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Addendum to PAL User Manual Installation and Operation

1. Adjust the gas flow to approximately 4 mL min 1 mL min This flow of gas will not damage the bed of the trap but the entire system is flushed about three times per minute Standard flush time is two minutes This means that the ITEX 2 device is flushed six times with gas for cleaning purposes The Cycle Composer macro ITEX2_GasFlowCheck can be used to measure the actual gas flow through the trap needle See the section Operation Gas flow adjustment without an installed restrictor can be done as described below This procedure Is necessary in case the ITEX Option is installed if the restriction frit was not provided or If it has been lost or is clogged 1 Release the pressure entirely from the PAL pressure regulator Use a liquid e g n hexane to check whether any bubbles form 2 Turn the pressure on very slowly and check for bubble formation in the liquid again If a good stream of bubbles Is visible measure the gas flow 2 3 3 Flush Gas Type For gas chromatographic technique three different carrier gases are typically used nitrogen helium and hydrogen Nitrogen and helium are inert gases and therefore can be safely used as flush gases for the ITEX technique Because of a slightly lower solubility in water the preferred gas for headspace analysis is helium Whenever possible helium should be used for the ITEX technique If helium is used as a carrier gas the carrier gas line can be divided and teed
2. up for a carrier and a flush gas Activating the flush gas valve should not result in irregularities in the GC detector baseline Safety Warning Hydrogen widely used as a carrier gas for GC capillary techniques Is a flammable explosive gas For safety reasons do not use hydrogen as a flush gas for the ITEX technique 22 PAL is a registered trademark of CTC Analytics AG Switzerland note note note note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 2 4 4 Flush Gas Quality The minimum quality level is grade 55 99 9995 purity Grade 59 99 9999 purity or Grade 60 99 99990 purity are preferable Good laboratory practice is to install a charcoal and a moisture filter to ensure that a high quality of gas is supplied to the GC system For further details on flush gas and contamination see section G Principles If the installation procedure has been carried out in the order described it Is necessary to power up the PAL System at this point Powering up executes a warm start During this procedure the software references the interfaces and the ITEX 2 trap heater is identified at AUX2 3 PAL Firmware and Firmware Object Installation for PAL ITEX 2 Option 3 1 PAL Firmware Installation for PAL ITEX 2 Option The PAL ITEX 2 Option requires PAL Firmware version 2 5 2 or higher for the PAL System and version 4 1 X or higher for the PAL x System Firmware version 3 0 X
3. ChemStation Empower EZChrom MassLynx Xcalibur For details see Point 3 PAL Firmware and Firmware Object Installation for PAL ITEX 2 Option 1 4 PAL ITEX Option compared to PAL ITEX 2 OPTION The PAL ITEX Option as used until now is the name of the first generation module designated for the ITEX technique It was based on a 2 5 mL headspace syringe with a standard syringe cartridge and a trap injection needle combination This earlier version was longer or higher in dimension than the current models The resulting total length required a special PAL Injection Unit PNo MZ 010 00E This earlier setup had certain limitations For example a change over to other injection techniques such as liquid injection or SPME was not possible without changing the PAL Injection unit back to the standard device With the new ITEX 2 Option it is possible to use standard PAL equipment for the ITEX application A special PAL Injection Unit is no longer required Any PAL System installed in the field fulfilling the hardware and software requirements Is compatible with the new ITEX 2 Option The hardware and software requirements are described above in Points 1 2 and 1 3 The first generation ITEX Option parts are not compatible with those of the new ITEX 2 Option All product number details for spare parts are provided in the Appendix PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYST
4. For the user it is easy to monitor the split flow Connect a flow meter to the split outlet line and monitor the split flow during the injection process Such high backpressures may be due for example to a capillary column of 0 25 mm D and length of 60 to 80 meters 39 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option If a split opening is observed either reduce the injection speed from the ITEX 2 device which should be done but without sacrificing the peak shape especially as seen in early eluters or reduce the column backpressure Some GC manufacturers provide special EFC EPC devices with different plumbing from the EFC EPC to the injector which adapts to such special cases and stabilizes the baseline as well For further information contact your GC manufacturer representative 2 5 GC Column Oven No recommendation can be given for column oven temperature This parameter is highly dependent on the application For very highly volatile compounds select a starting temperature of 30 to 35 C This low temperature permits focusing the sample at the column inlet Cryo cooling the oven to this low starting temperature Is advised 2 6 GC Column The type of GC column also depends greatly on the application and detection device for the GC system If a low starting temperature Is used check also the lower temperature limit of the GC column Some colu
5. is selected the Z axis moves to the position FiberExp A needle penetration of 25 mm is executed The needle guide is blocked and the needle is freely exposed for 25 mm If 0 No is selected the next step Is executed The lower needle guide has to be lifted up manually at the moment the needle is inserted into the vial containing the liquid The Injection Unit is moved to position Home The gas flush is executed the plunger is moved Flush Time up to allow a gas flow through the Syringe Trap assembly A timer is started to allow enough time to insert the needle into a vial containing liquid to check the flow of gas or to apply a flow meter to measure the gas flow We recommended a flow rate of 4 1 mL min After stopping the flush gas a timer Is started to Time to Finish Test allow removing equipment from the unit before the needle guide is released After the timer has run back to zero the gas flush mode Is stopped and the needle guide is released again Table 6 Description of the Macro ITEX2_ CheckGasFlow 30 PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 1 6 Macro or Cycle ITEX2_CleanTrap Macro Cycle used to clean or condition the Trap The Trap can be conditioned or cleaned at a selectable temperature and time For the cool down process the choice is open to use a continuous gas
6. 3 3 Ordering Information for Custom Traps 47 4 ITEX 2 Performance Test 47 4 1 Supplier and Order Information for ITEX 2 Test Sample 47 4 2 ITEX 2 Performance Test 48 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option C List of Figures and Tables Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure Figure 21 Figs 22 25 Figure 26 Enrichment Table Table Table Table Table Table Table Table Table Se ee E ae Oe a 9 10 11 12 13 14 Figs 15 18 Figure 19 Figure 20 Se e S 9 Table 10 Table 11 Table 12 PAL ITEX 2 Option PAL ITEX 2 Option Components Connecting the Guide Wire to the X axis End Cover Guide Wire connected to Heated Cartridge ITEX 2 Headspace Syringe Assembly with Trap Needle Grid removed from Syringe Heater Unit Prepared Cartridge with Trap Heater Assembled ITEX 2 Syringe inserted into Syringe Heater ITEX 2 Syringe and Heater Assembly Positioning the Trap Heater onto the Trap Needle Bottom View of Cartridge with angled Trap Fixation Illustrating the Space required in between Adapter and U bolt Fixation Final Assembly of ITEX 2 Syringe Heater and Trap Accessing the Set Screw to replace Syringe or Trap Needle Inserting the ITEX 2 Cartridge into the Z axis Heated Trap connected to AUX2 Interface Replacing the Original Adapter with
