 30 and 450 C Typical temperature is 200 C depending on the application you are using A general rule to apply is to set the temperature to a higher value than the maximum temperature reached by the GC column oven during the analysis See Recommended Filament Temperature and Voltages Enter an integer between 20 and 400 C This temperature heats the transfer line between the GC oven and the TCD cell We recommend setting a value 3 85 TRACE Gas Chromatograph Setup User s Manual Instrument Setup Filament Power Constant Filament Temperature Filament Temperature Fil 3 86 Filament Voltage Max Temperature Makeup X higher than or equal to the set oven temperature Check this box to turn on power to the TCD filaments Check this box to activate the Filament Temperature control only and disables Filament Voltage and Fil Max Temperature controls This operating mode keeps a constant filament temperature based on the relationship between the block temperature and the filament temperature and carrier gas When using low thermal conductivity gases the filament temperature is high for low voltage supply See Recommended Filament Temperature and Voltages Enter an integer between 50 and 450 Adjust in 10 increments Filament temperatures should be kept at least 20 C higher than the block temperature The greater the difference the better the sensitivity However the use
58. ature parameters for your TRACE GC Ultra Flows page These values show the actual and setpoint Flow parameters for your TRACE GC Ultra Pressure page These values show the actual and setpoint Pressure parameters for your TRACE GC Ultra Keypad Located in your Instrument Setup TRACE menu Your Xcalibur virtual TRACE GC Ultra Keypad operates just like if you were using it from the TRACE GC Ultra front panel The only difference is where you are pressing the keys from the instrument panel or your Xcalibur software You might find it helpful to learn the TRACE Keypad according to the following groups TRACE Gas Chromatograph Setup User s Manual 1 19 TRACE GC Ultra Configuration Action Keys Zone and Device Information Keys Instrument Setup Keys Shortcut Keys Data Entry Keys Information Keys Method Storage and Automation Keys 1 20 X Stop Prep Run and Start Oven Left Inlet Right Inlet Left Detect Right Detect Aux Left Carrier Right Carrier Left Signal Right Signal Leak Check Column Eval Config Temp Press Flow Time Ramp On Yes No Off Mode Type Clear Enter st 0 9 Status Info Diag Run Log Load Store Method Seq Edit Active Run Table Clock Table Auto Sampler Valves Seq Control Look for specific instructions for operating each key in the TRACE GC Ultra Operating Manual Chapter 2 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Th
59. autosampler and GC Mass spectrometer parameters download with the GC Configuring for LVI 1 Configure the autosampler TRACE or TOP GC and MS for LVOCI 2 Open the autosampler method editor and create a new method for the LVI method 3 Configure your autosampler to use the Large Volume Program Select Left for the Autosampler Placement and Large Volume and enter the maximum volume for the syringe that is installed Select OK The system configures for EPC gas control for the left LVI injector TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan Calculating Optimum Parameters When using the TRACE GC Ultra 1 Select the left carrier and set the flow mode to constant flow or programmed pressure with vacuum compensation Next select LVOCI and select Temperature On Enter 200 C for the SVE valve temperature to prevent residue accumulating from the solvent during desolvation Enter the required ramped pressure setting for downloading the two pressures that the LVI software calculates for the two step process of desolvation and then analyte analysis The first pressure is high for solvent evaporation andthe second pressure setting is lower for analytes enhanced resolution throughthe capillary column Note Do not enter the oven ramps for the analysis at this time they are entered after loading the parameters for the LVI You may also setup parameters for isobaric operation
60. c detector used for the specific detection of phosphorus and organic nitrogen The NPD is very sensitive and is instrumental in pesticide and herbicide residue analysis in various EPA methods This detector is also useful for the clinical analysis of caffeine nicotine and other nitrogen containing drugs 3 82 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Source Current Base Temperature Polarization Voltage v Air NPD H2 H2 Delay Makeup Range nA Thermo Finnigan NPD Parameters Detector Group Box Specify the current amperes necessary to generate a background current This is the temperature in degrees Celsius of the detector s base body Maximum range is 450 C Typically detectors that use the detector base temperature as the sole source of heat are set to 300 C Of course the detector base temperature should always be at least 10 C higher than the maximum column oven operating temperature Detectors that have a secondary heat source require a base temperature of typically 250 C Select a polarization voltage 1 0 9 9 to apply to the collector Polarizing voltage is a DC voltage that is superimposed on to the NP source assembly Adjust the polarizing voltage from 1 0 to 9 9 in 1 V increments Flow mL min Group Box Checking any of these boxes activates the gas flow from the DGFC module to the detector and downloads the method to turn on the particular gas
61. calculating inlet pressure from velocity at greater than zero outlet pressure is done using an approximation technique For more information refer to e Using Flow Calculator Vapor Calculator Calculates the vapor volume for the PTV and SSL inlets from the injection volume in proportion to the installed liner column Assuming if the vapor behaves like an ideal gas and only solvent vapor needs to be considered for dilute samples vapor volume V for n solvent moles at temperature T and pressure p is then approximated by the ideal gas law V nRT p Absolute temperature and pressure are used for the calculations and n is TRACE Gas Chromatograph Setup User s Manual 2 23 TRACE Menu XK determined from the solvent volume density and molecular weight Since 1 mole of an ideal gas occupies 22 4 liters at 0 C and 1 atmosphere pressure vapor volume in microliters can be calculated from the following equation V 22 4x r MW T 273 273 patm pi pa Vinj where V vapor volume microliters at inlet temperature and pressure Vinj solvent liquid volume microliters injected r solvent liquid density g ml MW2 solvent molecular weight g mole 22 4 liters occupied by 1 mole of ideal gas at O C and 1 atm pressure T inlet temperature C absolute temperature K C 273 pi inlet pressure gauge absolute pressure pi pa patm 1 atm pressure 14 7 psi 101 kPa or 1 01 bar pa
62. d interpret the data collected by the instrument TRACE Gas Chromatograph Setup User s Manua 5 121 Glossary electronic pressure control final value flow rate flow control gas chromatograph gas chromatography 5 122 X A system on the Finnigan GC CE 8000 TOP GC and the HP 5890 that controls the head pressure on a GC column at the injector The pressure can be maintained or modulated during an analysis to affect the separation efficiency and speed of an analysis For the first step this box sets the initial temperature for the program For all other steps this final value is the value the ramp is intended to reach Temperatures can range from 80 C to the maximum oven temperature value The rate of flow of the carrier gas through the GC column The unit of measurement for flow rate is mL min Gas chromatography is defined by the separation of analytes by partitioning between a mobile phase the carrier gas and a stationary phase This mobile phase flow rate must be regulated to provide reproducible results See also flow control Method for controlling the flow of carrier gas through the GC column Several methods are available depending on the type of GC An instrument that separates a sample mixture into its chemical components by gas chromatography A GC typically consists of an inlet for introduction of the sample a column for separation of the analytes and a detection system The characteristic retention
63. d pressure is applied to the column and remains unchanged throughout the analysis Programmed Flow controls in the left group box display Ramps Rate Flow and Hold Time Enter program to control column flow for analytical run Programmed Pressure controls in the left group box display Ramps Rate Pressure and Hold Time Enter inlet pressure program for analytical run In both the programmed flow and programmed pressure modes the flow or pressure changes according to a timetable similar to temperature programming The analyst may specify an initial pressure initial time up to three program ramps with rates targets and hold times for each needed ramp The programmed modes are typically used to shorten analysis times by increasing column flow to drive higher boiling components off the column faser at the end of analysis Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 69 Instrument Setup Flow Program graph Flow text box Gas Saver Flow text box Gas Saver Time text box 3 70 X Constant Flow Mode Click on the Carrier tab of the GC Setup view and then click on Constant Flow in the Flow Mode list box Use the Carrier page constant flow option to select a constant flow without ramping The parameter available are A graphical representation of a flow program for the carrier gas Itis a flat line if a constant flow program is selected The axes represent time for the x axis and flow in
64. e 0 00 Remaining time 0 00 Emergency conditions I Emergency shutdowr T Over temperature I Shorted RTD T Shorted oven RTD Keypad Figure 1 6 Status Tabs e Status e Temperatures e Flows e Pressures Status General Group Box Status Indicates if instrument is communicating to Xcalibur 1 18 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE GC Ultra Configuration X Elapsed time Remaining time Emergency shutdown Over temperature Shorted RTD Shorted oven RTD Thermo Finnigan Run Group Box The amount of time that has elapsed since the run started The amount of time that remains before the run finishes Emergency Conditions Group Box Your Xcalibur software automatically checks this box if an error condition like a leaking hydrogen sensor or something is malfunctioning internally in your TRACE GC Ultra The software automatically shuts the TRACE GC Ultra off Check your TRACE GC Ultra Maintenance and Troubleshooting Manual for possible solutions This box is checked only when Xcalibur software detects the temperature is over the recommended level This detected problem requires certified technical support Contact your local TMQ Tech Support office for service This detected problem requires certified technical support Contact your local TMQ Tech Support office for service Temperatures page These values show the actual and setpoint Temper
65. e GCQ Plus EI CI button locatedon the GCQ front panel to operate in high pressure mode Tips for Performing Large Volume Injections Read the LVI Manual e Select the smallest retained volume when optimizing your large volume injection method You can choose larger retained volumes if the smallest amount is not adequate e During the filament delay process the GCQ extends the filament delay until adequate vacuum has been detected the blue blinking light on the front panel of the GCQ MS will turn off and the green light will be on This is completely normal You can increase your filament delay time in the MS method to match the actual time it takes for the vacuum system to recover from the large volume injection e Get the best pressure value results by using the LVI Assistant program to select the Injected Volume option Then use the LVI calculated pressure values to download to the instruments TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan Before loading an LVI method from the AS method editor make sure the GC is configured for pressure program mode This will download the pressure values from the LVI optimization program and ensure that the correct times and flows are present to evaporate the solvent from the pre column Using the constant flow or constant pressure modes results in too much flow into the mass spectrometer during the run analysis Using programmed flow wi
66. e TCD detector sensitivity This is useful for known sample matrices which exhibit wide and varying analyte concentrations Select this option to invert the TCD detector response This is useful for quantifying a negative going peak such as Hydrogen when a carrier such as Helium is used as carrier and reference gas Select this option to allow for source current changes for the NPD detector during runtime PID specific Turns the UV lamp power on which strikes the lamp and thus creates a lamp current This event is useful to enable the PID lamp only during specific analysis times such as after solvent elution PID specific Selects the PID lamp current Valid selections are low and high The higher the lamp current the more intense the transmitted lamp transmission which enhances sensitivity but reduces lamp life Valve Event Group Box If you have either a valve oven or sample valves then click the valve event button to activate valve events Select from 1 to 8 for each external event to turn on from the Run Table page If you use all 8 then none are available for other events Select one Switching sampling or Multiposition Switching is On or Off Sampling is a valve used to inject a sample volume into the carrier stream Multiposition allows you to use 1 to however many positions your valve has Select Load or Inject for the sample valve settings Whichever valve type you select determines the available setting selecti
