Addendum to PAL User Manual Installation and ... - PAL System

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note 7.2. Preparation of Test Standard Solution Addendum to PAL System User Manual PAL ITEX-2 Option The test or calibration standard solution as received (concentration 100 µg/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 µL 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. • Secondary standard solution: Concentration 10 µg/mL • 1 µL aliquot = 10 ng/ µL 7.2.2. GC Detector FID, TCD or any other Non-selective Device Add 10 µL 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. • Secondary standard solution: Concentration 10 µg/mL • 10 µL aliquot = 100 ng/ µL 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 µg/mL can be used directly. Add a 1 µL 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: • Static Headspace: ITEX2_TestHS • ITEX enrichment: ITEX2_TestITEX 7.3.2. GC Method Parameters • GC column: nearly any capillary column can be used to separate the compounds in the test sample • GC Injector temperature: 200 to 250°C, split less for 1 min. • Detector: settings depend on the detector used • GC oven temperature: 40 0 C, hold 1 minute, 10 0 C/min up to 150 0 C, hold 2 minutes 36
7.3.3. PAL Injection Parameters Addendum to PAL System User Manual PAL ITEX-2 Option Parameter Value Parameter Value Syringe Temperature 80 °C Pullup Delay 5 s Trap Starting Temperature 35 °C Desorption Temperature 250 °C Incubation Temperature 80 °C Inject to GC Inj Incubation Time 5:00 min Desorption Speed 100 µL/sec Agitator Speed 500 rpm Trap Cleaning Temperature 250 °C Extraction Volume 1000 µL Trap Cleaning Time 2:00 min Extraction Strokes 10 GC Ready Time 10:00 min Extraction Speed 100 µL/sec Injection Volume (1) 500 µL (1) Injection Volume is 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’. note 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. 37
Page 1 and 2: Addendum to PAL System User Manual
Page 3 and 4: Commonly used Safety Symbols I ° C
Page 5 and 6: Table of Contents (contd.) Addendum
Page 7 and 8: note note D. How to Use this Manual
Page 9 and 10: note 1.1. Specifications Part numbe
Page 11 and 12: 2. Installation 2.1. Unpacking the
Page 19 and 20: 2.3. Inserting the PAL ITEX-2 Syrin
Page 21 and 22: note 2.4. Flush Gas Considerations
Page 23 and 24: note note note note 2.4.4. Flush Ga
Page 29 and 30: The Trap temperature is lowered to
Page 31 and 32: 1.6. Macro or Cycle ‘ITEX2_CleanT
Page 33 and 34: Step 3. Thermal desorption of analy
Page 35: Addendum to PAL System User Manual
Page 39 and 40: 2.1. GC-Injector Type or Mode Adden
Page 41 and 42: 3.1. Gas Quality Addendum to PAL Sy
Page 43 and 44: H. Appendices 1. Definition of Term
Page 45 and 46: Module Addendum to PAL System User
Page 47 and 48: 3.3. Ordering Information for Custo
Page 49: Addendum to PAL System User Manual

Addendum to PAL User Manual Installation and ... - PAL System

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