7. A Job contains the information needed by the PAL to process multiple samples by the same processing steps The elements of a Job are a Method and a Tray that define the location of the samples to be processed For identification Jobs are automatically numbered from 01 to 99 and then restarting with 01 when they are added to the Job Queue Cycle A Cycle consists of the specific operations necessary to process one sample The Cycle operations are repeated for each sample within a Job Cycles are designed for specific applications Method A Method defines how the samples are processed The elements of a Method are a Cycle a Syringe and a Parameter List Methods have names with up to eight characters and can be edited copied and deleted Method Parameters Method Parameters are associated with the Cycle operations User assigned Parameter values define how a processing operation Is performed A zero Parameter value will disable a Cycle operation Cycle Parameters are application specific Objects Objects are data structures describing the properties of physical modules Certain modules e g a Stack require several objects Tray Holder Holds one or more trays Each Tray Holder has a reference position X Y Z coordinates that defines its location 45 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option Stack A Stack is a particular type of Tray Hol
8. Vial Tray 78 positions 6 x 13 for 7 mm micro vials 1 mL opposite side of 98 positions Tray VT98 Vial Tray 98 positions 7 x 14 for 12 mm vials 2 mL VT200 Vial Tray 200 positions 10 x 20 for 7 mm micro vials 1 mL Table 10 Naming Convention 45 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 3 PAL ITEX Option Spare Parts 3 1 PAL ITEX 2 Option Spare Parts Part No Description SyrC ITEX 2 1 3 ITEX 2 Syringe 1 3 mL with Adapter M7x0 5 ITEX 2 PLG1 3 Replacement Plunger for ITEX 2 Syringe MSH 05 01 ITEX 2 Syringe Heater Unit ITEX 2 HT ITEX 2 Trap Heating Unit ITEX 2 TrapTXTA ITEX 2 Trap Tenax TA 80 100 mesh ITEX 2 TrapTXTA 3 ITEX 2 Trap Tenax TA 80 100 mesh set of 3 pcs Table 11 ITEX 2 Option Spare Parts 3 2 PAL ITEX Option Spare Parts Parts for the first generation ITEX are NOT compatible with the ITEX 2 Option The Trap needle for the ITEX Option has an outer diameter of 2 0 mm at the top and the ITEX 2 trap has an outer diameter of 3 2 Therefore the Trap Heater Unit is not interchangeable The Syringe Heater Unit for ITEX 2 is shorter because the syringe has a volume of 1 3 mL compared to 2 5 mL from the older ITEX Option Use the order information as shown below for the first generation ITEX Option spare parts Part No Description SyrC ITEX2 5 ITEX Syringe 2 5 mL with Adapter 14 28 UNF Fitting PLG G2500 Replace
9. be set low typically 30 to 250 uL s This macro should not be used for the analysis of highly volatile compounds At the moment of thermal desorption there could be partial loss of compounds See the macro description below Macro Description The syringe Agitator and ITEX 2 Trap are heated to the required temperature The vial is transported to the Agitator and equilibrium is established The ITEX 2 Trap Syringe needle is inserted into the vial 18 mm With pumping cycles as defined in the counter Extraction Strokes the plunger is moved up and down to load the analyte sample into the trap The plunger is moved up by the volume as defined by the injection volume in the Sample List The Ready Signal from the GC system for the PAL system is awaited at this stage After receipt of the signal the next step Is executed The needle is removed from the vial and the ITEX 2 device is moved to the GC Injector the inlet is selectable The needle is inserted Fixed needle penetration 36 mm into GC injector The ITEX 2 Trap is heated to the selected desorption temperature The sample volume is injected into the GC system A start signal Injected is sent out to start the GC system The ITEX 2 device is moved back to Home Position The Trap temperature is lowered to 70 2 C The treated sample vial is brought back to its original position in the Tray Holder The Trap cleaning step is
10. folder or corresponding folder for application within an integrated system as described under Section E point 3 3 Installation of Macros for Cycle Composer or Cycles for ICC Interpretation To operate the PAL ITEX 2 Option using Cycle Composer software it Is assumed that the user is familiar with the PAL Cycle Composer control software AN Safety Warning Do not touch the surface of the Trap Heater during operation The surface temperature can reach potentially harmtul levels when operated at high desorbing or cleaning temperatures The Trap surface can reach approximately 270 C if operated at the maximum trap temperature of 350 C lfa new Trap is installed the material has to be conditioned first Use the macro or cycle ITEX2_CleanTrap for the cleaning step and verify if a blank baseline can be reached with the specific GC configuration to be used for the analysis 26 PAL is a registered trademark of CTC Analytics AG Switzerland syste Addendum to PAL System User Manual PAL ITEX 2 Option 1 PAL ITEX 2 Option Cycle Composer Macros or ICC Cycles 1 1 Macro or Cycle ITEX2 Standard Macro Cycle for ITEX 2 application for medium and low volatility compounds At the moment of thermal desorption the plunger is in the uppermost position After reaching the Trap desorption temperature Injection into the GC inlet system follows For medium or low volatile analytes the injection speed can
11. gas stream Possible condensation can be eliminated Table 7 Description of the Macro ITEX2_CleanTrap 51 PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 2 PAL ITEX 2 Cycle Step by Step Step1 The sample vial is placed into the Agitator and the equilibrium Is established time and temperature controlled Figure 22 Step 2 The sample is loaded on the trap by continuously pumping the syringe plunger up and down dynamic headspace Figure 23 32 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual a SYSTEM PAL ITEX 2 Option Step 3 Thermal desorption of analyte directly into the GC inlet system Figure 24 Step 4 The Trap material is cleaned with inert gas Trap Cleaning Time Flush Time The Trap temperature can be raised for the cleaning step Figure 25 Figures 22 to 25 Step by Step Illustration of an ITEX 2 Cycle 55 PAL is a registered trademark of CTC Analytics AG Switzerland note note p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 3 Quantification of ITEX Technique The quantification of results obtained from the ITEX technique is based on the same principles as for static headspace or any other sample enrichment technique such as SPME for example In the case where analyte s is are combined with matrix it is
12. important to be able to have the calibration standard in the same matrix environment Since the ITEX technique could be considered a dynamic headspace technique the lack of identical or missing matrix could be compensated for by performing an exhaustive extraction Be aware that such a compromise must be validated very carefully 4 Available Trap Material The standard trap material shipped with a PAL ITEX 2 Option Is Trap material Tenax TA Mesh size 80 100 Fill volume 44 mg Bed length Approx 36 mm Positioning inserts Silanized glass wool Upper temperature limit 350 C Trap Needle material stainless steel inside wall neutral deactivated for analysis of e g organo sulfur compounds See also Appendices Section 3 PAL ITEX Option Spare Parts point 3 3 Ordering Information for Custom Traps 5 Cleaning the Trap Safety Warning Do not touch the surface of the Trap Heater during operation The surface temperature can reach potentially harmtul levels when operated at high desorbing or cleaning temperatures The Trap surface can reach approx 270 C if operated at the maximum trap temperature of 350 C It is advisable to clean a trap initially to eliminate all volatile contaminants Use the provided Cycle Composer macro ITEX2_CleanTrap A practical check is to run a blank injection monitor the detector baseline to check for sufficient cleanness of the trap Observe the maximum operating t
13. installed and set up properly before following the PAL ITEX 2 Option operating instructions PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option E PAL ITEX 2 Option Installation 1 General System Overview Figure 1 PAL ITEX 2 Option The PAL ITEX 2 Option is an add on module for the PAL and PAL xt Systems to extend the range of headspace techniques ITEX can be considered an automated dynamic headspace technique In classical headspace technique one sampling is done per vial In this device analytes are adsorbed loaded on a sorbent trap contained within a side hole needle attached to a gas tight syringe Following this loading procedure analytes are thermally desorbed and led directly into the GC injection port then analyzed by the required technique mainly using GC MS detection Loading takes place by continuously moving the headspace syringe plunger up and down passing the headspace gas phase that exists above a sample through the sorbent trap inside the needle numerous times Dynamic headspace extraction increases the concentration of analyte in order to extend the range of detection as compared to conventional static headspace techniques Required levels of detection can be reached by applying more pumping up and down cycles To reach the detection limit in the range of a ppm to ppb concentration three to twenty strokes are typically applie