67. e Volume only rate temperature and time in minutes Set the solvent evaporation temperature set the rate to reach the solvent evaporation temperature This group of controls allows you to specify controls for the sample transfer into the column Pressure PTV Splitless and PTV Large Volume only rate temperature and time in minutes Specify the pressure if available Set the rate in C s to reach the sample transfer temperature Set the temperature for sample transfer into the column Set the time in minutes for the transfer temperature to be maintained Set the rate necessary to reach the cleaning temperature Set the injector cleaning temperature Set the time in minutes the cleaning temperature must be maintained Options Group Box Start here Selections made in this group box determine which controls to activate in other group boxes Select this option to enter sub ambient temperatures 50 C to 400 C in the Temperature text box Check this box to activate the Evap controls listed in the Injection Phases group box If you selected the PTV Splitless or PTV Large Volume mode then this control is available for you to activate pressure controls for solvent injection evaporation and transfer Check this box to activate the Cleaning controls listed in the Injection Phases group box TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan Setting Up Parameters for
68. e programming of the injector The injector is a universal injector for capillary gas chromatography The injector may be operated in the cool on column mode large volume mode isothermal split or splitless mode or temperature programmed mode See also on column injection Large Volume Injection split injection and splitless injection This is the GC run time It is calculated by summing the ramp times and hold times in the temperature program The total elapsed time for a run cannot exceed 650 minutes At 650 minutes the run terminates and the oven temperature returns to the initial oven temperature In an isothermal operation no ramp steps or RATE 0 the instrument internally sets the run time to a maximum of 650 minutes The Ultra Fast Module UFM is a GC device allows the direct heating of the analytical capillary column properly installed inside the GC oven The UFM device integrates a GC capillary column with the components for its temperature control Compared to conventional air circulating oven this device features faster temperature programming TRACE Gas Chromatograph Setup User s Manual 5 127
69. ed in a flash vaporization off column mode See also negative ion and ion polarity The On Column Injector OCD allows to inject a sample directly into a 0 25 or 0 32 mm capillary column or 0 53 mm wide bore column Primary and secondary cooling system keep the injection block at ambient temperature and the injection zone cool to prevent sample vaporizazion and ensure complete sample transfer from the syringe to the column A special versions of this injector allows e to introduce large volumes of liquid sample LVOCI e to operate at high oven temperature by using an option HOT device HOTOC See also Large Volume Injection An atom radical molecule or molecular moiety that has lost one or more electrons or has been protonated thus acquiring a positive charge The charge state becomes 1 2 3 etc depending upon the number of TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Glossary X pressure program purge vent ramp rate resolution retention time secondary cooling split injection Thermo Finnigan electrons lost or protons gained See also negative ion and ion polarity Type of flow control used to regulate the flow of carrier gas through the GC column head pressureat the injector is specified in units of psi and the ramps are in units of psi min This produces a certain flow rate of the carrier gas through the GC column The head pressure is controlled by an EPC The
70. elect the following to further control your selected inlet SVE Valve Check this box to display Sub Ambient controls in the selected inlet s instrument setup pages This allows you to enter cryogenic programmable entries below zero if you have installed cryogenic hardware optional purchase Additionally SVE Valve allows volatile vapor to bypass the Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 1 11 TRACE GC Ultra Configuration Solvent Valve Column Select Valve X analytical column Typically used with a large volume injector If you have the cryogenic hardware installed be sure that configurations have been set manually into the TRACE GC Ultra using the TRACE GC Ultra keypad Check this box to use a split valve that is attached to the GC top This selection prevents condensation from reaching the split valve in a large volume injection when using a PTV Check this box when using a column select valve with a single DPFC and two inlets The carrier gas diverts to the selected inlet that you activate Active Inlet When you select Column Select Valve specify which inlet you want to exclusively use When you activate an exclusive side the other inlet side defaults to no settings Carrier gas diverts to the specified inlet Link to large volume assistant program Checking this box allows you to use the Run Large Volume Program found on the autosampler menu However it does disable other functions found on
71. equires 1 ms pulse Use of Argon Methane requires a 0 1 ms pulse to produce the highest linear range The value selected depends on the type of detector gas being used with the ECD Nitrogen requires a pulse width value of 0 5 or 1 0 Usually 1 0 is the desired value Flow mL min Group Box Specify how much make up gas 0 90 cc min to activate Nitrogen or Argon Methane is suggested as the make up gas to the ECD detector Checking this box enables the use of make up gas into the detector To reduce line out time use higher flow rates around 60 mL min when the detector is first turned on Reduce the makeup to 30 mL min for optimumresults Setting Up Parameters for ECD 1 Set the detector base temperature to 250 C 2 Set the ECD temperature to 300 C 3 Set the Reference Current to 1 nA 4 Set the Pulse Width to 1 u sec 5 Set nitrogen makeup gas at 30 40 mL min Allow several hours for the system to line out The detector frequency should stabilize below 5 kHz TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 13 FID Page Flame On Thermo Finnigan Note For auxiliary right and left usage only This page is the method editor for the flame ionization detector If you are using a stacked detector and using an ECD then the makeup gas is usually plumbed separately for the ECD and is specified as the Electron Capture medium This page is the method editor for the electron c
72. er select the file The TIC will appear Press the right mouse button and select ranges D Ble Edt View Display Gid Actions Toos Window Help ale x sjela al Jil seis ella ase seal eee Al lt 2 2 j Giel FID Test mic 2ul Stil RT 0 00 18 50 E TiC 04063911 100 ae DZ K Mass Range no file o Tic MS XK Mase Range no file 4069911 X Mass Range no file 90 X Mass Range no file X Mase Range no fie s5 X Mass Range no file 80 X Mass Range no file Relative Abundance 25 20 1 10 9 73 S 14 38 4457 1396 1412 en 18 27 OS maa a _ __ _ SEET o 2 4 6 8 10 12 14 16 18 LS Time min Show dialog for changing data ranges in displays NUM 4 AStan H Microsol Ofice Shortcut Ba X 040699 sid Open Seque HY Microsoft Word Simultane L Qual Browser 04069 Bae 9214M 4 114 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To Thermo Finnigan A dialog box will appear select another TIC and then change the detector from Mass Spec to Analog Chromatogram Ranges x Ranges Automatic Processing Range l Time Range minutes T I Fixed Scale Type Range Scan Filter Delay min Scale Raw File TIC 0 00 C Xcalibur tic 0 00 e xcalibur c D z D o o D P D D Plot Properties Raw File Je xcaliburkdatastest mix with splitters406991 6 raw x Detector s
73. er tab 3 Check the On box in the Flow group box to turn on the flow 4 Type ina value for the flow for the analytical column 5 Check the Vacuum Compensation box to compensate for a vacuum at the end of the analytical column When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure 6 Check the Gas Saver box to activate gas saver controls Checking the box will activate the other two features of gas saver Gas Saver Flow mL min The desired flow after the injection or in TRACE Gas Chromatograph Setup User s Manual 3 73 Instrument Setup 3 74 X standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run Gas Saver Time minutes The time after the injection when gas saver flow will be activated Setting Up Parameters for Constant Pressure Mode Use the following procedure to set up parameters for constant pressure l 2 Open the Instrument Setup window Select the Carrier tab Check the pressure box to enable flow to the inlet When this box is not checked gas flow goes to the inlet and through any installed column If the oven is taken to a high temperature the column may be damaged as well as any detectors or components attached to it Enter a value for the pressure for the analytical column Check the Vacuum Compensation box to compensate for a vacuum at the end of the anal
74. ermo Finnigan Chapter 2 TRACE Menu This chapter describes the Instrument Setup menu This chapter contains these topics Menu Description 22 Using Flow Calculator 25 Using Vapor Calculator 31 TRACE Gas Chromatograph Setup User s Manua 2 21 TRACE Menu 2 1 Menu Description Action Keys Zone and Device Information Keys Instrument Setup Keys 2 22 Shortcut Keys Data Entry Keys The TRACE menu is located on the Instrument Setup menu bar TRACE Send Method to GC Get Method from GC Keypad Flow Calculator Vapor Calculator Figure 2 1 Menu The pull down mwnu contains the following options Send Method to GC command Downloads the GC portion of the current method from the Instrument Setup window to the gas chromatograph Get Method from GC command Uploads the current method from the gas chromatograph to the Instrument Setup Window Keypad Located in your Instrument Setup TRACE menu Your Xcalibur virtual TRACE GC Ultra Keypad operates just like if you were using it from the TRACE GC Ultra front panel The only difference is where you are pressing the keys from the instrument panel or your Xcalibur software You might find it helpful to learn the TRACE Keypad according to the following groups Stop Prep Run and Start Oven Left Inlet Right Inlet Left Detect Right Detect Aux Left Carrier Right Carrier Left Signal Right Signal Leak Check Column Eval Config Temp Press
75. etector base of the FID You must remove the outside chimney to the detector first by unscrewing the thumbscrew and lifting the entire detector TRACE Gas Chromatograph Setup User s Manual 4 107 How To K body off Verify the following flows and tolerances e H2 20 ml min 2 60 ml min 5 e Air 60 ml min 6 300 15 e Makeup 10 1 5 50 3 If the flows do not match the tolerances then change the DPFC module Remove the flow adapter and reinstall the detector body Installing the Test Column The test column is installed into the split splitless injector The column is inserted beyond the FID jet and then pulled back 2 3 mm This prevents burning the end of the column in the flame If the column is burned at the tip the response will be low and only a small peak for the solvent will be seen Column Characterization Once the column has been connected set the base temperature to 250 C and perform the column characterization The Right carrier is set to constant pressure at 30 kpa with vacuum compensation off Check to see that the split splitless septum purge and split vents are off by pressing VALVE on the keypad and ENTER Next perform the column characterization A K value of 0 148 is typical for the Rtx 5 0 32mm x 7 meter 0 25 micron film GC test column Igniting the Flame Once the column has been characterized the detector gases may be turned on at the key pad of the GC and the flame ignited Press
76. ever this duration time stays on until the required amount of solvent is vented It is necessary that the GC run be started at the beginning of sample injection 3 52 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 7 LVOCI Page Sec Cooling Time text box Thermo Finnigan This is the method editor for the large volume on column inlet To display this page Click on the LVOCI page from the Instrument Setup view iven Left Inlet LVOCI Left Carer Right Inlet SSL Right Carrer Left Det FID Right Det FID Run Inlet Sec Cooling Time min 1 00 m LYI Evaporation Start LYI Assistant Pressure kPa 10 Duration min 0 00 m SVE Valve ro SVE Duration min Figure 3 7 LVOCI Page View Related topics e Setting Up Parameters for an LVOCI e Operating Precautions for the LVOCI es Tips for Performing Large Volume Injections LVOCI Page Parameters Inlet Group Box This is the time after injection that the secondary cooling air or other cooling fluid for example N2 or CO2s on Allow the cooling to be on long enough to allow the liquid injection to move away from the syringe needle tip before the syringe is withdrawn After the syringe is withdrawn this cooling is no longer necessary 3 53 TRACE Gas Chromatograph Setup User s Manual Instrument Setup Pressure text box Duration text box Temperature c
