Thermo Scientific Nicolet iS50 GC-IR User Manual
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Summary of Contents for Thermo Scientific Nicolet iS50 GC-IR
- Page 1 Nicolet iS50 FT-IR Spectrometers iS50 GC-IR Module User Guide 269-278100 Revision A July 2012...
- Page 2 © 2012 Thermo Fisher Scientific Inc. All rights reserved. Nicolet, OMNIC, and ValPro are registered trademarks of Thermo Fisher Scientific Inc. in the United States. Agilent is either a trademark or a registered trademark of Agilent Technologies Inc. in the United States and possibly other countries.
- Page 3 GC-IR Module This section describes the Thermo Scientific iS50 GC-IR module which is an optional sampling module for your Nicolet™ iS™50 spectrometer. Contents • About the GC-IR Module • Important Features • Specifications • Operating Precautions • Compatible Software •...
- Page 4 (GC) with the selectivity of an infrared spectrometer. The GC-IR module is compatible with the Nicolet™ iS™50 FT-IR spectrometer and the following gas chromatographs and autosamplers: • Thermo Scientific TRACE™ 1300 series gas chromatographs with autosamplers • Agilent™ 7890 gas chromatograph Figure 1.
- Page 5 GC-IR Module A Thermo Scientific TRACE 1310 GC is shown in the illustrations in this document. Installation procedures for injectors, detectors and columns are explained in the operating guides provided with the GC and will not be reproduced here. For instructions to connect your column to the GC-IR module transfer line, see “Setting Up the GC-IR...
- Page 6 Ready for use System is not configured for GC-IR sampling Blinking Optics are reconfiguring Back Panel Features Figure 3. iS50 GC-IR module back panel Accessory (Detector) Power switch Exhaust vent Computer AC power Purge iS50 GC-IR Module User Guide Thermo Scientific...
- Page 7 Maintaining the Carbon Filter Specifications Table 2. Specifications for the iS50 GC-IR module Feature Specification Compatible gas chromatographs • Thermo Scientific TRACE 1300 series • Agilent 7890 Maximum temperature of 300 °C transfer/exhaust lines and flow cell Temperature status output...
- Page 8 OMNIC. This software provides an extensive suite of chemometrics features you can use to identify raw materials, perform quantitative analysis, and take spectral measurements. For more information, refer to the help system in your TQ Analyst software. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 9 GC-IR experiments. • Cabling the GC-IR Module • Connecting a Purge Source • Connecting the Transfer and Make-up Gas Lines • Installing a Standard Capillary GC Column • Installing a Wide-Bore Capillary GC Column Thermo Scientific iS50 GC-IR Module User Guide...
- Page 10 GC-IR module. The other end goes to the Accessory port on the back of the spectrometer. (The spectrometer has a right and left Accessory port. Use the one that is closest to the GC-IR module.) iS50 GC-IR Module User Guide Thermo Scientific...
- Page 11 We recommend using dry air supplied by a purge gas generator or pure air generator (available from us), or nitrogen. Please refer to your Site and Safety Information guide for specific purge gas requirements. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 12 The transfer line and the make-up gas line are connected by a stainless-steel Tee union. The third opening on the Tee union connects to either the GC column or a splitter if the GC column is routed to both the IR detector and the GC detector. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 13 Transfer line and make-up gas line connections Make-up gas line Graphite ferrule (size GFF/16) Smaller I.D. cap nut Tee union Graphite ferrule (size GFF/16) Larger I.D. cap nut 1/16 in (0.2 cm) O.D. stainless-steel, glass-lined transfer line Thermo Scientific iS50 GC-IR Module User Guide...
- Page 14 Turn the nuts about one full turn past finger-tight. Related Topics • Installing a Standard Capillary GC Column • Installing a Wide-Bore Capillary GC Column • Measuring and Adjusting the Make-up Gas Flow Rate iS50 GC-IR Module User Guide Thermo Scientific...
- Page 15 3. Choose Collect > Experiment Setup and select the Bench tab. 4. On the Bench tab, set Sample Compartment to GC-IR. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 16 Then tighten the nut another one-quarter turn. 12. Choose OK to close Experiment Setup. Related Topics • Installing a Wide-Bore Capillary GC Column • Connecting the Transfer and Make-up Gas Lines • Connecting the GC Detector iS50 GC-IR Module User Guide Thermo Scientific...
- Page 17 4. Remove 2 to 3 mm from the end of the column to create a clean end with no burrs or jagged edges. To do this, score the column with a tool or scribe intended for this purpose and snap off the end piece. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 18 The larger diameter tubing from the splitter connects through the Tee union and transfer line to the flow cell. The smaller diameter tubing connects to the GC detector. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 19 3. Connect the larger diameter (darker) capillary tubing from the splitter body to the Tee union that joins the transfer line and make-up gas line. a. Remove the cap nut from the free arm of the Tee union. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 20 1. Connect a length of 1/8-in diameter plastic tubing to the exhaust vent on the back of the GC-IR module. The other end can be routed to a room vent or fume hood if necessary. Related Topics • Back Panel Features • Maintaining the Carbon Filter iS50 GC-IR Module User Guide Thermo Scientific...