14. is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual PAL ITEX 2 Option Figure 10 Positioning the Trap Heater onto the Trap Needle Please note that the U bolt fixation has to be installed with an angle as shown in Figure 11 viewed from the bottom of the cartridge Figure 11 Bottom View of Cartridge with angled Trap Fixation The explanation for this specific angled position Is illustrated in Figure 12 The adapter size for the long tension cord at the Z axis syringe slider prevents a square fixation of the U bolt on the Trap Heater PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option Figure 12 Illustrating the Space required in between the Adapter and the U bolt fixation 5 Attach the plunger holder to the syringe plunger The final assembly of the ITEX 2 headspace syringe inserted in the syringe heater and trap heater is shown in Figure 13 Figure 13 Final Assembly of ITEX 2 Syringe Heater and Trap PAL is a registered trademark of CTC Analytics AG Switzerland note p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option If a syringe or a Trap Needle has to be replaced and is inside the grid use the hole provided to access the set screw with a screw driver from the front without removing the grid Be aware that the grid itself can be hot at the surface Be careful w
15. the Flow restricted ITEX 2 Adapter at the Pressure Regulator PAL Object Manager loading ITEX 2 Firmware Objects Step by Step Illustration of an ITEX 2 Cycle Test Chromatogram Static for Headspace and ITEX 2 Commonly used Safety Symbols Description Macro ITEX2 Description Macro ITEX2 Volatile Description Macro ITEX2_ TestHS Description Macro ITEX2_ TestlTEX Description Macro ITEX2_CheckGasFlow Description Macro ITEX2_ CleanTrap Trap Heating up Rate and Cooling off Times PAL Injection Parameters for Performance Test Naming Convention ITEX 2 Option Spare Parts ITEX Option Spare Parts PAL is a registered trademark of CTC Analytics AG Switzerland note note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option D How to Use this Manual This manual covers the COMBI PAL and the PAL COMBI xt systems Issues specitic to the PAL COMBI xt model have been emphasized accordingly The major sections of this Addendum are Safety Information PAL ITEX 2 Option Installation PAL ITEX 2 Option Operation Explanations and Description of the ITEX Technique Appendices This Addendum is intended for frequent PAL users or new users who are experienced at using automated systems to perform analytical methods The Appendices provide information on PAL ITEX 2 options and spare parts A performance test to demonstrate the enrichment of the analyte Is described The COMBI PAL must be
16. 350 C Other trap material is available see section Appendix Spare Parts e Gas Flow 4mL min 1 mL min Restrictor for pressure regulator outlet is provided Net Weight Approx 210 g total weight including trap heating cable Dimension Height 160 mm Width 78 mm total width including side adapter of cartridge PAL Firmware PAL System Version 2 5 2 or higher PAL x System Version 4 1 X or higher Software Control Using Cycle Composer Software Version 1 6 0 current version 1 6 0 any lower version Is suitable as long as serial communication Is selected or PAL ICC Cycle Editor PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 1 2 Hardware Requirements The PAL ITEX 2 option can be used with any PAL System equipped for static headspace technique e g the COMBI PAL or PAL COMBI xt Systems The revision level of the PAL Injection Unit must be Rev E or higher a slot at the left side is required Example PNo MZ 02 00 Revision E 1 3 Software Requirements The PAL ITEX 2 Option requires PAL Firmware 2 5 2 or higher for the PAL System and firmware version 4 1 X or higher for the PAL xt System It can be controlled using PAL control software the Cycle Composer or any CDS chromatography data system software that controls the PAL System including those using the Cycle Editor for PAL ICC interpretation e g Analyst
17. AL conditions as described in section F point 7 Performing ITEX 2 Test GC Column ZB 5MS 30 m x 0 25 mm Film thickness 0 25 um Flow Rate 1 5 mL min Constant Flow Helium GC MS Detection Mass Range 50 250 m z Full Scan Scan Time 0 200 s Acknowledgment Data provided by Brechbiihler AG 8952 Schlieren ZH Switzerland Operator UH TF 48 PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option This page intentionally left blank s PAL is a registered trademark of CTC Analytics AG Switzerland
18. Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option Addendum to PAL User Manual PAL ITEX 2 Option ITEX In Tube Extraction Installation and Operation Printing History Edition 1 April 2009 Edition 2 October 2009 Edition3 July 2010 Original Instructions CTC Analytics AG reserves the right to make improvements and or changes to the product s described in this Addendum at any time without prior notice CTC Analytics AG makes no warranty of any kind with regards to this product including but not limited to implied warranties of merchantability and suitability for a particular purpose Under no circumstances shall CTC Analytics AG be held liable for any coincidental damage or damages arising as a consequence of or from the use of this document 2010 CTC Analytics AG All rights reserved Neither this publication nor any part hereof may be copied photocopied reproduced translated or reduced to electronic medium or machine readable form without the prior written permission of CTC Analytics AG except as permitted under copyright laws CTC Analytics AG acknowledges all trade names and trademarks used as the property of their respective owners EPO patent granted Patent number EPO 1697736 PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option A Safety Information Declaration of Conformity See the Declaration of Conform
19. EM PAL ITEX 2 Option 2 Installation 2 1 Unpacking the Components The PAL ITEX 2 Option is shipped in one box Check for the following items some parts are preassembled 1 1 pc Headspace Syringe Heater ID 25 for syringe with 1 3 mL volume 2 1 pc Plunger Holder 3 1 pc Fixation Clamp for Syringe Heater 4 2 pcs ITEX 2 Trap standard packing Tenax TA 80 100 mesh 5 1 pc ITEX 2 Syringe 1 3 mL complete including Plunger 6 1 pc Replacement Plunger for ITEX 2 Syringe 7 1 pc ITEX 2 Trap Heater 8 1 pc End Cover left side 9 1 pc Flow Restrictor for Pressure Regulator 10 1 pc CD ROM containing e Object Manager ITEX 2 Lists e Cycle Composer macros and ICC cycles Figure 2 PAL ITEX 2 Option Components PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 2 2 Installing the PAL ITEX 2 Option Turn off the power to the PAL System before beginning the installation process 1 Replace the X axis end cover on the left side of the unit with the cover provided which permits fixing the guide wire of the electrical cable Connect the guide wire as shown in detail in Figure 3 below Figure 3 Connecting the Guide Wire to the X axis End Cover PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 2 The hea
20. ady Time the time for the next sample to be placed in the Agitator and to establish equilibrium is calculated This optimization of cycle time is useful in case of a longer sample preparation time compared to the GC run time Remark This step is required to avoid possible contamination of the trap syringe system in case a substance is only partially desorbed Pulling up the plunger at the desorption temperature for gas flush cleaning could bring the substance into the syringe part of the device Trap Cleaning Temperature Trap Cleaning Time Flush Time Remark Cleaning Temperature can be higher than Desorption Temperature Observe the maximum operating temperature for the trap material Trap Starting Temperature GC Ready Time Remark Time from GC start to GC ready Table 3 Description of the Macro ITEX2_ Volatile 1 3 Macro or Cycle ITEX2_ TestHS Macro Cycle used to run ITEX 2 test procedure One plunger stroke to simulate static headspace without a concentration step Macro Description This macro ts identical with the macro ITEX2 The exception is the fixed counter step Extraction Strokes see below The counter Extraction Strokes is replaced by a fixed one fill stroke to simulate static headspace technique Waiting for a timer tolerance is not necessary at the end of the cycle for a single test Macro Variable Remark Unused variables for this simplified