77. ff values so that the temperature setting may be turned off without affecting the setpoint usually used for troubleshooting purposes Specify the total split flow coming out of the inlet This is the total flow out of the inlet when the split valve is open The ratio of split vent flow to the column flow Calculate the split ratio as shown Split Ratio column flow split vent flow column flow You must select the PTV Split or CT Split mode to use the Split Ratio control Then select the Carrier page and select Constant or Programmable Pressure mode to activate the Split Ratio control The amount of time after the injection at which the split vent opens This control activates only after selecting SVE Valve from the Inlet Configuration dialog see nlets Page Check this box to enter a temperature value for a PTV large volume injection instead of the PTV solvent With this control you can regulate the temperature for the PTV large volume heating valve Purge Group Box This entry allows the septum purge flow to be turned off for a specified amount of time after injection Allowable entries is On or Off If you select On using a needle to penetrate to a normal injection depth then you will see little sample loss If the constant septum purge box is unchecked specify the time after injection that the septum purge flow is turned off Keep the flow off for the minimum time amounts so those septum bleed products are not transferred
78. flow for the GC The available parameters are Use the Carrier page programmed flow option to set up a programmed flow for the GC The available parameters are The controls in the Ramps group box depend on the Flow Mode you choose Use the up down control to add or subtract the number of ramps to use in the pressure or flow program This is the rate of change in mL min that the column flow is increased or decreased Click the down arrow to add another ramp level Click the up arrow to delete the last ramp displayed The initial flow for the inlet and column at the start of the analytical run The amount of time the flow is held at the beginning of the run before the first ramp The rate of change in mL minute that the columns flow is increased or decreased TRACE Gas Chromatograph Setup User s Manual 3 71 Instrument Setup Ramp Flow text boxes Ramp Hold Time text boxes Gas Saver Flow text box Gas Saver Time text box Ramps arrow buttons Initial Pressure text box Initial Hold Time text box Ramp Rate text boxes 3 72 X The amount of flow to be used for each ramp The amount of time the flow is held at the end of the ramp Setting Up Parameters for Programmed Flow Mode Vacuum Compensation check box Check this box to compensate for a vacuum at the end of the analytical column This is usually the case where the detector is a mass spectrometer When the box is not checked calculations are
79. ght PTY Right Carrier Left ECD Right FID Run Table Mode PTV Split Thermo Finnigan m Inlet r Injection Phases C P Rat Ti Fl M Temperature C 35 RS tee oa min ei I Split Flow ml min 10 Injection 70 0 05 Split Ratio In Evap 140 d 145 200 1 00 Transfer EE 45 200 1 00 Spitless Time min ee Cleaning re T 20 1 00 50 E Soy Valve Temp te 100 Show Graph Purge M Constant Septum Purge pate I Sub ambient IT Backflush Enabled Stop Purge Time min 0 00 T Evaporation Phase I Cleaning Phase eg E Ramped Pressure Surge Pressure kPa 3 PTV Split X Surge Duration min 0 00 Figure 3 10 PTV Page View Related topics e Setting Up Parameters for PTV PTV Page Parameters Mode list box Select a PTV mode from the Mode list box PTV Modes All PTV injection modes are programmable ramped temperatures you operate at varying temperatures with specified times and temperature increments Selecting PTV modes activates various controls listed the Injections Phases group box The carrier flow is split in the injection port with the bulk going out the split 3 63 TRACE Gas Chromatograph Setup User s Manual Instrument Setup PTV Splitless PTV Solvent Split PTV Large Volume CT Split CT Splitless CT Splitless w Surge Temperature checkbox 3 64 and text box X vent Use this injection mode when
80. heck box and text box SVE Duration text box 3 54 x LVI Evaporation Group Box This is the inlet pressure used during the evaporation stage of the large volume injection This parameter is usually generated by the LVI software program and not entered by the user This can be the same as inlet pressure if a single pressure program is being used and this entry will be grayed out Allowable values are 0 250 or 0 700 kPa depending on the carrier flow module Enter a duration time for the injection s LVI evaporation stage This parameter is usually calculated by the LVI software and transferred into this page SVE Valve Group Box The solvent vapor exit valve is normally heated to a temperature above the boiling point of the solvent being injected in order to prevent solvent condensation in the valve which may cause a flow change during injection Allowable values are 0 200 C or On Off This is the time that the SVE valve is open after injection to vent most of the solvent s large volume The LVI program usually calculates this parametersince the exact time to cut off is critical for the LVI injection to properly operate This time determines the volume of residual solvent that is allowedto enter the analytical column Setting Up Parameters for an LVOCI Setting up parameters for an LVOCI method is a three step process configuring instruments for LVI calculating optimum parameters and then downloading parameters to the
81. ime is a measure of time that sample components spend in the mobile phase Hold up time is measured to determine the average linear velocity F outlet flow in ml min measured at Tref and pref standard conditions F 60pr 16hL pi po po po pref Tref T Eq 1 average linear velocity at column temperature T cm sec TRACE Gas Chromatograph Setup User s Manual 2 33 TRACE Menu 2 34 x L tM Eq 2 Under a given set of experimental conditions the average linear velocity can be calculated from the column dimensions viscosity and pressure D 3r 32hL pif po pi pobo 3 Flow can then be determined indirectly from the average linear velocity 2 EK 3 2 2 vun F 60pr Tref T 2 pi po 3 pref pif pof UU Eq 4 The equation used to calculate inlet pressure from velocity could be quite slow under certain column conditions At outlet pressures greater than vacuum the equation cannot be solved directly Instead the equation is solved by a successive approximation method You can speed this process up by using the flow slider bar to indirectly change the velocity value Electronic pressure control EPC provides an alternative to mechanical pressure control for regulating the gas flow in your TRACE GC Ultra Additionally EPC provides stability and precision in flow settings which makes it possible to use pressure flow programming in GC methods and to document pressures along wi
82. ing l C Nea Polarity ma I Goen o GE CUTE r 5 oi Zuto r Ost Target Curent fis pE Cancel _ Figure 3 20 Add Run Time Event Page View Event Time group box Select one of the following two options This option makes the selected Detector Valve or External happen before the run begins This option makes the selected Detector Valve or External happen at the time specified during the run Detector Event Group Box Click the detector event button to activate a selected detector group of events Only the detectors you have selected from your TRACE GC Ultra Instrument Configuration program display in the Instrument Setup window Select the one you wish to add a run time event for during this run Each detector has some programmable events and the ones you have available depend on your detector selection TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Autozero Range Gain Neg Polarity Source current Lamp Lamp current Valve number Valve type Setting Thermo Finnigan Select this option to cause the detector offset to automatically adjust and force the output signal to zero 1000 signal counts Select this option to change the electrometer sensitivity for ionization detectors This function is useful for known sample matrices which exhibit wide and varying analyte concentrations Select this option to change th
83. is the temperature the oven will be at Checking the Link to Large Volume Assistant program located on the Configuration Inlet dialog disables this control This is because you are able to set these controls in the Large Volume Assistant program which you will find located in the autosampler menu If you want to activate this control then uncheck the Link to Large Volume Assistant program located on the Configuration Inlet dialog box The amount of time to maintain the initial temperature The rate of change of the temperature when increasing the temperature from one value to the next Described in degrees Celsius per minute C min The ramp begins at the previous step s final temperature value and proceeds to the current step s final temperature at the specified rate The temperature the oven is set at for the next ramp of the temperature program For isothermal runs this is the oven temperature for the run After Preready or Prep Run this is the temperature the oven will be at The time to maintain the temperature specified in the Final Value control box Oven Group Box This refers to an installed subambient additional purchase which allows subambient oven cooling Specify the maximum temperature for this run The GC has a maximum temperature of 450 The maximum allowable temperature for the column being used in the method is automatically set Specify how long the GC should remain in the Ready to Inject mode before
84. its kPa psi or bar and outlet pressure 1 atm vacuum or outlet settings save and load automatically when you open the screen again Values for all of the other parameters return to the factory default settings Related Topics For other details refer to e Pressure Flow Calculations e Split Ratio Calculations e Average Linear Velocity e Vacuum Outlet Conditions Other Pressures TRACE Gas Chromatograph Setup User s Manual 2 27 TRACE Menu 2 28 X Pressure Flow Calculations The rate of carrier gas flow through an open tubular column can be calculated using the well understood relationships between pressure and flow in capillary GC These calculations are useful in your method development and for you to determine the inlet pressure for a particular column and carrier flow or the change in flow resulting from a temperature or pressure program The TRACE GC Ultra performs a column evaluation where the actual column resistance is calculated Thus insuring and achieving accurate column flows for a specific column length i d and the wall coating Split Ratio Calculations The split ratio for a capillary inlet is determined by the relationship between the split vent flow and the column flow Chromatographers calculate split ratio in several ways and refer to this subject as split flow column flow column flow split flow or total flow column flow For these calculations split ratio is defined as Split Ratio S
85. ivstadenendeesveesssiedbsnseevecdeee 18 LACUS TADS wey chav E E piatass EE E eete tesusniganaeisnesainde 18 ISS saan seni E ceafudsy szdesmeaaiacovecds vvaclalesbetatevese Gena vadint auton neibycciaeeebes 18 Temperatures page 20 19 Ellen EE 19 ET 19 K ypad tcctsissreslevedeshendiclerr aati aii E dee 19 Chapter 2 TRACE E E 21 Menu DescriptOn EE 22 Using Flow Calculator eelste Eege ied uni 25 Column Flow Calculator Page AA 25 Using slider bar and buttons oo eee ceeeeeeeceeeeeeeeeaceaecesaecaeceeeeeeeeeeeseaeeaaeenaeees 26 Related TOPICS E 27 Using Vapor Calculator E 31 Vapor Calctlator Page garen duugEue Jeske tsactiacs eebe d it nee A 31 Related TOPICS satticncdetcvescigcvasieidaeotesse Sege gheet 33 Chapter 3 Instrument Setup 555 sesasas GesdesGavcisesissicae cin ues Eed 35 Edit TRACE GC Ultra Parameters iseccseics ci ivsctecsccaceisetaa deeds ENEE AAA EET E E 36 IMtrOGUCHION EE 36 LO Open this View eiert ast Re eae ToN Ee E EAEE E OE E 36 Using the TRACE Tab E 36 Related TOPICS ciasctiessduteveivcstesetesuasateccen SEENEN et de g der 37 Oven e E E tare au avis sities Shen ares dint nits ature Ai dea decnnaieiideal 38 Oven Page Parameters sista siisteacteiasedeeiassecnadsaddnagt NE E aa 38 Setting Up Oven Ramp Parameters 0 cece ceseeseceseceeeeeeeceseeeaeeeaeesaeeeeeeaeeeeeaes 40 Thermo Finnigan____ s TRACE Gas Chromatograph Setup User s Manual iii HENSE E E P CAEG deed REENEN SEANCE 42 UFM Page Par
86. ld the slider and drag it along the length of the slider bar e Click on the arrow buttons on either end of the slider bars to increase or decrease the associated value The amount of increase or decrease depends on the number of decimal places in the parameter and will vary for different slider bars es Click on the area between the slider and the arrow buttons to increase TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu Thermo Finnigan or decrease the slider bar s associated value at 10 times the rate of clicking on the arrows e Use your mouse or tab key to select a slider bar and then use the right and left arrow keys located on your PC s keyboard to adjust the values This method produces the same results as using the arrows Radio Button 1 Atm Vacuum Other Use radio buttons to select one or several choices however only one radio button from any group can be selected at the same time Reset Button Click to reset all control parameters back to the factory settings The only parameters for which default values can be changed and saved are pressure units kPa psi or bar and the controls listed in the Column Outlet Pressure group box 1 atm vacuum other and outlet pressure Done Button Press Done to exit the screen The pressure units and outlet pressure currently selected save to disk and become the new defaults for the remaining work session Current pressure un
