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Application News No. G323 The Nexis GC-2030 gas chromatograph has begun to support packed columns. The detectors compatible with packed columns are a flame ionization detector (FID) and a thermal conductivity detector (TCD). As an example of SUS packed column TCD analysis using the Nexis GC-2030, this article introduces gas analysis using a Molecular Sieve 5A (MS-5A) column. K. Kawamoto Packed Column Support System An SUS column which can be used for the Nexis GC- 2030, a system compatible with packed columns, is the same as that used for the GC-14, GC-17 or GC-2014, and it can be shared between these instruments. For the TCD for packed columns (PTCD-2030), a column is connected to the sample vaporization chamber (SINJ) and the carrier gas flow rate is controlled by the Advanced Flow Controller (AFC). Fig. 1 shows the appearance of the instrument equipped with the PTCD-2030 and an example of connecting an SUS column and an empty pipe to the analysis line and reference line, respectively. Also, it is possible to eliminate the effect of baseline drift identified in a column temperature program analysis by connecting the same type of column as that for the analysis line on the reference side. Gas Analysis Gas samples were analyzed using an SUS packed column (MS-5A). As samples to be analyzed, approximately 1000 ppm (v/v) each of H 2 , CH 4 , CO and C 2 H 6 were prepared using He as the base gas. The samples were prepared by repeatedly taking a certain volume of the target ingredient using a gas-tight syringe and adding it to a bag filled with He, which served as the blank. In the analysis, 1 mL of each gas sample was aspirated by a gas-tight syringe and injected manually. Since ambient gas was mixed into the bag or syringe (needle) during these operations, N 2 or O 2 , which was not added intentionally, was also analyzed. Analysis Conditions Table 1 lists the configuration of the instrument used for analysis and the analysis conditions. Table 1 Instrument Configuration and Analysis Conditions Gas Chromatography Packed Column Analysis of Gases Using Nexis™ GC-2030 (TCD) Fig. 1 Appearance of Instrument with PTCD-2030 and Example of SUS Column Installation Model : Nexis GC-2030APT Injection Mode : Direct Injection Volume : 1 mL (gas-tight syringe) Injection Temp. : 120 °C Carrier Gas : He Carrier Gas Control : 40 mL/min Column : MS-5A 60/80 (2 m × 3 mm I.D.) * Reference line measurement was performed via a directly connected single column Detector : Thermal Conductivity Detector (TCD) Detector Temp. : 220 °C Current : 100 mA Column Oven Temp. : 60 °C (5min) - 10 °C/min – 200 °C (6min) In gas analysis using a TCD, as the mount of sample injected increases, this may cause greater baseline drift associated with sample injection, and the peak of the compound whose retention time is short is affected by the drifting baseline. To reduce baseline drift, an effective countermeasure is to change the carrier gas control from flow rate control to pressure control, as is the case with analysis using the GC-2014. In this situation, we recommend to install an advanced pressure controller (AUX APC) for pressure control.
www.shimadzu.com/an/ No. G323 Application News Shimadzu Corporation For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. Shimadzu disclaims any proprietary interest in trademarks and trade names used in this publication other than its own. See http://www.shimadzu.com/about/trademarks/index.html for details. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. © Shimadzu Corporation, 2020 Results of Gas Analysis The chromatogram of gas analysis is shown in Fig. 2. First Edition: Jun. 2020 Fig. 2 Chromatogram of Gas Analysis Conclusion With an SUS packed column connected to a TCD for packed columns of the Nexis GC-2030, gas analysis was performed. The peaks of compounds were favorably separated. Additionally, the analysis results reconfirmed that pressure control using an APC is an effective technique for gas analysis when a large quantity of sample injected. Optional Information on Nexis GC-2030 Nexis GC-2030 system makes a wide variety of useful options available. <Hydrogen sensor> For customers who are considering the use of H 2 as carrier gas in a situation where it is difficult to obtain helium, installation of a hydrogen sensor is recommended to ensure the safe operation of the instrument. This sensor monitors the hydrogen concentration in the gas chromatograph oven and promptly detects potential leakages. When a leakage is detected, it stops the temperature control operation and automatically switches the mode to the safe standby mode. If the hydrogen concentration increases further to exceed 2%, the main power to the gas chromatograph is cut to prevent accidents. Nexis is a trademark of Shimadzu Corporation in Japan and/or other countries. Baseline Drifts Associated with Sample Injection Fig. 3 shows the baseline drifts caused by injection of 0.5 mL, 1 mL and 2 mL of the sample gas while controlling the flow rate of the carrier gas. As shown in the figure, as more sample is injected, this is associated with a lower baseline, and these baseline drifts are still detected at 0.6 minutes when the H 2 peak is eluted. As a comparison, Fig. 4 shows the baseline drifts while the pressure of the carrier gas was controlled using an APC. When the pressure of the carrier gas is controlled, the result is baseline drifts associated with sample injection, but the baselines return to the original level at approximately 0.4 minutes after 2 mL of sample is injected, indicating that the baselines return to their original level earlier than when the flow rate of carrier gas is controlled. Fig. 3 Baseline Drifts at Sample Injection (Flow Control) min 0.0 0.2 0.4 0.6 0.8 1.0 ⿊:2 mL注入 赤:1 mL注入 ⻘:0.5 mL注入 CO C 2 H 6 CH 4 N 2 O 2 H 2 min 0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 min 0.0 0.2 0.4 0.6 0.8 1.0 ⿊:2 mL注入 赤:1 mL注入 ⻘:0.5 mL注入 Black: 2 mL injected Red: 1 mL injected Blue: 0.5 mL injected Black: 2 mL injected Red: 1 mL injected Blue: 0.5 mL injected Fig. 4 Baseline Drifts at He Gas Injection (Pressure Control)
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