21. ation time Is longer than 60 minutes and a very sensitive detection device is used such as GC MSD All three listed parameters are necessary to be able to detect a possible contaminant The design of the ITEX 2 syringe and needle fixation are different trom the standard headspace syringe therefore the points described above do not apply to the ITEX syringe See also point 3 4 below With the high enrichment factor achieved by using the ITEX technique there is a higher risk that contamination can occur Experimentally all components of the PAL internal gas supply have been tested namely the pressure regulator gas flush valve gas flush tube and all connections including the gas distribution block mounted at the end cover of the X axis In case a contaminant is detected in the chromatographic and or mass range detection it is advisable to install a filter between the gas inlet and the injection unit and after the built in gas flush valve 4 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 3 4 ITEX 2 Syringe and ITEX 2 Trap Contamination of the ITEX syringe has not yet been observed The needle connection is different from that used with the static headspace syringe Contamination due to glue out gassing is eliminated by design Contamination of the trap can occur during the application or due to insufficient cleaning However if certain rules are obse
22. d and for the ppt level of concentration 40 to 60 pumping strokes may be necessary The PAL ITEX 2 Option consists of a dedicated gas tight syringe with an adapter for a replaceable side hole needle and a heated syringe cartridge The side hole needle includes an integrated trap standard trap material is Tenax TA and a trap desorber heater PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 1 1 Specifications Part number PAL ITEX 2 Option Description PAL ITEX 2 Option for COMBI PAL Headspace Syringe PNo SyrC ITEX 2 1 3 Volume 1 3 mL Syringe Heater PNo MSH 05 01 Syringe ID 25 Temperature range 30 150 C Trap Heater PNo ITEX 2 Trap Heater Temperature range 30 350 C Heating up rate 30 to 250 C 25 30 seconds Cooling off time 250 to 70 C approx 3 minutes Cooling off time 250 to 40 C approx 5 minutes Cooling off time 250 to 30 C approx 7 minutes requires AUX interface connection standard is AUX2 note Nominal volume 1 3 ml Syringe Maximum Scale Length 27 mm 1 125 mL actual syringe volume ITEX 2 Trap e Material Stainless steel deactivated by SilTek e Needle Injection needle gauge 23 O D 0 63 mm Point style 5 side hole Injection needle length 41 mm e Trap Upper part of needle 3 20 mm O D Standard trap material Tenax TA 80 100 mesh fill volume 44 mg Upper temperature limit
23. der that is designed to hold micro plates A six drawer Stack holds 12 standard micro plates two in each drawer A three drawer Stack holds six deep well micro plates two in each drawer Tray A Tray holds multiple samples Trays are defined by designating the Tray Type see below and the Tray Holder Tray names are used to identify the sample source within a PAL Job Tray Type A Tray Type defines the pattern and sampling sequence of sample locations within a Tray PAL Object Manager Software to load a PAL Object List to an instrument if a Module hardware module has been added to the PAL System In a special mode Object Manager can also be used to create and maintain Object Lists PAL Object List If a PAL Module hardware is added to an instrument several Objects have to be loaded in the firmware These Objects are collected in an Object List and stored in a file with the extension pol Object Lists are delivered together with Object Manager Software and are grouped into folders for the different kind of Modules e g Syringes Tray Holders Valve Drives The name of an Object List starts with the Module part number with variants added e g first or second Stack The name of the root folder includes the revision which is dependent on the firmware version e g Object Lists Rev L for firmware 2 X and 3 X or PAL xf Object Lists Rev B Object Class Each Object belongs to an Object class e g Syringes Tra
24. emperature for the trap material 54 PAL is a registered trademark of CTC Analytics AG Switzerland gt AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 6 Trap Heating up Rate and Cooling off Time In the second generation of the ITEX apparatus improvements have been made to the heating up rate The cool off time however became slightly longer Parameter ITEX 2 Option ITEX Option Heating up rate 30 to 250 C 25 to 305 approx 30 s Cooling off time passive 250 to 70 C approx 170s approx 120 s 250 to 35 C approx 360 s approx 300 s Table 8 Trap Heating up and Cooling off Times 7 Performing ITEX 2 Test This section describes a short test procedure to demonstrate the enrichment of the analyte in the trap as compared to that obtained using static headspace technique 7 1 ITEX 2 Test Sample The ITEX 2 Test sample is composed of e 1 2 Dichlorobenzene CAS 95 50 1 e 1 3 Dichlorobenzene CAS 541 73 1 e 1 4 Dichlorobenzene CAS 10646 7 The concentration is 100 pg mL each dissolved in Methanol solvent P amp T quality The test sample is available from Restek Chromatography Products order number RT 564309 For details see Appendix 4 These compounds were selected because they exhibit good response with many GC detectors including the flame ionization detector FID the electron capture detector ECD and the mass selective detector MSD Furthermore separation of the three is
25. executed with the Flush command At the same time the temperature for the Trap is raised to the selected cleaning temperature Table 2 continues Macro Variable Syringe Temperature Trap Starting Temperature Incubation Temperature Desorption Temperature Incubation Time Agitator Speed Extraction Strokes Extraction Volume Extraction Speed Pullup Delay SL Volume Pullup Delay Remark to SL Volume This is not a Macro Variable Inject to INJECTOR Desorption Temperature Desorption Speed injection speed Remark Post Injection delay is fixed to 20 seconds Remark This step is required to avoid possible contamination of the trap syringe system in case a substance was only partially desorbed Pulling up the plunger at the desorption temperature for gas flush cleaning could bring the substance into the syringe part of the device Trap Cleaning Temperature Trap Cleaning Time Flush Time Remark Cleaning Temperature can be higher than Desorption Temperature Observe the maximum operating temperature for the trap material 27 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual PAL ITEX 2 Option system After stopping the gas flow the Trap temperature is lowered to the starting conditions for the next run Trap Starting Temperature With the variable GC Ready Time the time is calculated for the next sample to be p
26. flush to protect the trap material or if the Trap should be cooled in a passive way not to have gas protection Macro Description Macro Variable From the Home position the gas flush mode is activated Temperature and Time for Trap cleaning or Trap Cleaning Temperature conditioning are selectable Trap Cleaning Time After reaching the time limit for cleaning the Cool_ Off Temperature Desorber heater is set to Cool_ Off Temperature This temperature can be a higher temperature Note Temperature Accuracy 0 Temperature than ambient set such that the trap material can s not checked within a range next step Is be cooled off to a level where gas protection can executed immediately be turned off The user has the choice to cool off the trap inan Cool_Off with Flush YES_1 NO_0 active or passive manner by selecting or not selecting the flush mode again We recommend activating the flush mode again to speed up the cooling process and protect the trap material with an inert gas stream If 1 YES has been selected the flush mode is Cool_ Off Temperature activated again Gas flow is provided until Cool_ Off Temperature is reached within 5 C If 2 NO is selected the Trap material will cool off passively The variable Cool_ Off Time is obsolete A second temperature setting allows cool down Standby Temperature Accuracy 2 C to ambient or near to ambient without a
27. he PAL Object Manager This software is usually installed in the following path C Program Files PAL Object Manager Object Lists Start PAL Object Manager software The ITEX 2 Option folder should be visible in the structure shown in the window Choose Object List Folder on the left side of the Object Manager program window Select ITEX 2 Option on the left side Select PAL ITEX2Opt on the right side and click Send selected Object Lists to PAL The example shown in Figure 21 is the PAL System Object Lists t PAL Object Manage C Program Files PAL O bject er O0bject Lists Rev JNITEX 2 Choose Object List Folder Object Lists GC Injectors a PAL ITEX20 pt Incubators L ITEX Option LHS Upgrade Maldi Option Firmware 3 x x L Multi Position Valve Drives Firmware 2 O Output Expansion Box Firmware 2 4 0 Solvent Reservoirs SPME Fiber Conditioning Stations d SPME Upgrade Stack Coolers d Stacks Syringes di 0 Send selected Object Lists to Pal Figure 21 PAL Object Manager loading ITEX 2 Firmware Objects The following PAL Firmware Objects are loaded e Class Syringe 1 3ml IT 1 3 mL ITEX 2 Syringe e Class Injectors Desorb2 Heater H2Desorb assigned e Class Heaters H2Desorb temperature range 30 to 350 C HSyr Heater for ITEX 1 3 mL Syringe temperature range 30 to 150 C e Class Motors Drives MPIgHS Plunger Motor drive for Headspace syringe e C