87. led to split the analytical column flow between the Mass Spec and the Flame Ionization Detector FID An SGE outlet splitter union with fused silica transfer lines at a combined i d of 70 80 if the i d of the analytical column is used to make the split The kit includes a single hole ferrule for the analytical column side of the union and a two hole ferrule for the split side for attachment of the two transfer lines to the Mass Spec and the GC detector The actual split is initially calculated to balance the flows between the two outlets with one operating under vacuum Mass Spec and the GC Detector at atmospheric pressure The response may be enhanced on the Mass Spec by shortening the transfer line diverting more of the split to it than the GC detector Since the sample is being split between two outputs the injection volume must be doubled Installing the System to Meet Instrument Specifications The GCQ should be installed to manufacturing specs with the standard test column connected to the splitless injector and the Mass Spec After specs have been met the Mass Spec is shut down and the splitter installed Two microliters of the 3 component GCQ test mix is injected at a concentration of 1 ng uL in hexane The response retention time and peak shapes are checked The retention times on the Mass Spec and the FID should be within 0 02 minutes of each other and the peaks should not show any significant tailing The response for the i
88. lit such that the flow volume is reduced but the analyte concentration is enriched in the exiting gas stream See also open split An optional Auxiliary Interface An open split interface is used to reduce the flow of the column effluent eluting from the GC column to a lower one that is compatible with the vacuum system of the TRACE GC Ultra An open split interface typically consists of a column transfer line with a mass spectrometer transfer line placed near or inserted into that column transfer line The system may also use an additional makeup or purge gas for finer flow control The column transfer line is typically of a wider bore than the mass spectrometer transfer line and as such only a specific percentage of the column effluent enters the mass spectrometer This split is non discriminatory that is an approximately equal percentage of both sample and carrier gas is split away from the mass spectrometer See also jet separator TRACE Gas Chromatograph Setup User s Manual 1 17 TRACE GC Ultra Configuration K 1 6 Road Map Home Page Status Tabs Status pages for your TRACE GC Ultra are located on your Xcalibur Roadmap Home page Just highlight TRACE GC Ultra from the Roadmap Status tab scroll list and see the following pages status temperatures flows and pressures display the current GC status Status Tabs Status Temperature Flow Pressure General Status Not connected Run Elapsed tim
89. ll cause too little flow to be present during the desolvation period overloading the vacuum system of the mass spectrometer Some parameters will be grayed out in the GC and autosampler method parameter after downloading the LVI method These values are calculated and automatically set by the LVI software If you are using a TRACE GC Ultra check to see that the initial pressure time is equal to the inject time plus the SVE delay time You may need to change this manually If you are using a CE 8000 Top and you note residual solvent in the background spectrum throughout the run shorten the fused silica line on the SVE valve For injection of 100 uL of Hexane remove 15 cm TRACE Gas Chromatograph Setup User s Manual 3 57 Instrument Setup 3 8 PKD Page Temperature check box 3 58 and text box x This page is the method editor for the packed column inlet To display this page Click on the PKD page from the Instrument Setup view Oven UFM Left PKD Left Carrer Right PPKD Right Carrer Right FID Run Table Inlet MV Temperature TC 35 Figure 3 8 PKD Page View Related topics e Setting Up Parameters for PKD PKD Page Parameters Inlet Group Box This is the temperature setting for the packed column PKD inlet The allowable entry range is 30 400 C This temperature is usually selected to be 20 above the evaporation temperature for all components of interest in the analysis s
90. lume Temperature Pressure gauge Vapor Volume Thermo Finnigan A liquid sample injected into a heated GC inlet rapidly vaporizes and expands Vapor Volume Calculator rapidly calculates the expansion volume using several factors solvent injected liquid volume temperature and inlet pressure Included with this calculation is the resulting vapor expansion volume relative to the inlet liner s inner dimensions Because if the volume of vapor is greater than that of the liner the excess can expand into other areas of the inlet and result in loss of sample or contamination of the gas lines Vapor Calculator Page apor Volume Calculator x m Inlet parameters Solvent parameters Injection volume pl 1 0 Type Methylene chloride WR 2 Temperature C 200 Boiling point C 40 Wm Al Density g ml Pressure gauge kPa 101 3 A m gt Mol weight Lamut Vapor volume Liner volume Yapor volume ml 0 30 Type CE Instruments part no PTV 2mm metal 45322044 DI Liner volume ml 0 38 ret Figure 2 3 Vapor Calculator Page Inlet parameters group box Slide the bar to the volume amount to inject Slide the bar to the temperature your method calls for Slide the bar to the pressure amount your method calls for Vapor volume group box An injected solvent s calculated expansion volume Compare this to a list of the most frequently used liners and their available internal volume
91. m The jet separator is sometimes referred to as a momentum separator or an enrichment device A jet separator is used to reduce the flow of the column effluent eluting from the GC column to a lower one that is compatible with the vacuum system of the GCQ and TRACE A jet separator consists of two quartz jets that are separated by a small gap which is held under vacuum The first jet is connected to the end of the GC column where it receives the GC column effluent as it elutes from the column The second jet is connected to a piece of tubing 1 16 inch i d glass lined stainless steel or 0 53 mm i d deactivated fused silica that is TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE GC Ultra Configuration open split Thermo Finnigan connected to or passes through the transfer line of the GCQ As the column effluent exits the first jet it must jump across the gap into the second jet to be transferred to the MS Because the carrier gas has a low molecular weight it tends to diffuse and its stream spreads out in space as it exits the first jet thus only a small percentage of the carrier gas makes it into the second jet Analyte compounds are of higher molecular weight than the carrier gas and do not spread out as much in space as they cross the gap Thus a higher percentage of the analytes relative to carrier gas are able to cross the gap into the second jet and move into the MS This acts as a discriminatory sp
92. mL min for the y axis A flow for the analytical column For an oven temperature programmed run the GC automatically increases pressure to keep a constant flow on the column compensating for increased viscosity of gas due to increase in temperature Vacuum Compensation check box Check this box to compensate for a vacuum at the end of the analytical column This is usually the case where the detector is a mass spectrometer When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure Gas Saver check box and group box This group box contains gas saver controls which reduce carrier gas consumption especially when a large split flow is used The gas saver options are set to come on at some point well after the injection to conserve gas Checking the box will activate the other two features of gas saver The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run The time after the injection when gas saver flow will be activated Constant Pressure Mode Click on the Carrier tab of the GC Setup view and then click on Constant Pressure in the Flow Mode list box Use the Carrier page with constant pressure option to select a constant pressure for the analysis The parameters are TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X
93. module is directly measuring the column flow This mode is useful for a short lt 30m wide bore capillary column 0 53 mm or gt as well as packed columns These column usually operate at flow rates gt 5 cc min so that direct column measurement is feasible Column evaluation is not performed for this mode TRACE Gas Chromatograph Setup User s Manual 3 61 Instrument Setup K Wide Bore w Surge This selection allows you to program a higher inlet pressure during the mode sample injection This reduces the vaporized sample volume and enhances the injection vapor cloud transfer onto the column in a narrow time window Thus yielding a better component resolution by the column Packed w Surge mode This selection allows you to program a higher inlet pressure during the sample injection This reduces the vaporized sample volume and enhances the injection vapor cloud transfer onto the column in a narrow time window Thus yielding a better component resolution by the column Setting Up Parameters for PPKD mode Setting Up Parameters for PPKD 1 Select the desired operation mode Wide Bore Packed mode Wide Bore w Surge or Packed w Surge mode 2 Go to the Inlet group box and select Temperature 3 Go to the Purge group box and select Constant Septum Purge or Stop Purge Time If you selected any mode w surge then go to the Surge group box Enter the desired parameters into the Surge Pressure control and the Surge Duration c
94. n addition to the sample s carrier gas to measure the gas conductivity when sample moves across both filaments Reference gas must be same type of carrier gas and use the same flow rate Signal Group Box Gain Set the gain to x1 or x10 When a x10 gain is selected the GCs sensitivity increases the detector output signal and electrical and mechanical noise amplification Negative Polarity Select this control to reverse the polarity output signal as a TC carrier gas function versus the sample and the analytical column channel right or hannel left used Setting Up Parameters for TCD These steps are typical parameters for analyzing samples using Helium as a carrier gas 1 In the Detector group box select Block Temperature and enter 150 Select Transfer Temp and enter 150 Check the Constant Filament Temperature box to turn the filament power on Enter 250 in the Filament Temperature text box 2 Inthe Flow group box select Makeup if you are using makeup gas Select Reference if you need to set a reference gas flow 3 Inthe Signal group box set the Gain ifyou need amplified sensitivity Select Negative Polarity to reverse the TC gaspolarity Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 87 3 16 FPD Page Auxiliary usage only This page is the method editor for the flame photometric detector To display this page Click on the FPD page from the Instrument Setup view Oven UFM Left SSL Left Carrer
95. nce of volatile analytes that would co elute with most commonly used solvents making split injection necessary One type of injection mode available on a Split Splitless SSL Injector In this mode the split vent is closed during the injection and a large amount of sample is transferred to the GC column from the injection port This type of injection is used for trace residue analysis See also split splitless injector and split vent A type of injector available on a gas chromatograph This is the standard injector offered on the GCQ The SSL Injector is made up of a septum nut a septum a liner a metal body an influent line for the carrier gas a septum purge vent and a split vent that allows a portion of the carrier gas to be vented into the atmosphere See also split vent purge vent carrier gas flow rate split injection and splitless injection The exit port of the Split Splitless SSL Injector The split vent is opened and closed by the split valve and or split solenoid When the split vent is open a portion of the carrier gas and sample mixture if present is allowed to pass through the split vent into the atmosphere Below room temperature or ambient temperature The oven of the gas gas chromatograph Ttemperature programmable injector and on column injector can be cooled to subambient temperatures if the appropriate valving and coolant supply is configured accordingly An option available on the with the split s