- Page 21 You can do this either by setting the column flow rate to zero (if your GC has an electronic flow control) or by reducing the column head pressure until the column flow reaches zero. 7. Measure the flow rate again. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 22 This detector is sensitive to infrared radiation between 5000 cm and 600 cm An MCT detector must be cooled with liquid nitrogen before you collect data. The detector dewar is located under the dewar cover on the GC-IR module. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 23 Cool the funnel and funnel stem first: fill the funnel and let it drain completely into the detector two or three times. Always let the liquid nitrogen flow into the detector before adding more liquid nitrogen. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 24 For more information, see “Measuring and Adjusting the Make-up Gas Flow Rate.” 2. Turn on the power switch for the GC-IR module. 3. Press the Touch Point on the top of the GC-IR Module. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 25 7. Enter a value between 30 and 300 °C for each heater and then choose Update Heaters. The table below describes the functions of the status indicators: Table 7. Heater Status LED status and failure modes Thermo Scientific iS50 GC-IR Module User Guide...
- Page 26 GC-IR sensitivity is best when your sample elutes with sharp, narrow peaks. This level of performance is usually obtained by operating your chromatograph in its optimum efficiency range. For best results with the GC-IR application, use these recommended flow rates. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 27 To run the performance test 1. Open OMNIC software. 2. Choose Collect > Advanced Diagnostics. 3. Choose Performance Test. The Nicolet iS50 Diagnostics window lists the available performance tests. Figure 13. Nicolet iS50 Diagnostics window Thermo Scientific iS50 GC-IR Module User Guide...
- Page 28 You simply press the Touch Point to start the workflow. To configure your GC-IR workflow 1. Start OMNIC software. The OMNIC window is displayed. For information about the OMNIC window, choose Help > OMNIC Help Topics. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 29 The Touch Point dialog box provides commonly used settings that define how your GC-IR data will be collected, displayed, measured and reported. Brief descriptions are provided below. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 30 Collecting a background after a specified number of minutes is a good choice for many applications. You will be prompted to collect a background the very first time you collect sample data. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 31 Height” in OMNIC Help Topics. • Threshold. The Y value above which peaks can be found. • Sensitivity. Determines how readily shoulders on peaks and small peaks in the baseline will be found. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 32 6. If you want to overwrite the default settings without overwriting the default experiment, choose Set Default. 7. Choose Save. 8. Choose Experiment Setup at the bottom of Touch Point Setup. 9. In Experiment Setup, select the Series tab. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 33 Experiment Setup, choose Help from Experiment Setup. Note Some settings appear in Experiment Setup and Touch Point Setup. Setting these options in one location automatically changes them in the other. Related Topics • Preparing the GC-IR System for Sampling Thermo Scientific iS50 GC-IR Module User Guide...
- Page 34 9. Wait for the spectrometer and heaters to stabilize. Related Topics • Measuring and Adjusting the Make-up Gas Flow Rate • Setting Flow Cell and Transfer Line Temperature • Configuring Your GC-IR Workflow iS50 GC-IR Module User Guide Thermo Scientific...
- Page 35 The Collect Series Basis Vectors window appears showing the progress of the collection. When data collection is finished, the Save Group box appears. 6. Specify a file name and directory location and choose OK. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 36 GC column, passed through the spectrometer beam path and absorbed infrared energy. Figure 18. Gram-Schmidt reconstruction Spectral intensity axis Peaks Time axis Spectral data display Time response display The spectrum currently being collected appears in the spectral data display. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 37 Figure 19. Using the spectral cursor tool to display the spectrum collected at a specific time in the series data Spectral cursor Spectrum collected at specified time Note To return to a “live” display that shows the spectrum currently being collected, click the Live button. Thermo Scientific iS50 GC-IR Module User Guide...
- Page 38 GC-IR module. There should still be purge gas flowing through the GC-IR module. Related Topics • Connecting a Purge Source • Setting Flow Cell and Transfer Line Temperature iS50 GC-IR Module User Guide Thermo Scientific...
- Page 39 Troubleshooting This section explains how to troubleshoot problems with the GC-IR system. These topics are covered. • Chromatographic Hardware Problems • Spectrometer or GC-IR Module Hardware Problems • Other Problems Thermo Scientific iS50 GC-IR Module User Guide...
- Page 40 GC appears to be operating correctly as a stand-alone instrument, check the transfer lines and flow cell. Sources of leaks or blockages may include: • Transfer lines. Ferrules may be unseated, or graphite or other contaminants may be blocking the lines. iS50 GC-IR Module User Guide Thermo Scientific...
- Page 41 GC beam path is selected. To do this, either press the Touch Point button on the top of the GC-IR module or choose Collect > Experiment Setup, select the Bench tab and set Sample Compartment to GC. Thermo Scientific iS50 GC-IR Module User Guide...