28. hen touching any parts around the ITEX2 Headspace Syringe Heater Safety Warning Do not touch the surface of the Trap Heater during operation The surface temperature can reach a potentially harmtul level when operated at high desorbing or cleaning temperatures The Trap surface can reach approximately 270 C if operated at the maximum trap temperature of 350 C Figure 14 Accessing the Set Screw to replace a Syringe or Trap Needle PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 2 3 Inserting the PAL ITEX 2 Syringe Assembly into the Injection Unit 1 Move the PAL Injection Unit manually to the side to allow free movement of the syringe slider Lower the syringe slider as shown in Figure 11 in order to gain access to install the syringe heater assembly Lift the lower needle guide sliding it into the upper needle guide Insert the syringe needle tip and match the magnetic pins of the syringe holder with their corresponding positions on the syringe slider Let the lower needle guide return slowly and make sure the needle tip does not catch on the guide See Figures 15 and 16 Figure 15 Figure 16 2 Press the heated cartridge firmly against the Z axis slider to ensure that the Syringe heater Unit engages Move the plunger up plunger holder until the thread of the screw catches the
29. is not compatible for the ITEX 2 technique The ITEX 2 Option can be controlled either by a Cycle Composer macro or by any CDS chromatography data system software that controls the PAL or PAL xt System using for example Cycle Composer macros or PAL ICC cycles e g Analyst ChemStation Empower EZChrom MassLynx Xcalibur The PAL xt System requires PAL Firmware 4 1 X or higher the PAL xt Object List Revision B or higher the control board APR Control xt 3 2 PAL Firmware Object List for PAL ITEX 2 Option A CD ROM Is provided together with the PAL ITEX 2 Option which contains the required PAL Firmware Objects to enable the use of the technique Required PAL Object Manager Object Lists e PAL System PAL Object List Revision J or higher e PAL xfsystem PAL xfObject List Revision B or higher In case an upgrade is made from ITEX to ITEX 2 it is advisable to first delete the PAL Firmware Objects of the previous version ITEX Option from the firmware This applies mainly to the object in the class Injector Desorber The objects in the class Out Signal CarGas and SpitPurg can be deleted as well see below 25 PAL is a registered trademark of CTC Analytics AG Switzerland note p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option If an earlier version of the Object Manager Lists are used copy the ITEX 2 Option folder to the Object Lists folder which has been installed with t
30. ition FiberExp PAL Firmware class Vials must be defined first The lower needle guide of the Z axis has to be positioned on the lid of the Agitator such that one screw of the lower needle guide sits at the edge the red magnetic ring does not touch the Agitator and the needle can move freely test by manually lifting up the lower needle guide Adjust the X Y and Z positions accordingly The same concept of blocking the needle guide is used for the SPME technique as well For details on Flush Gas see the Installation section point 2 3 At the moment when gas is flowing through the ITEX syringe trap assembly a flow meter can be connected to measure the gas flow A simple test to check if gas is flowing Is to fill a vial with solvent and insert the needle into the liquid A steady stream of gas bubbles should be observed The selected solvent should be an organic solvent with a lower boiling point such as n hexane Gas bubbles do not form readily in water Insert the needle trap tip into the vial only after the gas flush has been started Avoid sucking liquid into the trap device Macro Description Macro Variable This macro provides the option to block the NdlGuide Blocking YES_1 NO_O needle guide of the Z axis for better and more convenient access to the trap needle at the moment of flow measurement With a counter a decision is made to enable needle guide blocking or to leave this step out If 1 Yes
31. ity sheet enclosed with the instrument General Considerations Any changes or modifications to this unit not expressly approved by the party responsible for compliance could nullify the user s authority to operate the equipment The user should be aware that if the equipment Is used in a manner not specified by the manufacturer the protective and safety features of the equipment may be impaired Electrical Hazard Every analytical instrument features specific hazards Be sure to read and comply with the precautions as described in the corresponding PAL User Manual Use only fuses of the type and current rating specified Do not use repaired fuses and do not short circuit the fuse holder Other Hazards To avoid injury during PAL System operation keep hands away from the syringe Safety Warning Do not touch the surface of the Trap Heater during operation The surface temperature can reach a potentially harmful level when operated at a high desorbing or cleaning temperatures The Trap surface can reach approximately 270 C if operated at the maximum trap temperature of 350 C For detailed Safety Information see the additional warnings in the corresponding PAL User Manual PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option Commonly used Safety Symbols A Caution Risk of Needle Stick Puncture ea me Fuse Electrical Power ON Fisch PAL P
32. jector The trap heater is started to achieve the selected Desorption Temperature At the same time the plunger is moved up slowly to reach the total volume injection volume as defined in the Sample List The sample volume is injected into the GC system A start signal Injected is sent out to start the GC system The ITEX 2 device is moved back to Home Position Table 3 continues Macro Variable Syringe Temperature Trap Starting Temperature Incubation Temperature Desorption Temperature Incubation Time Agitator Speed Extraction Strokes Extraction Volume Extraction Speed Pullup Delay SL Volume 0 5 Pullup Delay Remark to SL Volume This is not a macro variable Inject to INJECTOR Desorption Temperature SL Volume 0 5 Desorption Speed injection speed Remark Post Injection delay is fixed to 20 seconds 28 PAL is a registered trademark of CTC Analytics AG Switzerland system Addendum to PAL System User Manual PAL ITEX 2 Option The Trap temperature is lowered to 70 2 C The treated sample vial is brought back to its original position in the Tray Holder The Trap cleaning step is executed with the Flush command At the same time the temperature for the Trap is raised to the selected cleaning temperature After stopping the gas flow the Trap temperature is lowered to the starting conditions for the next run With the variable GC Re
33. laced into the Agitator and to establish equilibrium This optimization of cycle time is useful in case of a longer sample preparation time compared to the GC run time GC Ready Time Remark Time from GC start to GC ready Table 2 Description of the Macro ITEX2 1 2 Macro or Cycle ITEX2_ Volatile Macro Cycle used for very volatile compounds Examples Vinyl chloride dichloroethane etc The difference between this and the standard macro Is that at the moment of thermal desorption the plunger moves up slowly to keep volatile compounds in the system not permitting them to diffuse from the trap to the GC inlet port Macro Description The syringe Agitator and ITEX 2 Trap are heated to the required temperature The vial is transported to the Agitator and equilibrium is established The ITEX 2 Trap Syringe needle is inserted 18 mm into the vial With pumping cycles as defined in the counter Extraction Strokes the plunger is moved up and down to load the analyte sample into the trap The plunger is moved up by 50 of the volume defined as the injection volume in the Sample List The Ready Signal from the GC system for the PAL system is awaited at this stage After receipt the next step is executed The needle is removed from the vial and the ITEX 2 device is moved to the GC Injector the inlet is selectable The needle is inserted Fixed Needle penetration of 36 mm into GC in