96. nnigan section by placing them in a vial of solvent A steady stream of bubbles will be seen The FID transfer line will be inserted into the FID beyond the jet and then pulled back 2 3 mm below the jet to prevent burning the end of the fused silica in the hydrogen flame which would result in loss of response The loss would be severe only a small peak for the solvent would be observed The make up flow for the FID is set to 30 ml min of nitrogen or helium with the air at 350 ml min and hydrogen to 30 ml min The detector temperature is set to 250 C The transfer line to the Mass Spec is inserted 2mm beyond the vespel tip of the heated transfer line into the trap The Mass Spec will indicate a vacuum of 20 mTorr at the lower flow rate of 0 8 ml min Setting up the Carrier Flow The carrier gas flow exiting the analytical column was set to 1 5 ml min helium in the constant flow mode The flow may be entered at the keypad on the GC during set up and then in Xcalibur in the method under Instrument Setup With the restrictor attached to the Mass Spec the carrier gas control is set to vacuum compensation off Leak Checking It is critical to tighten the splitter union so that no leaks are observed by checking with a gas leak detector It is not recommended to use any soap leak test solutions like SNOOP on any fittings on the GCQ Also check the bulkhead fittings on the back of the GC for leaks Evaluating the DFPC Modules for the Detector
97. ns Serial Port com l 7 Pressure Units kPa X Network Address 192 168 0 101 Get Annulla Figure 1 1 TRACE GC Ultra Configuration Window Select the TRACE GC Ultra and then select the configure button The following TRACE GC Ultra detector pages display General Page e Inlets Page e Detectors and Data Page e Auxiliary Page GET Use this button any time you want to automatically enter the configurations already entered into your TRACE GC Ultra This program automatically enters the exact configuration parameters that were programmed into the TRACE GC Ultra key panel embedded system However you will still have to enter the channel parameters located on the Detectors and Data page To open this view 1 Choose Start Programs Xcalibur Instrument Configuration 1 8 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan K TRACE GC Ultra Configuration 2 Click the TRACE GC Ultra button located in the Available Devices column 3 Click Add then Configure Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 1 9 TRACE GC Ultra Configuration K 1 2 General Page TRACE Configuration x N General o Inlets a Detectors and Data dP Ausbau and Oven options Connection Options Serial Port OMI e Pressure Units kPa Ce Network Address 192 168 0 101 Advanced Get Anra SCH Figure 1 2 General Page Connection Group Box Serial
98. ns are low and high The higher the lamp current the more intense the transmitted lamp transmission which enhances sensitivity but reduces lamp life 3 90 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Makeup Sheath Gas Range Analog Filter Thermo Finnigan Flow mL min Group Box Turns on the makeup gas Typical value is 15 mL min Flows around the outside of the cell to reduce temperature Typical flow value is 30 mL min Signal Group Box Changes the electrometer gain Valid selections are 1 10 100 1000 With one yielding the most sensitivity Electronic filtering used to reduce baseline noise Select On or Off The analog filter applies a time constant to the analog output reducing the response times to high frequency baseline noise thus filtering the analog output Setting Up Parameters for PID 1 In the Detector group box set the Base Temperature to 180 C Set the Lamp Current to low Optional selections Lamp On 2 Inthe Flow group box set the Makeup gas to 15 20 mL min Set the Sheath Gas to 20 30 mL min 3 Inthe Signal group box set the Range to X1 Optional selections Analog Filter TRACE Gas Chromatograph Setup User s Manual 3 91 Instrument Setup X 3 18 Aux Zones Page 3 92 Ths page is the method editor for the setting auxiliary connections All selections on this page must exactly match the settings you have manually entered i
99. nto your TRACE GC Ultra and the TRACE GC Ultra detector configuration window See Detectors and Data Page To display this page Click on the Aux Zones page from the Instrument Setup view Oven Left SSL Left Carter Right PTV Right Carrier Left FID Aux Zones Run Table Aux Temperature Zones M Aux 1 C 30 M Aux 2 C 30 Figure 3 18 Aux Zones Page View Related topics e Setting Up Parameters for Aux Zones Aux Zones Parameters Aux Pressure Zones Group Box When you check one of these boxes Aux 1 or Aux 2 you let the GC know you have an auxiliary heater Set a temperature from 0 450 If any of these pressure channels Aux 1 3 are connected to your TRACE GC Ultra then check the box and enter a value from 0 700 kPa TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan X Instrument Setup Setting Up Parameters for Aux Zones 1 Make sure that auxiliary configurations are selected in the TRACE GC Ultra Configuration program 2 Check either Aux 1 or Aux 2 in the Aux Temperature Zones box and then enter a temperature value of 0 450 3 Check if any of these pressure channels are present Aux 1 Aux 2 or Aux 3 controls located in the Aux PressureZones box and then enter a temperature value of 0 700kPa Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 93 Instrument Setup X 3 19 Run Table Page 3 94 Time Item This page is the method edi
100. ogen flow 0 200 cc min to activate Acceptable values are On Off When the Hz is turned on enter the value of Hydrogen to supply to the detector to optimize the flame Typical flow is 25 mL min Specify how much makeup gas 0 90 cc minute to activate Nitrogen is recommended as the makeup gas to the FID detector Acceptable values are On Off Makeup gas enhances FID sensitivity Typical flow is 30 mL min Signal Group Box The range for the detector signal to be acquired Selections are 1 10 100 100 however the lowest setting 0 gives the most sensitivity A higher range may be needed for high concentration samples Range represents the amount of current required in nano amps from the detector to offer a full scale output at the selected range Electronic filtering used to reduce baseline noise Acceptable values are On Off The analog filter applies a time constant to the analog output reducing TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Thermo Finnigan the response times to high frequency baseline noise thus filtering the analog output Setting Up Parameters for FID 1 2 Check the FID base temperature check box Check the base temperature box and set the temperature to 250 C Turn on the detector gas settings to H2 30 mL min Air 350 mL min Makup 30 mL min Turn the flame on TRACE Gas Chromatograph Setup User s Manual 3 81 Instrument Setup K 3 14 N
101. on trap will be quite a bit higher than on the Flame Ionization Detector FID Connecting a Post Column SGE Splitter Using an SGE Capillary Outlet Splitter two pieces of 0 1 mm i d fused silica transfer line were cut 60 cm in length for the Mass Spec and 20 cm in length for the FID Connect the analytical column to the inlet side of the splitter union and connect the transfer lines to the outlet side with a SGE two hole ferrule Connect the outlet end of the transfer line to the FID with the standard detector nut and the CE Instruments graphite ferrule Part 29013489 Materials Required TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan How To Thermo Finnigan e SGE phone 800 945 6154 e SGE Outlet Splitter 123630 e Fused Silica 0 1mm x 10 meter 062469 e Two hole ferrules 0 3mm i d 072660 e Single hole ferrule 0 4 mm i d 072663 Calculating Transfer Line Dimensions for the Mass Spec and the GC Detector The flow calculator in Xcalibur was used to determine the length and i d of the transfer lines for the split The flow calculator is accessed by selecting the TRACE GC Ultra icon button under the Instrument Setup Press the word Trace and Flow Calculator will be listed in the menu After selecting the Flow Calculator a dialog box will be displayed Select helium for the carrier gas type First determine the pressure above atmospheric pressure 14 69 psi required providing a flow rate of
102. ons in this box External Event Group Box External events are external valves switches and options Click the external event button to activate external events TRACE Gas Chromatograph Setup User s Manual 3 97 Instrument Setup K External number Select which of the eight 8 external events you wish to program There are 8 available open collector outputs on the GC rear panel which can be configured to switch external valves switches and other options Setting Select On or Off to set the external event at the specified programmed run time 3 98 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Thermo Finnigan Chapter 4 How To This Chapter contains these topics Installing the Desolvation Column and Connecting the Tee 100 Characterizing Columns 101 Post Column Splitting of the GCQ with the Flame Ionization Detector 102 Operating an FID with Xcalibur Software 107 Simultaneous Analysis on the Ion Trap and the FID 113 TRACE Gas Chromatograph Setup User s Manua 4 99 How To X 4 1 Installing the Desolvation Column and Connecting the Tee 4 100 Turn the carrier gas off at the keypad on the GC Open the butterfly valve to the OC injector and manually insert an extra 250 uL into the inlet The syringe needle will extend into the GC oven Install the desolvation column by sliding it over the needle using the needle as a guide Tighten the male nut with the tapered end of the fe
103. ontrol The PPKD inlet may be operated in two primary modes wide bore or packed In wide bore mode the inlet operates like a direct capillary inlet Column flow is not measured directly but is calculated from inlet pressure oven temperature and a measured k factor The k factor is automatically measured by the TRACE GC Ultra in the column evaluation process and represents a summation of selected factors such as the carrier gas type outlet pressure column resistance versus pressure and others In packed mode the carrier flow module measures the column flow This mode is appropriate for packed column and short wide bore lt 30 m and gt 53 mm i d columns These short columns do not provide enough resistance to flow to allow measurement of k factors for typical capillary column control As a general rule the inlet must provide column carrier gas flow control andvaporize the injected samples for transfer to the analytical column Because the proper temperatures and flow are sample and method dependent noguidelines are available 3 62 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 10 PTV Page This is the method editor for the programmable temperature vaporizing inlet This is a right inlet only Several controls require purchasing additional TRACE GC Ultra options To display this page Click on the PTV page from the Instrument Setup view Oven UFM Lett SSL Left Carer Ri
104. oo eee ceeeeeeesceeeeecneecnseesaeceaeceeeeeeeeaes 95 Using the Add Event Run Time Event Dialog 0 0 0 eee eeceesseceneeeeceeceneeeeeees 96 Chapter 4 PLOW DO EE 99 Installing the Desolvation Column and Connecting the Tee cece cecceeeceseeeeeeeeeeseeeeeeeenaeeeaeenaees 100 Characterizing Columns eet SeEEAEEE NEESS ils EENS 101 Post Column Splitting of the GCQ with the Flame Ionization Detector 0 eee eeeeeeeeeeeneereeeneees 102 ie ee EE 102 Installing the System to Meet Instrument Specifications cee eeeeeteeeeeees 102 Connecting a Post Column SGE Splitter oo ceeeceeeceeeceeeeeeeeseeeeaeeeenee 102 Calculating Transfer Line Dimensions for the Mass Spec and the GC Detector 103 Installing the Post Column Splitter 104 Setting up the Carrier PlOW satasccsiutcestinsideodssnachiaseadeesided nadeuaetivtia eatvinaecsiveedeodess 105 Leak Checking ET 105 Evaluating the DFPC Modules for the Detector and Carrier Gases 105 Operating an FID with Xcalibur Software oo eee eeceseeeseesnceeseceeceseeeseeseeeeaaecaeeeeseeeeaeeseeeeaaees 107 ege LEE 107 Configuring Xcalibur and the TRACE GC Ultra oo eecceseeeeeeereeeeeenee 107 Connecting the Gases eessen ees ebe eege ege 107 Installing the Test Column cece eeessecseceteeseeceseceeeeeaeeeaecaecnaeeeaeeeeseaeeenees 108 Column Character Zanon esseistinen ieccassovaveetuveh o eie an aia 108 Igniting the Plame eeiuegesugei reese Si teias vanced Hace eat este yeais asta as
105. ot done if the inlet temperature is set within 20 C of this value Instead a message displays indicating that a higher temperature should be specified For dense solvents with low molecular weights give the largest vapor volume per microliter injected The effects of inlet temperature and pressure on vapor volume can also be seen from the equation increasing temperature increases volume while increasing pressure decreases volume Molecular weight The average mass of a molecule of a compound compared to 1 12 the mass of carbon 12 and calculated as the atomic weights sum of the constituent atoms Or simply stated the average mass of a molecule of a compound expressed in atomic mass units AMU Liner volume group box Select a liner type from the list box Vapor Volume Calculator automatically displays the Liner Volume TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu Thermo Finnigan Related Topics Comparing Vapor Volume to Liner Volume Comparing Vapor Volume to Liner Volume Comparing vapor expansion volumes with liner volumes gives an estimate of the sample volume that can be injected under different conditions In practice mixing and diluting sample vapor with carrier gas during rapid evaporation means that the actual volume occupied by vapor may be greater than the calculated volume and it depends on the liner design and how rapidly carrier gas is moving through the inlet A good star
