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Application News No. G320 The Nexis GC-2030 gas chromatograph has recently begun to support packed columns. The detectors compatible with packed columns are a flame ionization detector (FID) and a thermal conductivity detector (TCD). In this article, the amount of ethanol in liquor was analyzed using the Nexis GC-2030 (FID) with a glass- packed column in accordance with the analytical method prescribed by the Japanese National Tax Agency. C. Kanamori, K. Kawamoto Packed Column Support System The glass column that can be installed into the Nexis GC- 2030, a system compatible with packed columns, is the same as that used for the GC-17 or GC-2010, and it can be shared between these instruments. Using the FID-2030Packed kit (P/N: S221-85191-41), the FID-2030 can be easily modified to become a packed FID by: • Replacing the standard nozzle for the FID with one for a packed FID; • Removing the FID’s capillary column adaptor. Fig. 1 shows the appearance of the instrument and an example of glass column installation. Example of Analysis Analysis of Ethanol in Liquor According to the analytical method prescribed by the Japanese National Tax Agency, ethanol, as the standard sample, was diluted with water and prepared at concentrations of 5%, 10%, 15% and 20% (v/v). To 0.1 mL of each ethanol standard solution, 0.9 mL of the internal standard solution (acetone) was added to make samples that were analyzed to create the calibration curve. Actual samples of beer and Japanese sake available on the market were prepared. In the same manner as above, 0.9 mL of the internal standard solution was added to 0.1 mL of each liquor sample. These samples were analyzed, and the ethanol was quantified using the calibration curve created. 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 Ethanol in Liquor Using Nexis™ GC-2030 (FID) Fig. 1 Appearance of Nexis™ GC-2030 and Example of Glass Column Installation Model : Nexis GC-2030 /AOC-20i +SINJ-2030+FID-2030Packed Kit Injection Mode : Direct Injection Volume : 1.0 μL Injection Temp. : 200 °C Carrier Gas :N 2 Carrier Gas Control : Constant flow rate (35 mL/min) Column : PEG 1000 10% CW 60/80 AW-DMCS (2 m × 3 mm I.D.) Column Temp. : 100 °C Detector : Flame ionization detector (FID) Detector Temp. : 200 °C Detector Gas :H 2 32.0 mL/min, Air 200 mL/min (no makeup gas required) Extendable to Dual Line A packed column analysis of samples with a column temperature program may cause greater baseline drift due to the elution of the liquid phase from the column, which can affect identification or quantitative processing. The FID-2030 (compatible with packed columns) can be extended to a dual line system comprising a reference line, which has a sample vaporization chamber, column and detector, for elimination of baseline drift, as well as the sample line for analyzing samples.
www.shimadzu.com/an/ No. G320 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 Chromatogram and Calibration Curve for Standard Samples The chromatogram of the standard samples are shown in Fig. 2, and the calibration curve is shown in Fig. 3. Table 2 Quantitative Results for Beer and Japanese Sake Fig. 4 Chromatogram of Actual Samples Beer Japanese sake Concentration value of analysis (%) n = 1 5.287 15.514 n= 2 5.286 15.517 n= 3 5.288 15.516 n= 4 5.285 15.524 n= 5 5.287 15.523 n= 6 5.29 15.525 n= 7 5.288 15.519 n= 8 5.288 15.532 n= 9 5.289 15.532 n = 10 5.294 15.533 Average 5.288 15.524 %RSD 0.047 0.045 First Edition: Jun. 2020 アセトン(IS) エタノール 20% 15% 10% 1.50 2.00 2.50 3.00 3.50 min 5% Acetone (IS) Ethanol Fig. 2 Chromatogram of Standard Samples Chromatogram of Actual Samples and Quantitative Results for Ethanol The quantitative results for beer and Japanese sake are shown in Table 2. R 2 =0.99966 0.0 5.0 10.0 15.0 濃度比 0.0 0.2 0.4 0.6 0.8 1.0 面積比 Area ratio Conc. ratio Fig. 3 Calibration Curve for Ethanol アセトン(IS) 日本酒 ビール min 0.0 2.5 5.0 7.5 10.0 12.5 Acetone (IS) Japanese sake Beer Conclusion With a glass packed column connected to the FID modified for packed columns in the Nexis GC-2030, ethanol in liquor was analyzed using a single line FID. The average concentrations of ethanol in liquor obtained using the same samples with the GC-2014 gas chromatograph are as follows: 5.31 (%RSD: 0.413) in beer and 15.56 (%RSD: 0.138) in Japanese sake. As these results are the same as those obtained using packed columns in conjunction with the GC-2014, they confirmed that packed analysis with GC-2030 could obtain favorable results. Optional Information on Nexis GC-2030 The Nexis GC-2030 system makes a wide variety of useful options available. <Oven light> The light illuminating the entire oven makes column replacement easy. The moderate brightness illuminates the column connection areas while minimizing strain on the operator. Nexis is a trademark of Shimadzu Corporation in Japan and/or other countries.
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