34. lass Vial Fiber Exp position for Blocking Needle Guide PAL Firmware Objects of the classes Out Signals CarGas and SpitPurg have been included with the first generation the PAL ITEX Option During the developmental phase of the ITEX technique it became evident that these options were no longer necessary for the technique 24 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 3 3 Installation of Macros for Cycle Composer or Cycles for PAL ICC interpretation Every PAL ITEX 2 Option is shipped with a CD ROM containing the various macros or cycles as described below Copy these files to the corresponding folder as described below 3 3 1 Installation of Macros for Cycle Composer Navigate in Explorer to the Cycle Composer folder This is usually installed in the following path C Program Files PAL Cycle Composer If you wish to create a separate Method Folder for ITEX 2 copy the folder ITEX 2 from the CD to the Cycle Composer folder In the Cycle Composer use menu File Options Choose Method Folder select the ITEX 2 folder as the Method Folder If you wish to add the ITEX 2 macros to an existing method folder just copy the macro pma and method pme files from the ITEX 2 folder on the CD to the appropriate method folder Use the provided test methods to run a short test to verify the operation
35. macro are eliminated The remaining variables are identical as used for ITEX2 Remark Extraction Strokes 1 Counter is not available Variable GC Ready Time is eliminated Table 4 Description of the Macro ITEX2_ TestHS 1 4 Macro or Cycle ITEX2_TestITEX Macro Cycle used to run ITEX 2 test procedure Ten plunger cycles up and down plunger movements to demonstrate the concentration factor for the trap Macro Description This macro is identical with the macro ITEX2 The exception is the fixed counter step Extraction Strokes see below The counter Extraction Strokes is replaced by a fixed number of ten pumping cycles Waiting for a timer tolerance is not necessary at the end of the cycle for a single test Macro Variable Macro variables are identical with variables from Macro ITEX2 Extraction Strokes 10 Variable eliminated Fixed number Variable GC Ready Time is eliminated Table 5 Description of the Macro ITEX2_ TestITEX 29 PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 1 5 Macro or Cycle ITEX2_ CheckGasFlow Macro Cycle used to check and adjust gas flow through the Trap This Macro Cycle provides the option of blocking the needle guide for the sake of convenience at the moment of gas flow measurement If this option is used the pos
36. ment Plunger for ITEX Syringe 2 5 mL MSH 02 00 Syringe Heater Unit for 2 5 mL HS Syringe ITEX HT ITEX Trap Heating Unit ITEX Trap TXTA ITEX Trap Tenax TA 80 100 mesh ITEX Trap TXTA 3 ITEX Trap Tenax TA 80 100 mesh set of 3 pcs Table 12 ITEX Option Spare Parts 46 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 3 3 Ordering Information for Custom Traps Tenax TA is the standard material for the ITEX 2 Trap Other materials can be custom filled into the ITEX 2 trap or ITEX Trap An exact description of the material including mesh size and expected fill volume must be provided If a two layer bed is required for the trap the order of the layers must be specified After receiving the ordering information BGB Analytik AG will verify feasibility and if in doubt will contact the customer Minimum order quantity is three traps of the same kind Custom traps are handled and provided solely through BGB Analytik AG Rohrmattstrasse 4 4461 Boeckten Switzerland Phone No 41 0 61 991 0046 Fax No 41 0 61 991 0025 E mail Sales bgb analytik com Web www beb analytik com 4 ITEX 2 Performance Test 4 1 Supplier and Order Information for ITEX 2 Test Sample The test or calibration standard for ITEX 2 as described in section F point 7 Performing ITEX 2 Test can be ordered directly at 3 4 1 Supplier Restek Chromatograph
37. min helium or approximately 5 mL min nitrogen at a pressure setting of 0 5 bar at room temperature See Figure 20 E m ma N Gas Inlet Figure 20 Replacing the Original Adapter with the Flow restricted ITEX 2 Adapter at the Pressure Regulator The original adapter removed from the pressure regulator must be stored for future use If the PAL system Is to be used for static headspace technique the flow setting of approx 4 mL min may be too low to flush the standard headspace syringe A maximum flush volume of two or three fold per minute Is the lower limit For MHE Multiple Headspace Extraction technique the required pressure of 1 0 to 1 5 bars cannot be reached with the ITEX 2 flow restricted adapter installed For static headspace and MHE techniques it Is recommended that the original adapter without any flow restriction be re installed 21 PAL is a registered trademark of CTC Analytics AG Switzerland note note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 2 4 2 Gas Flow Adjustment If your system was previously used for static headspace techniques you must adjust the gas flow to ITEX technique requirements If the original adapter for Headspace without flow restriction is in place it is likely that the pressure setting of 0 5 bar needs to be lowered
38. mn phases cannot be used at such low temperatures For highly volatile compounds focusing at the column entrance is important Use a greater film thickness to permit better trapping A greater film thickness normally causes greater bleeding which will affect the baseline and detector stability Compromise on film thickness with the temperature range used for the column and the detection type MSD is critical to bleeding 2 7 Injection Speed The injection speed depends to the volatility of the analyte Very highly volatile compounds can be injected thermally desorbed at a speed of approximately 100 uL s Less volatile compounds can be injected at a speed of 20 to 100 uL s Finding the right injection speed for a specific application is based mainly on judging the peak shape Is any distortion or even peak splitting visible 3 Contamination of the Analytical Device It is Important to realize that the ITEX Technique is a very efficient sample enrichment technique As described detection levels in the ppt range can be achieved However each step in the handling and device setup must be considered with care with respect to any possible contamination Contamination of the analytical device originates from several sources as described below 40 PAL is a registered trademark of CTC Analytics AG Switzerland gt AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 3 1 Gas Quality If the gas quality is rather poor im
39. mperature As a standard starting condition injection into a hot injector is recommended typically 200 C isothermal Check the peak shape and reproducibility and vary the parameters If necessary to improve the results For extremely volatile compounds such as vinyl chloride or 1 2 dichlorethane different experiments have been done such as starting with a cool injector and ramping the temperature up quickly Another approach has been to cryofocus the sample before the actual transfer to the GC column This provides some ideas on how to adapt if problems arise with a specific application The final method selected depends mainly on the available GC equipment and application 2 4 GC Injector EFC EPC One important point to be aware of is the combination of high column backpressure and electronic flow or pressure carrier gas control If column backpressure is relatively high for example 2 bars or approx 25 to 30 psi and a gas plug from the ITEX 2 device is brought into the injector the injector pressure will rise and will possibly reach the EFC EPC limit to control the flow pressure efficiently and accurately Reaching a critical pressure limit for the electronic control causes the GC control to open the split until the pressure returns to a normal level This opening of the split is not very obvious to the user the peak shape Is still good but reproducibility can be very bad relative standard deviations of 20 to 40 have been observed
40. of the instrument 3 3 2 Installation of ICC Cycles Navigate in Explorer to the Cycle Editor folder and or the corresponding folder of the application within an integrated system If you wish to add the ITEX 2 cycles to an existing method folder just copy the cycles cyx files from the ITEX 2 folder on the CD to the application folder 4 Adjusting Object Reference Positions The PAL ITEX 2 Option does not require a special reference position The needle tip should be at exactly the same position as If a liquid or headspace syringe were being used However it is good practice to check the individual positions by using the PAL Utilities functions as described in the COMBI PAL User Manual 25 PAL is a registered trademark of CTC Analytics AG Switzerland note note note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option F PAL ITEX 2 Option Operation The PAL ITEX 2 Option can only be used together with the PAL Cycle Composer control software or with the Cycle Editor assuming the intent is to achieve ICC interpretation using another data handling software system Verify that your system meets the bas c hardware and software requirements before operating the ITEX 2 Option See points 1 2 Hardware Requirements and 1 3 Software Requirements The PAL ITEX 2 Option is shipped with a CD ROM containing various cycles macros for the ITEX application Copy these macros to your Cycle Composer method