106. perature for the FID the detector will be turned on during acquisition and appear as an analog plot in real time at the bottom of the page with the real time spectrum at the top and TIC in the center UX C Xcalibur Data Test Mix with Splitter 04069915 RAW Real Time Plot File Actions View GoTo Help lala pela ale ele Alke gl 04089915 963 RT 13 12 P NL 6 32E3 EZ T Full ms 60 00 460 00 Stats Acquistion Queue 100 10911 2549 Sequence C Xcalibur methads 040699 sid Sample Name 3 on Working On Seq Row 15 Position 11 60 Raw File C Xcalibur Data Test Mix with Ster a Inst Method C Xcalibur methods testfid Sa 4 3108 amp AS2000 Autosampler 3 20 SZ 3148 Ready to Download 417 2 429 0 446 3 amp GCQ Mass Spectrometer oe i Running 50 100 150 200 250 300 350 400 460 amp TRACE GC 2000 miz Running RT 0 00 13 77 28 m CB ka 3 5286 304 me ms wl 04063315 136 ay a mi 60 4 OK H zen OK Z so OK oo OFF Esl 204 20 mT on lon Gauge Pressure OFF ein 4 14 458 480 509 636 6 1 740 ES sso SD 9 91 1048 NI nar 1222 19 06 n ese po H 1 2 3 H 5 6 DH 3 3 0 H D D Time min RT 0 00 19 35 VE m RB 1005 13067 304 Channel t BS echt 04063315 g mi 604 amp oi ES 373 10 03 10 43 13T 1216 Gan Time min NUM SCRL 4 6 99 5 08 PM Opening a Data File in Qual Browser To open a data file in Qual Brows
107. perature value in degrees Celsius in the Temperature text box Setting Up Parameters for Splitless Mode Use the following procedure to specify parameters for a splitless GC run 1 Open the Instrument Setup window 2 Click on the TRACE GC Ultra panel button 3 Select the SSL tab 4 Choose Splitless from the Mode spin box If you would like to enter a temperature for the injector click in the temperature check box then enter the desired temperature in the temperature text box If you would like to enter a split flow click in the Split Flow check box and TRACE Gas Chromatograph Setup User s Manual 3 47 Instrument Setup K enter a value mL min in the Split Flow text box 5 Enter a value in the Splitless time text box If you want to use constant septum purge click in the Constant Septum Purge check box Otherwise enter the time in minutes in the Stop Purge Time textbox Setting Up Parameters for Splitless with Surge Mode Use the following procedure to specify the carrier gas flow rate and pressure for ramped pressure 1 Open the Instrument Setup window 2 Click on the TRACE GC Ultra panel button 3 Select the SSL tab 4 Choose Splitless w surge from the Mode list box If you would like to enter a temperature for the injector click in the temperature check box and enter the desired temperature in the temperature text box If you would like to enter a split flow click in the Split Flow check
108. plit Splitless Large Volume Injection and on column injection The inlet system for a gas chromatograph The injector is a gas tight connection at the entrance of the GC column that delivers carrier gas to the column and provides a path for introduction of the sample into the GC See also Large Volume Injection on column injector split splitless injector and temperature programmable injector The charge on an ion positive or negative The part of a mass spectrometer where ions are formed molecular ions and fragment ions or in an MS MS experiment precursor ions Injection mode possible using a Finnigan TPI and the CE On Column Injector OCD In this mode up to 500 microliters of sample can be injected into the GC With the Finnigan TPI during the injection the temperature of the injector is held slightly above the boiling point of the solvent but below the boiling points of the analytes with the split vent open After most of the solvent evaporates the split vent is closed and the temperature of the injector is ramped quickly to a high enough temperature to cause the analytes to vaporize and be swept onto the analytical column LVI is accomplished with the CE On Column Injector by incorporation of a desolvation pre column connected through a tee union to the analytical column and the solvent vent valve During the injection the oven temperature is held below the boiling TRACE Gas Chromatograph Setup User s Manual 5 123
109. plitless injector If the Use Surge Pressure check box is selected in the GC Instrument Setup window Pressure tab you can enter the pressure to surge to in psi the time minutes into the GC run for the surge to come on and the time for the surge to go off During the GC run the head pressure will be set to the value specified in the Pressure box and the On Time and it will hold at that pressure until the Off Time The selected head pressure will override the EPC value s while it is on surge pressure is often coordinated to be on during the injection of a sample into the injection port By surging the pressure during the injection then the sample is pushed more quickly onto the GC column in a tighter band This helps improve loading of the components The surge pressure it also useful with analytes that are thermally degradable and tend to break down when exposed to the high temperatures of the injector Using surge TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Glossary X temperature program temperature programmable injector total time UltraFast Module Thermo Finnigan pressure helps to sweep the sample out of the injection port and onto the GC column quickly See also electronic pressure control A temperature program where the oven temperature is changed at a specified rate The TPI is an injector available as an option for the Finnigan GC This injector provides the capability for temperatur
110. quisition Time min Ee Oven Run Time 3 00 C Specific Time f10 00 Figure 3 2 TRACE GC Ultra Oven Page View Related topics e Setting Up Oven Ramp Parameters Oven Page Parameters Oven Temperature Program graph Graphical representations of the oven temperature program including any post run events The axes are temperature in degrees centigrade and time in minutes An isothermal run just gives a flat line Oven Temperature Program Parameters Ramps arrow buttons Use the up down control to add or subtract the number of ramps to use in the oven temperature program This is the rate in degrees Centigrade per minute 3 38 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X Initial Temp text box Initial Hold Time text box Ramp Rate text boxes Ramp Temp text boxes Ramp Hold Time text boxes Oven Subambient check box Max Temp text box PrepRun Timeout Thermo Finnigan the GC oven is ramped up or down from the initial temperature or the previous level s final ramp temperature Clicking on the Down arrow automatically adds a ramp level after the last one listed Clicking on the Up arrow deletes the highest level or the one being displayed on the bottom The initial temperature the oven is set at the beginning of the temperature program For isothermal runs this is the oven temperature for the entire run After Preready or Prep Run this
111. re 1 4 Detector and Data Page Configuration changes are stored with a method s configuration file A method uses the stored configurations so that a change in configuration results in making the method incompatible You will not be able to load a method if it was created with a different configuration Remember that you can upload a method from the GC to save with the new method Detectors group box Select the detector type None FID ECD NPD TCD FPD PID installed on your GC s right inlet connection The right side is as you are facing the front Select the detector type None FID ECD NPD TCD FPD PID installed on the GC s left inlet connection The left side is as you are facing the front TRACE Gas Chromatograph Setup User s Manual 1 13 TRACE GC Ultra Configuration Auxiliary Detector Gas Flow Control Line Frequency Channel 1 3 Channel Name Scan Rate Hz X Select the detector type None FID NPD FPD installed on the GC s AUX position Option Group Boxes Configuration option for the Detector method editors The default for this check box is checked on in which case you get the detector method editor controls with Flow text edit controls If you unselect this checkbox then all detector gas flow text edit boxes in the detector method editors are removed then you may check on or uncheck off the gas flow check boxes In other words if this configuration option is on then you can
112. res the spilt valve be opened after the injection to prevent band broadening due to solvent flooding Splitless times of 1 minute are typical A surge is applied during the splitless time to reduce residence time of the analytes in the inlet This will reduce band broadening and may sharpen peaks especially for more volatile components which are not improved by cold trapping effects on the column Usually this technique involves an oven temperature 50C below BP of analyte Inlet Group Box The setpoint for the inlet s temperature Depending on the mode of injection it should be set at a temperature appropriate to vaporize the sample and solvent Specify the total split flow coming out of the inlet This is the total flow out of the inlet when the split valve is open The ratio of split vent flow to the column flow Calculate the split ratio as shown Split Ratio column flow split vent flow column flow The amount of time after the injection at which the split vent opens Purge group box This group controls the septum purge for the inlet Septum purge is used to sweep the bottom of the septum to reduce contamination from sample analytes This prevents carryover from run to run Septum purge also prevents contamination of the inlet from septum bleed The septum purge may be turned off during a splitless injection Checking this box will keep the septum purge valve open continuously By leaving this box unchecked the an
113. returning to Stand By If the GC Start button is not pressed within the prep run timeout period then the GC will return to Stand By mode This feature is a protective measure to keep the GC from being in the Ready to Inject mode too long For example this will prevent accumulation of contaminants on the analytical column when doing splitless injections TRACE Gas Chromatograph Setup User s Manual 3 39 Instrument Setup Equilibration Time min text box Use Oven Run Time radio button Use Other Time button and text box Temperature text box 3 40 Time text box Pressure text box X Specify how much time the GC should wait after the initial conditions are met before going to standby Acquisition Time Group Box Check this box for the Acquisition Time to be the same as the oven run time however this does not include the post run time You can define the time for acquisition Enter a value in the text box Post Run Conditions check box and group box Use this option to specify post run conditions When you select the Post Run Conditions check box the group box becomes active The post run temperature setpoint Use as a bakeout to clean up the column or use as a cool down phase after the run has finished The amount of time the oven remains at the post run temperature setpoint The post run pressure setpoint for the left and right EPC inlet Setting Up Oven Ramp Parameters Setting Up Oven Ramp Parame
114. rge Time min 0 00 m Surge Surge Pressure kPa 3 Surge Duration min 0 00 Mode Splitless w Surge Figure 3 4 S SL Page View Related topics e Setting Up Parameters for Split Mode e Setting Up Parameters for Splitless Mode e Setting Up Parameters for Splitless with Surge Mode SSL Page Parameters SSL Modes list box Use this spin box to select one of the following The carrier flow is split in the injection port with the bulk going out the split vent Use this injection type when analyzing high concentration or neat samples or in instances where sensitivity is less important The split vent remains open all the time This method yields the sharpest peaks if the split TRACE Gas Chromatograph Setup User s Manual 3 45 Instrument Setup Splitless Splitless w surge Temperature check box and text box Split Flow check box and text box Split Ratio text box Splitless Time text box Constant Septum Purge check box Stop Purge Time text 3 46 box X gas is properly mixed Additionally this technique can improve peak shape and resolution The split vent is closed during the injection to drive most of the sample into the column Solvent effect is required to refocus the analytes especially more volatile components You can achieve solvent effect by keeping the analytical column or guard column near the sample s solvent boiling point This technique also requi
115. ring used to reduce baseline noise Acceptable values are On Off The analog filter applies a time constant to the analog output reducing the response times to high frequency baseline noise thus filtering the analog output Setting Up Parameters for FPD 1 In the Detector group box set the Base Temperature to 250 C Set the FPD Temperature to 180 C Set the PMT Voltage to low Optional Flame On 2 Inthe Flow group box set the Air to 200 C Set the H2 to 150 C Set the Makeup gas to 30 C 3 Optional In the Signal group box set the Range and Analog Filter TRACE Gas Chromatograph Setup User s Manual 3 89 Instrument Setup K 3 17 PID Page This page is the method editor for the photoionization detector To display this page Click on the PID page from the Instrument Setup view Oven UFM Left SSL Left Carier Right PTV Right Carrier Left NPD Right PID Run Table m Detector Signal I Lamp On Range fi x MV Base Temperature C 35 I Analog Filter Lamp Current Low r Flow ml min IT Makeup 20 IT Sheath Gas 20 Figure 3 17 PID Page View Related topics e Setting Up Parameters for PID PID Parameters Detector Group Box Lamp On Turns the UV lamp power on which strikes the lamp and thus creates a lamp current Base Temperature Turns the detector base body temperature on Lamp Current Selects the PID lamp current Valid selectio
116. rrule pointing up while pressing the column upward as far as it will go Tighten the nut with a wrench La turn beyond finger tight Be sure to install the uncoated or front end of the column into the injector Use the GCQ software to open a new method in the method editor and save it to a new name This is your LVI method Press the GC icon and then select Inlet and change the inlet selection to left Save the method and then send it to the GC This will switch the DFPC or carrier gas control to divert the carrier gas from the right inlet to the left Turn the carrier gas on at the keypad on the GC Place the effluent end of the desolvation column into a vial of solvent and note bubbles indicating flow Position the end of the desolvation column with a ferrule and nut loosely into the tee If the tee has not been installed remove it from the bag and insert it into the solvent vent valve bulkhead from inside of the oven with a ferrule and 1 16 nut Slide the analytical column into the tee and inside the desolvation column with the ferrule and nut in place The analytical column should protrude through the desolvation column about 4 cm Tighten the fittings 4 turn beyond finger tight Note flow through the end of the analytical column by placing the end in a vial of solvent Install the column into the mass spectrometer as described in the GCQ Plus Hardware Manual If the analytical column was previously installed in the right inlet simply move i
117. s When using the GCQ Plus Mass spectrometer 1 Press the mass spectrometer icon button Select the first line for the first segment and double click the left mouse button The dialog box for the MS opens Enter the appropriate values and set the start time to 5 0 minutes or longer You will have a residual amount of solvent going through the detector and want to delay the filament ignition until after this solvent has passed through Select a time that provides detection of the first analyte but not the solvent ook at the fore pressure located on the homepage Status page during the first run to verify the time for the solvent to pass out of the mass spectrometer The fore pressure may be monitored during filament delay Save the method Set the mass spectrometer to a high pressure operation mode by selecting the CI mode from the GCQ Plus front panel Downloading LVI Parameters into the GC Method 1 From Instrument Setup click on the autosampler icon The autosampler menu displays on the menu bar which contains two selections necessary to run a large volume injection select Run Large Volume Program and the Load Large Volume File Select Run Large Volume Program to begin creating a LVI method file For step by step instructions on how to create LVI method files just click the Help button listed in the LVI dialog box Be sure to save the file TRACE Gas Chromatograph Setup User s Manual 3 55 Instrument Setup Run
118. s for NPD 1 In the Detector group box set the Source Current to 2 720 or as required to generate a background current Set the Base Temperature to 300 C Set the Polarization Voltage to 3 5 2 Inthe Flow group box set the Air to 7 0 Set the H2 to 3 0 Set the H2 delay to how many minutes you want to wait before starting the hydrogen flow Set the Makeup gas to 15 3 Inthe Signal group box set the Range to the desired sensitivity Check the Analog Filter box if you want to reduce the response to high frequency noise and signal 3 84 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup X 3 15 TCD Page Block Temperature Transfer Temp Thermo Finnigan This page is the method editor for the thermal conductivity detector To display this page Click on the TCD page from the Instrument Setup view Goen UFM Left SSL Left Carrier Right PTV Right Canier LeftFPD Right TCD Run Table m Detector r Signal V BlockTemperature C 35 Gain vi OF CS V Transfer Temp CH I Negative Polarity T Filament Power Constant Filament Temperature Filament Temperature 50 Filament Voltage 5 Fil Max Temperature 50 gt Flow ml rnin IT Makeup 20 T Reference 20 Carrier Source Right zl Figure 3 15 TCD Page View Related topics e Setting Up Parameters for TCD TCD Parameters Detector Group Box Sets the TCD cell temper
119. sure at the column outlet po is about 1 atm In GC MS systems however the column outlet pressure is zero This makes the flow rate at outlet conditions very high but column flow under reference conditions can still be calculated from equation 1 This corresponds to the flow that would be measured with a flow meter connected to the discharge of the vacuum pump if such a measurement could be made With po lt lt pi equation 1 becomes F 60mr 16 NL pir pret Tret T Eq 4 Other Pressures There are some cases where the column outlet is neither at atmospheric pressure nor under vacuum One example is a column with a restrictor installed at the end This could be a length of narrow bore tubing connected to a mass spectrometer as discussed in the topic Vacuum Outlet Conditions or a splitter with connections to two different detectors Another example is in work with the atomic emission detector AED where the cavity has a positive pressure of about 1 5 psig When the total pressure drop is low that is with short wide bore columns this can cause a significant difference between the calculated and actual flow values Selecting the other setting for outlet pressure on the flow calculator allows the appropriate value 14 7 1 5 16 2 psia to be entered and used in the calculations TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan TRACE Menu X 2 3 Using Vapor Calculator Injection vo
120. t Flow Mode o 0 eee eesceeseeeeeeneceeeeeeeeeaeeeaes 73 Setting Up Parameters for Constant Pressure Mode AA 74 Setting Up Parameters for Programmed Flow Mode AAA 74 Setting Up Parameters for Programmed Pressure Mode 75 ECD WEE 77 BCD Parameters soccorsi onere Ene EE EEE EREE EE ETE EER 77 Setting Up Parameters for ECD o oo cece eccceceeeeeeeseesseeceseneceeneeceeeeeeaeneaaeceeaeeeeaes 78 BUD RS 79 FID Pairamnie teenrina a EE EAEE 79 Setting Up Parameters for FID sirsersicissiorssetieresisiresise kasesinin 81 A a D RTE 82 NPD SE 83 Setting Up Parameters for NPD A 84 TOD Pa Se sereni eaea i o NEEE E dies ANE Geesse getest dE Aere Edge 85 Ke Eu EE 85 Setting Up Parameters for TCD o e cc ececcceceecceceteeesaeceeeeeceeeeeceeeeesaeeeaeeneaeeeaes 87 IS NR 88 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan X FPD Parameters sasc sscec sanecsssais attests on e E EA O E EEE 88 Setting Up Parameters for PPD crsssiiisieicons eiiieaenii eisi 89 PID Pace o ee oeiee ea A A E TEE EAEE EOE EA EE E TE N tees TRE 90 PID Parameters EE 90 Setting Up Parameters for PID wecticcssiccsecccacsccecentsscies coueceveaecusd sense aieaeeecatenussctioosces 91 AUX ZONES Pape site travian niente E EENS 92 AUX Zones Parameters eege gidd 92 Setting Up Parameters for AUX ZONES 0 eeesscceseceeceseeeeeeeaeeeeaeesaecsaecneeenseeeaes 93 Run Table Page Zenger aen geegent Eeer EES 94 Rum Table E e 94 Setting Up Parameters for Run Table
121. t to the tee You do not have to shut down the mass spec since the restriction of the narrow bore capillary will prevent venting the detector to atmosphere Proceed to Characterizing Columns TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan K How To 4 2 Characterizing Columns Columns must be characterized after they are installed in order to deliver the correct flow rate set in the GC Method Editor The procedure is performed at the keyboard of the GC A constant for the algorithm for regulation of column flow is determined This constant K is the restriction of the column Column characterization may be invoked at the keyboard of the GC Press the column characterization button The display will show the electronic gas control change the pressure and record the actual flow rate for each setting These values will be inserted into a formula to calculate the K value or restriction of the column To test the column for leaks raise the oven 50 C higher than the temperature that the column characterization was performed and press the LEAK CHECK button on the GC Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 4 101 How To X 4 3 Post Column Splitting of the GCQ with the Flame lonization Detector 4 102 Introduction Through Xcalibur a simultaneous analysis may be made on a GC detector and the Mass Spec from of a single injection A post column or effluent splitter may be instal
122. ters Set oven ramp parameters 1 Open the Instrument Setup window 2 Display the Oven page by clicking on the TRACE panel button 3 Type in the temperature degrees Celsius and time in minutes for the initial oven parameters 4 To add ramps to the oven temperature program click on the down arrow of the up down control If you add too many ramps click on the up arrow to delete them Set post run conditions Select the Post Run Conditions check box and enter the time temperature and pressure parameters 1 To keep the default analysis time check the Total Run Time box If you want to set a different analysis time leave the Total Run Time box unchecked and enter a value for the analysis time TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan X Instrument Setup 2 Select Oven Subambient if your system has this option for subambient cooling 3 Enter the Max Temp and Equilibration Time values Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 41 Instrument Setup K 3 3 UFM Page This page is the method editor for setting up parameters in the GC run To display this page Click on the UFM page from the Instrument Setup view Oven Left Inlet OCI Left Carrier Right Inlet PTV Right Carrier Left Det FID x Right Det TCD Run Table 50 25 W Sa A S Cn GLI LS TSU Sn LG S D SEN SES DS OESS LSS 0 00 020 040 0 60 O80 1 00 1 20 1 40 1 60 180 200 220 24
123. tesdadaaynetnn 108 Setting up the Method visi secs sc csscediccees fiscesetbaccesed inaidai 108 Setting up a Sequence in Xcalibur for Acquisition of the FID Only 00 109 Setting Up Qual Browser for the FID Analog Chromatogram eee 111 Meeting FID Specifications 00 ee esesseceseccsseeeeceeeceseeeseeesaecsaecneeeseeeeeeeneeaee 112 Simultaneous Analysis on the Ion Trap and the FID 113 E eg LEE 113 Instrument Method Set Up cecccesesssseseeseecenteseesseesseceeneeceteonetenesseetsesenseesnaee 113 Opening a Data File in Qual Browser 00 0 eeceecessseceeecnseceeeeeeeeeeeeaeeeaeesaeenaaees 114 Developing a Processing Method AAA 117 Report Writing EE Ree ESA 120 Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual V Chapter 5 EOIS EN PA vi TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Chapter 1 TRACE GC Ultra Configuration This chapter contains the instruction to configure your TRACE GC Ultra This chapter contains these topics Introduction 8 General Page 10 Inlets Page 11 Detectors and Data Page 13 Auxiliary Page 15 Road Map Home Page Status Tabs 18 Thermo Finnigan TRACE Gas Chromatograph Setup User s Manua 1 7 TRACE GC Ultra Configuration K 1 1 Introduction This dialog box is available from the Instrument Configuration window TRACE Configuration x General lg Inlets a Detectors and Data Auxiliary and Oven options Connection m Optio
124. th the other parameters TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Thermo Finnigan Chapter 3 Instrument Setup This chapter contains the instructions to edit the TRACE GC Ultra parameters according to the inlets and detector installed This chapter contains these topics Edit TRACE GC Ultra Parameters Oven Page UFM Page SSL Page OCI Page HOTOC Page LVOCI Page PKD Page PPKD Page PTV Page Carrier Page ECD Page FID Page NPD Page TCD Page FPD Page PID Page Aux Zones Page Run Table Page TRACE Gas Chromatograph Setup User s Manua 36 38 42 45 49 51 53 58 60 63 68 77 79 82 85 88 90 92 94 3 35 Instrument Setup X 3 1 Edit TRACE GC Ultra Parameters Introduction The parameters to set for the TRACE GC Ultra oven injectors and detector should be set according to your GC configuration All parameters can be sent to or loaded from the instrument connected by using the functions available in TRACE Menu To open this view 1 Choose Instrument Setup from the Home Page window 2 Click on the TRACE panel button located in the Instrument Setup window X Roadmap Home Page Fie Actions View Tools GoTo Help aale lei mj gl Status Acquisition Queue E Run Manager No Devices Sequence Sample Name Working On Position Raw File Inst Method B AAS 3000 Detached B TRACE GC 2000 Detached ON LINE Browser