41. omers Is possible with all common GC column phases in the range of non polar to polar phases An equal response with all three isomers is expected The test consists of two experiments e first running one sample simulating static headspace one sampling stroke only e second using the enrichment technique by applying 10 pumping cycles plunger up and down movements 55 PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 7 2 Preparation of Test Standard Solution The test or calibration standard solution as received concentration 100 ug mL of each compound is diluted 1 10 with methanol This secondary standard solution is used for the tests as described below Ensure that the methanol used for the dilution step is of high purity 7 2 1 Selective GC Detector e g MSD and ECD Add 1 uL of the secondary standard solution directly into a 20 mL Headspace vial and seal the vial immediately Use a microcap device or a GC syringe to dose the aliquot of the standard solution e Secondary standard solution Concentration 10 ug mL e 1 ul aliquot 10 ng uL 7 2 2 GC Detector FID TCD or any other Non selective Device Add 10 uL of the secondary standard solution directly into a 20 mL Headspace vial and seal the vial immediately Use a microcap device or a GC syringe to dose the aliquot of the standard solution e Secondary standard solution C
42. on Speed 100 uL sec Injection Volume 1 500 uL 1 Injection Volume ts specified in Sample List Table 9 PAL Injection Parameters used for the Performance Test An example of the test Is given in Appendix 4 ITEX 2 Performance Test For the syringe temperature setting a compromise has to be made One has to avoid condensation in the syringe but if the temperature Is too high the hot gas stream could have a desorption effect when pressed through the bed of the trap during the plunger down movement As higher the Incubation Temperature is selected as higher is the pressure in the vial if a solvent e g water is part of the matrix The ITEX 2 performance test can be done with settings such as Syringe Temperature 65 C and Incubation Temperature 60 C These lower temperature settings are always a good starting point 57 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option G Principles of ITEX 2 Enrichment 1 Introduction As described above ITEX is a powerful sample enrichment technique to be used in conjunction with gas chromatographic separation and detection As designed the ITEX sample preparation device lends itself only to sampling from the headspace phase Sampling from a water phase will coat or possibly even saturate the trap material with a liquid film By the process of thermal desorption this liquid would be brought onto
43. oncentration 10 ug mL e 10 ul aliquot 100 ng uL If the calibration standard Is used only for the less sensitive GC Detectors such as FID or TCD then the primary standard with a concentration of 100 ug mL can be used directly Add a 1 uL aliquot of the primary standard solution into a 20 mL headspace vial 7 3 Instrument Preparation for the ITEX Test 7 3 1 Cycle Composer Macros or ICC Cycles The Cycle Composer macros or ICC cycles used for the ITEX 2 tests are e Static Headspace ITEX2_ TestHS e TEX enrichment ITEX2_ TestlTEX 7 3 2 GC Method Parameters e GC column nearly any capillary column can be used to separate the compounds in the test sample e GC Injector temperature 200 to 250 C split less for 1 min e Detector settings depend on the detector used e GC oven temperature 40 C hold 1 minute 10 C min up to 150 C hold 2 minutes 56 PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 7 3 3 PAL Injection Parameters Parameter Value Parameter Value Syringe Temperature 80 C Pullup Delay 55 Trap Starting 75 OC Desorption 950 C Temperature Temperature Jee sti 80 C Inject to GC In Temperature Incubation Time 5 00 min Desorption Speed 100 uL sec Trap Cleaning Agitator Speed 500 rpm TEPENE 250 C Extraction Volume 1000 uL Trap Cleaning Time 2 00 min Extraction Strokes 10 GC Ready Time 10 00 min Extracti
44. owersupply Fisch PAL Poner Supply Used with Main PAL Power Supply Used with Optional Device s oimatoaity ee Optional Device s AN Caution Risk of Electrical shock high voltage Disposal Do not dispose in municipal waste X Follow local waste regulations to reduce electrical and electronic waste WEEE Table 1 Commonly used Safety Symbols PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option B Table of Contents A Safety Information 2 B Table of Contents 4 C List of Figures and Tables 6 D How to Use this Manual 7 E PAL ITEX 2 Option Installation 8 1 General System Overview 8 9 1 1 Specifications 1 2 Hardware Requirements 10 1 3 Software Requirements 10 1 4 PAL ITEX Option compared to PAL ITEX 2 OPTION 10 2 Installation 11 2 1 Unpacking the Components 11 2 2 Installing the PAL ITEX 2 Option 12 2 3 Inserting the PAL ITEX 2 Syringe Assembly into the Injection Unit 19 2 4 Flush Gas Considerations 21 3 PAL Firmware and Firmware Object Installation for PAL ITEX 2 Option 23 3 1 PAL Firmware Installation for PAL ITEX 2 Option 23 3 2 PAL Firmware Object List for PAL ITEX 2 Option 23 3 3 Installation of Macros for Cycle Composer or Cycles for PAL ICC interpretation 25 4 Adjusting Object Reference Positions 25 F PAL ITEX 2 Option Operation 26 1 PAL ITEX 2 Option Cycle Composer Macros 27 or ICC Cycles 27 1 1 Mac
45. purities can be enriched in the trap and can cause interference or so called ghost peaks in the chromatogram 3 2 Gas Supply Lines etc Extreme precautions must be taken with respect to the gas supply the gas lines and the entire handling thereof It is good practice and for the ITEX technique highly recommended to install an appropriate gas filter or filter set to adsorb any impurities from the gas supply system See also the section Installation point 2 3 If in doubt install a dedicated gas cylinder of known gas quality and check the system thoroughly Be aware that possible contaminants may have already migrated into the GC plumbing and pressure control system The material of the carrier gas tube should be heat cleaned cooper stainless steel or a selected polymer tube or a polymer tube which does not release softener and is non permeable to ambient gases Good laboratory practice must be applied when handling the material Ultra clean material only should be used greasing or the like is strictly forbidden 3 3 Gas Supply System Inside the COMBI PAL The gas supply system inside the COMBI PAL system Is outlined for static headspace technique In general no contamination was observed in routine work A known exception for the static headspace technique is possible contamination from the glue of the headspace syringe This can be observed if the syringe Is operated at the highest temperature 150 C sample prepar
46. ro or Cycle ITEX2 27 1 2 Macro or Cycle ITEX2_ Volatile 28 1 3 Macro or Cycle ITEX2_ TestHS 29 1 4 Macro or Cycle ITEX2_ TestITEX 29 1 5 Macro or Cycle ITEX2_ CheckGasFlow 30 1 6 Macro or Cycle ITEX2_ CleanTrap 3 2 PAL ITEX 2 Cycle Step by Step 32 3 Quantification of ITEX Technique 34 4 Available Trap Material 34 5 Cleaning the Trap 34 6 Trap Heating up Rate and Cooling off Time 35 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option Table of Contents contd 7 Performing ITEX 2 Test 35 7 1 ITEX 2 Test Sample 35 7 2 Preparation of Test Standard Solution 36 7 3 Instrument Preparation for the ITEX Test 36 G Principles of ITEX 2 Enrichment 38 1 Introduction 38 2 Instrumentation for the ITEX Technique 38 2 1 GC Injector Type or Mode 39 2 2 GC Injector Septum 39 2 3 GC Injector Temperature 39 2 4 GC Injector EFC EPC 39 2 5 GC Column Oven 40 2 6 GC Column 40 2 7 Injection Speed 40 3 Contamination of the Analytical Device 40 3 1 Gas Quality 4 3 2 Gas Supply Lines etc 4 3 3 Gas Supply System Inside the COMBI PAL 4 3 4 ITEX 2 Syringe and ITEX 2 Trap 42 3 5 Sample Vial Septum Cap 42 3 6 Contamination Summary 42 H Appendices 43 1 Definition of Terms 43 2 Naming Convention 45 3 PAL ITEX Option Spare Parts 46 3 1 PAL ITEX 2 Option Spare Parts 46 3 2 PAL ITEX Option Spare Parts 46