125. the analyte has a retention time on the column of 5 14 Cools the On Column Injector and the first few centimeters of the GC column This is an external gas supply typically bottled air or CO3 that is supplied to the secondary cololing valve located on the rear of the GC Use this option to cool the column head and the first few centimeters of column where sample is introduced Flow rate is depencdant upon the pressure supplied from the gas source Secondary cooloing gas consumption is usually very large so you should minimze the time between the GC Ready mode and Run Start mode One type of injection mode available on a split splitless injector As the injection is made and at all times during the GC run the split vent is opened TRACE Gas Chromatograph Setup User s Manual 5 125 Glossary splitless injection split splitless injector 5 126 split vent subambient temperature surge pressure X to allow a specific portion of the sample to be swept into the atmosphere that is split away while the rest of the sample is swept onto the GC column Only a certain percentage of the sample makes it onto the GC column depending on the ratio of the split flow to the column flow the split ratio Split injection is used for the analysis of high concentration samples that would overload the GC column if all of the sample were placed onto the column Some types of samples can not be diluted with a solvent because of the prese
126. ting point in method development is to choose the liner injection volume temperature and pressure so that the vapor volume does not exceed the liner volume For splitless injections the liner volume should also be considered in choosing the purge hold time so that the inlet will be swept at least once by carrier gas flowing onto the column Typical volumes for capillary inlet liners have a range of 250 to 1000 microliters Volume for an open liner can be calculated from the length and inner diameter but it may be reduced by internal constrictions or packing Rate of carrier gas flow at the column outlet usually given as volumetric flow in ml minute Because the volume for a given mass flow will depend on temperature and pressure pV nRT the conditions under which flow is calculated or measured must be specified See the section on Column Outlet Flow for details of the calculations Velocity at which carrier gas moves through the column at temperature T is represented in cm sec Because pressure varies continuously along the column from pi to po linear velocity also changes at each point between inlet and outlet The elution time for an unretained component provides a measure of the average linear velocity This is related to outlet velocity and flow through the compression correction factor j See the topic on Average Linear Velocity for details of the calculations An unretained component s at column temperature T elution t
127. tor to program events to happen before or during a run For example a valve could open two minutes into a run Listed in the run table page are settings entered prior to the run in the Run Time Event dialog Time item and settings display in this run table Controls listed in the Initial Values group box are for switching external devices On Off To display this page Click on the Run Table page from the Instrument Setup view Oven UFM Left SSL Left Carrier Right PTV Right Carrier Right TCD Run Table item Setting Add 1 00 Right Detector TCD Autozero Initial values IT Evemal Event 8 Dn TI Extemal Event 5 On IT ExternalEvent 20n TI Extemal Event 6 On IT ExtemalEvent 30n TI Extemal Event 7 On I ExtemalEvent 40n T Extemal Event 8 On Figure 3 19 Run Table Page View Related topics e Setting Up Parameters for Run Table e Using the Add Event Run Time Event Dialog Run Table Parameters Time Item and Settings Displays which Event Time Prep run or Run Time was selected in the Run Time Event dialog Displays which event Detector Valve or External was configured in the TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Setting External Event Thermo Finnigan Run Time Event dialog Displays the Detector Events settings or On Off states for Valve and External Events Click Add to view the Add Event Run Time Event dialog bo
128. tron Capture Detector in degrees Celsius Select a temperature above the final oven temperature and high enough to prevent sample condensation inside the detector The ECD temperature heats separately from the base temperature Typical operating temperatures for the ECD are 300 to 350 C Reference Current The amount of current in nano Amps applied as reference current to the Thermo Finnigan TRACE Gas Chromatograph Setup User s Manual 3 77 Instrument Setup 3 78 Pulse Amplitude Pulse Width Makeup X detector Sometimes referred to as standing current The value entered here is the current for the detector to maintain at a constant level The settings for this current depends on the type of detector used with the ECD Values from 0 3 nano Amps may be entered Changes in this value may effect linearity See the TRACE GC Ultra Operators Manual for more detailed information The voltage applied to the detector Consult your ECD Detector manual for more detailed information Values from 5 V to 50 V may be entered Typically the pulse amplitude is set to 50 V However very clean systems may operate equally as well at 25 V or 15 V This voltage is used to aid in achieving the selected reference current or standing current Detectors exhibiting line out frequencies below 1 2 kHz should be operated at 25 V or 15 V Select from 0 1 0 5 or 1 microseconds to control the pulse going to the detector The use of Nitrogen as make up r
129. ts to minutes Average Linear Velocity The rate at which carrier gas moves through the GC column can also be expressed in terms of its linear velocity Because pressure on the carrier gas changes at each point along the column the gas will expand as it flows through the column and linear velocity will increase from the inlet to the outlet The retention time for a component reflects the average linear velocity which is measured by determining the elution time for an unretained peak l average linear velocity at column temperature T cm sec L tu Eq 2 where L column length cm tm hold up time elution time for an unretained component sec The average linear velocity is related to the outlet velocity by the compression correction factor U uoxj where j compression correction factor compressibility correction factor 3 po pi po 2 pi po As with equation 1 for flow under a given set of experimental conditions the average linear velocity can be calculated from the column dimensions TRACE Gas Chromatograph Setup User s Manual 2 29 TRACE Menu 2 30 x viscosity and pressure D 3r intim po ni po Eq 3 Linear velocity is calculated here at oven temperature to correspond with retention time measurements Temperature does not appear explicitly in equation 3 but the viscosity value is a function of temperature Vacuum Outlet Conditions With most GC detectors pres
130. turn detector gases on and off and specify their flow rates in the text boxes If this option is off then you can only turn the gas flows on amp off Select the AC power frequency 50 Hz or 60 Hz that your GC is plugged into The line frequency control indicates allowable scan rate values Data Channel Definition Group Boxes Channels 1 through 3 are the data source connected to your TRACE GC Ultra Select the detector card position located nearest to the front of the GC as Det A The detector card just behind Det A is Det B and the detector card closest to the rear of the GC is Det C Other data source connections include Oven Actual Oven Power Oven Exhaust Open Chassis Temp and Line Voltage Type a name for the channel s data source displaying the chromatogram during runtime For example if you have an FID installed on the right position of your TRACE GC Ultra type Right FID elect the number of data points to take per second during the acquisition TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan XK TRACE GC Ultra Configuration 1 5 Auxiliary Page These controls allow you to configure and use an auxiliary interface Your selections on this page directly influence the controls you will use on the Aux Zones page located in the Instrument Setup window Whatever configurations you manually enter into your TRACE GC Ultra must exactly match what controls you enter into this Auxiliary configuration dialog
131. ument Setup view Programmed Flow Figure 3 11 Carrier Page View Related topics e Setting Up Parameters for Constant Flow Mode e Setting Up Parameters for Constant Pressure Mode e Setting Up Parameters for Programmed Flow Mode e Setting Up Parameters for Programmed Pressure Mode TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan X Instrument Setup Flow Mode list box The controls you see on this page are dependent on the Flow Mode selection Please select one of the following modes and jump to that topic for detailed information Constant Flow Mode es Constant Pressure Mode e Programmed Flow Mode e Programmed Pressure Mode Four flow modes are available and affect the controls listed in the Ramps group box Constant Flow controls in the Ramp group box display Flow cc min Enter a column flow for the analytical column When using an oven temperature program run the GC to automatically increase the pressure constant flow on the column This compensates a gas s increased viscosity due to an increase in temperature In this mode the inlet pressure is varied during an analytical run as needed to maintain the column flow at a specified setpoint This means that when a column is heated and its restriction to flow increases the inlet pressure is increased Constant Pressure controls in the Ramp group box display Pressure Enter inlet pressure for the analytical run In this mode a specifie
132. vent is closed during the injection to drive most of the sample into the column The solvent effect is required to refocus the analytes especially more volatile compounds You can achieve the solvent effect by keeping the analytical column or guard column slightly below the solvent s boiling point Splitless times of 1 minute are typical Activates controls listed in the Purge group box Constant temperature isothermal activates controls listed in the Surge group box Same as CT Splitless but can also program a surge during an injection Surge starts at Prep Run and continues until the surge duration time is finished Surge is further defined in the Surge Group Box Inlet Group Box Allowable entry ranges are 30 400 C However if you selected the SVE Valve in the Inlet Configuration dialog then you can enter cryogenic temperature values below 0 C in the range 50 to 400 TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup Split Flow checkbox and text box Split Ratio Splitless Time text box Solv Valve Temp Constant Septum Purge checkbox Stop Purge Time text box Surge Pressure text box Thermo Finnigan For non cryogenic use this temperature is usually set for 20 above the evaporation temperature for the sample s components of interest Optimum temperature for an analytical method varies with the method and sample requirements The entry also has a check box for on o
133. x Run items you select from this dialog are added to the time item and setting table Click Edit to edit a selected run item listed in the Time Item and Setting table Select an item listed in the time item and setting table Click Remove to remove the selected run item from the run table Initial Values Group Box Located on the back of your TRACE GC Ultra is a port with eight contacts that switches external devices On Off During a specific run times you can use these controls to set the status of these external switches prior to the run Factory defaults for the beginning of each run is off not checked Setting Up Parameters for Run Table 1 Select a control from the Event Time Group Box When do you want to start the run at Prep Run or at Run Time 2 Select a Detector Event Valve Event or External Event 3 Select the controls available under the evnt type you selected 4 Click Ok TRACE Gas Chromatograph Setup User s Manual 3 95 Instrument Setup Prep Run Run Time Detector 3 96 X Using the Add Event Run Time Event Dialog If you selected Add or Edit from the Run Table Page this dialog box displays x r Event time Prep run Runtime 11 00 min Detectorevent pC Valve event C Extemal event Detector Right TCD D Valve number fi S External number fi z Auto Zero Valve type Sampling Setting Of e Hange j d Inject for fo 00 min C Gain Sett
134. ytical column When the box is not checked calculations are made for a normal GC detector which is usually at atmospheric or slightly higher pressure Check the Gas Saver box to activate gas saver controls Checking the box will activate the other two features of gas saver Gas Saver Flow mL min The desired flow after the injection or in standby Gas saver flow displays the carrier gas in milliseconds and minutes until the end of the run Gas Saver Time minutes The time after the injection when gas saver flow will be activated in the Instrument Setup window Setting Up Parameters for Programmed Flow Mode Use the following procedure to set up parameters for the Programmed Flow option 1 Open the Instrument Setup window 2 Select the Carrier tab TRACE Gas Chromatograph Setup User s Manual Thermo Finnigan Instrument Setup 4 Select Programmed Flow from the Flow Mode spin box Check the Flow box to enable flow to the inlet When this box is not checked gas flow goes to the inlet and through any installed column If the oven is taken to a high temperature the column may be damaged as well as any detectors or components attached to it Type in values for the initial flow and hold time for the analytical column Use the Ramp control to add extra ramps to the program Enter rate flow and hold time values for each additional ramp in the program Check the Vacuum Compensation box to compensate for a

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