47. rved this risk can be minimized e Sample from the gas phase only not from the liquid layer e Extend the cleaning time flush e Increase the trap temperature after thermal desorption to a higher cleaning temperature Observe the maximum temperature for the trap material In case the trap material has been contaminated and cannot be cleaned by applying reasonable effort replace the trap This only delays routine work by a few minutes As described above in section F point 5 Cleaning the Trap Is it necessary to clean or condition a newly installed trap first 3 5 Sample Vial Septum Cap Vial septum and the cap can be contaminated by the laboratory environment When working in trace analysis it is advisable to bake out contaminants and cool down in a protected atmosphere such as by using a desiccator 3 6 Contamination Summary This list of possible sources of contamination Is not complete However It should help in identifying the main sources of contamination and gives Ideas of other areas to explore when faced with this problem 42 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option H Appendices 1 Definition of Terms Job Queue A Job Queue is a list of sample processing Jobs Jobs are executed in the order displayed on the JOB QUEUE menu screens New Jobs may be added to the queue while samples are being processed Job
48. technique is another important point to consider The resulting gas flow from the thermal desorption step can be controlled by the plunger movement The gas flow into the GC inlet port must be within the range required by the capillary column and detection system 2 Instrumentation for the ITEX Technique In the early stage of experimental work with the ITEX technique it was thought that all gas sources carrier gas septum purge should be shut off and the split outlet closed during the thermal desorption process There was concern that too much gas would pass into the GC column However It was experimentally proven that these precautions are not necessary 38 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 2 1 GC Injector Type or Mode The recommended GC instrumentation is a split injector with a split liner to provide enough volume to receive the gas phase from the ITEX thermal desorption step Whether the split is closed or open depends greatly on the particular application and must be defined case by case 2 2 GC Injector Septum The standard injector septum can be used however ITEX needle gauge 23 is appropriate for the Merlin adapter If a Merlin adapter is used be aware that the seal can leak if used with a cold injector cold injector to start with ramping the temperature up at the start of injection see text below 2 3 GC Injector Te
49. ted cartridge is prepared such that the electrical cable for the Trap Heater is attached to the side adapter of the heated cartridge Check the assembly by comparing the details as shown in Figure 4 Figure 4 Guide Wire connected to the Heated Cartridge 3 Assemble the headspace syringe and the trap needle as shown below Bi Figure 5 ITEX 2 Headspace Syringe Assembly with Trap Needle PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 4 Insert the assembled ITEX 2 syringe into the Syringe heater as shown below For enhanced access remove the grid from the syringe heater as shown in Figure 6 Figure 6 Grid removed from the Syringe Heater Unit The heated cartridge is prepared such that the electrical cable for the Trap Heater s fixed by a U bolt to the Trap itself See Figure 7 Figure 7 Prepared Cartridge with Trap Heater Thread the needle into the trap heater as shown in Figures 8 and 9 Reinstall the grid onto the syringe heater to protect from high temperatures PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option Figure 9 ITEX 2 Syringe and Heater Assembly In its final position the trap needle fits into the conical shape of the trap heater as shown in Figure 10 Tighten the set screw to fix the heater onto the trap PAL
50. the GC column and would influence the chromatographic separation perhaps even to the point of losing the separation Therefore the removal of water humidity should be a first step outside of the GC inlet system The danger here is loss of volatile compounds at the dry off stage This stepwise desorption Is not provided with the available ITEX 2 device For this reason the only recommended application for the ITEX sample enrichment technique Is for the gas phase the headspace in the vial The ITEX technique can be used with various sample concentration levels The only parameter that varies is the counter for the plunger pumping cycles For example a few pumping cycles can easily reach the ppb level which Is often good enough for detection and quantification of the target compounds The most common application in the ppt range Is the determination of organic Impurities in drinking water To date the recommended technique for drinking water analysis has been the Purge amp Trap technique It has been proven experimentally by various groups that the same analysis can be done with the ITEX sample enrichment technique The ITEX technique makes it possible to reach the ppt level even with very volatile compounds such as vinyl chloride The ease of handling of this technique and the rapid replacement of a trap or a syringe when needed are the main advantages of this enrichment technique The compatibility of ITEX with the GC capillary
51. thread of the plunger bushing Tighten the screw to fix the plunger holder and attach the holding clamp around the cartridge See Figures 17 and 18 PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option aE 4 al Le mr im L Figure 17 Figure 18 Figures 15 to 18 Inserting the ITEX 2 Cartridge into the Z axis 3 Connect the electrical cable from the heated trap to the interface AUX2 at the back side of the unit as shown in Figure 19 Figure 19 Heated Trap connected to the AUX2 Interface Figure 19 shows the electrical connection to the new electronic board for the PAL xtversion APR Control xt The AUX2 interface Is also used for the PAL System 20 PAL is a registered trademark of CTC Analytics AG Switzerland note Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option 2 4 Flush Gas Considerations A gas flow level greater than 6 mL min can destroy the bed of the trap which will result in non reproducible trapping efficiency 2 4 1 Flush Gas Pressure Settings A gas flow restrictor union for the pressure regulator is provided with the ITEX 2 Option kit tem 9 in Figure 2 Remove the original adapter trom the pressure regulator body and replace it with the ITEX 2 adapter with the built in flow restriction frit This restriction allows a flow of approximately 7 mL
52. y Products www restek com or BGB Analytik AG address see above or Any other Restek distributor 3 4 2 Order Information e Article No RT 564309 e Description ITEX Calibration Standard 100 pg mL each solved in P amp T Methanol 41 PAL is a registered trademark of CTC Analytics AG Switzerland p AL Addendum to PAL System User Manual SYSTEM PAL ITEX 2 Option 4 2 ITEX 2 Performance Test The purpose of the test is to verify the enrichment of the analyte s on the trap and to understand the technique as such The enrichment factor can be expressed as the ratio of the simulation of the static headspace sampling compared to the ITEX trapping A quantitative conclusion is not the aim of this test The chromatogram below shows an overlay of the performance test Static Headspace simulation and the enrichment of the analytes using the ITEX 2 technique Note that the ITEX 2 enrichment step was performed 50 times 50 Extraction Strokes The test as described calls for 10 plunger strokes only This number of Extraction Strokes Is sufficient to demonstrate the enrichment technique within a reasonable time frame ITEX with 50 strokes 146 50 lt _ gt 30x higher intensities ae 0 strokes static headspace simulation J JA 545 569 584 609 638 650 677 6 91 705 Figure 26 Test Chromatogram for Static Headspace and ITEX 2 Enrichment 4 2 1 GC and PAL Conditions GC and P
53. ys Injectors The Object Class defines the Items of an Object Object Item An Object contains several Items which can be numerical values with a physical unit e g X Y Z Position Penetration Syringe Scale Length Syringe Volume or references to other objects Note that the term Parameter is reserved for ATOM Parameter PAL firmware commands to be used for a PAL Cycle or Macro 44 PAL is a registered trademark of CTC Analytics AG Switzerland Addendum to PAL System User Manual A SYSTEM PAL ITEX 2 Option Module PAL hardware module either part of a standard PAL configuration e g COMBI PAL HTS PAL or an optional addition e g Cooled Stack MALDI Tool Dilutor The term Module is intentionally used to distinguish from Object which is reserved for the PAL Firmware Object 2 Naming Convention This section recommends standard naming conventions for PAL ITEX 2 targets Following these conventions will allow the PAL ITEX 2 setup to be pre configured for certain applications This will simplify software backups and application development and will improve technical support and training Tray Type Tray Description VT32 20 Vial Tray 32 positions 4 x 8 for 23 mm headspace vials 20 mL VT32 10 Vial Tray 32 positions 4 x 8 for 23 mm headspace vials 10 mL VT21 Vial Tray 21 positions 7 x 14 for 12 mm vials 2 mL VT54 Vial Tray 54 positions 6 x 9 for 12 mm vials 2 mL VT78

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