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Application News No. G300A Gas Chromatography Analysis of SF6 Insulation Gas Using a GC-BID System LAAN-A-GC-E065A Sulfur hexafluoride (SF6) is an extremely stable gas with excellent dielectric properties and is used in various fields. Applications include tracer gas as well as insulation gas used in electrical equipment such as gas-insulated transformers and circuit breakers. On the other hand, SF6 is also known to be a highly potent greenhouse gas and was identified as an emission reduction target in the Kyoto Protocol at the COP3 meeting. Conventional analysis of SF6 employs an electron capture detector (ECD) which is capable of detecting electrophilic compounds with high sensitivity. However, the quantitation accuracy in the high-concentration range and the hassle of procedures necessary due to the use of radioisotopes have been an issue. Shimadzu's barrier discharge ionization detector (BID) offers high-sensitivity detection of almost all components. Utilizing proprietary barrier discharge technology, the detector achieves both the same stability as general conventional detectors and high sensitivity. This article introduces example analyses of SF6 and SF6 decomposition products. R. Kubota, S. Uchiyama Analysis of Impurities in SF6 SF6 is used as an insulation gas in various electrical equipment and requires purity analysis for quality control to maintain insulation properties and when recycling the gas. Fig. 1 shows the result of analyzing impurities in SF6 using a BID. The primary component SF6 is saturated, but did not influence the quantitation accuracy of surrounding components, showing that high-sensitivity batch analysis of impurities including inorganic gas and lower hydrocarbons was successful. (Under the analytical conditions using this type of column, C2H6 is overlapped by SF6.) The concentrations of impurities found in the SF6 sample are as follows. H2 : 0.9 ppm CO : 0.9 ppm CH4 : 1.7 ppm CO2 : 21 ppm N2O : 2.0 ppm C2H2 : 2.4 ppm C2H4 : 1.4 ppm C3H6 : 1.0 ppm C3H8 : 1.0 ppm Table 1 Measurement Conditions Model : Nexis TM GC-2030 Detector : BID-2030 Inj. Mode : Split 1:4 Inj.Temp. : 150 °C Carrier Gas : 7 mL/min (constant flow rate) Column : MICROPACKED-ST 2.0 m × 1.0 mm I.D. (Input 250 m × 0.50 mm I.D. and df = 10 μm for flow rate calculation) Column Temp. : 35 °C (2.5 min) – 20 °C/min – 250 ˚C (0 min) – 15 °C/min – 265 °C (3.0 min) Purge flow : 3 mL/min Det. Temp. : 280 °C Discharge Gas : 50 mL/min (He) Inj. Volume : 3.0 mL (MGS-2030) Fig. 1 Analysis of Impurities in SF6 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 min H 2 Air CO CH 4 CO 2 C 3 H 6 C 2 H 4 C 2 H 2 C 3 H 8 N 2 O SF 6 1.0 H 2
Application News No. G300A www.shimadzu.com/an/ 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. See http://www.shimadzu.com/about/trademarks/index.html for details. Third party trademarks and trade names may be used in this publication to refer to either the entities or their products/services, whether or not they are used with trademark symbol “TM” or “”. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. 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, 2018 First Edition: Mar. 2018 Revision A: Mar. 2023 01-00000-EN Analysis of Trace SF6 in the Atmosphere Since SF6 is a potent greenhouse gas and its emission into the atmosphere must be avoided, leak tests for insulation gas from electrical equipment and residue tests after collecting gas may require analysis of trace amounts of SF6. Table 2 lists the measurement conditions and Fig. 2 shows the result of analyzing trace SF6 in the atmosphere. SF6 at a concentration of 0.1 ppm was detected (S/N = 24 *1 ) and favorable linearity was obtained in the range from 0.1 to 50 ppm (R 2 = 0.9998). *1 Determined by calculating noise from the baseline between 0.5 and 1.5 min. Table 2 Measurement Conditions Model : Nexis TM GC-2030 Detector : BID-2030 Inj. Mode : Split 1:7 Inj.Temp. : 150 °C Carrier Gas : 45 cm/sec (constant linear velocity) Column : SH-Msieve 5A (0.53 mm I.D.×30 m, d.f.50 μm) *1 Column Temp. : 35 °C (2.5 min) – 20 °C/min – 250 °C (0 min) – 15 °C/min – 270 °C (3.42 min) Purge flow : 3 mL/min Det. Temp. : 280 ˚C Discharge Gas : 50 mL/min (He) Inj. Volume : 3.0 mL (MGS-2030) *1 P/N: 221-75763-30 Analysis of SF6 Decomposition Gas SF6 is used as an insulation gas in circuit breakers. Breakers are installed on electrical grids to shut off high voltages that may occur due to causes such as lightning strikes. When performing maintenance on such breakers, SF6 decomposition gases are analyzed to judge the degradation level of insulation gas. Table 3 lists the measurement conditions and Fig. 4 shows the results of an example analysis of CF4 and SOF2 which are SF6 decomposition gases. Sample injection using a gas sampler and a gas-tight syringe is possible on the same system, allowing analysis of gas samples in various forms and concentrations. Table 3 Measurement Conditions Model : Nexis TM GC-2030 Detector : BID-2030 Inj. Mode : Split 1:4 Inj.Temp. : 150 °C Carrier Gas : 7 mL/min (constant flow rate) Column : MICROPACKED-ST 1.0 m × 1.0 mm I.D. (Input 1,250 m × 0.50 mm I.D. and df = 15 μm for flow rate calculation) Column Temp. : 50 °C (1.0 min)– 25 °C/min – 150 °C (0 min) – 5 °C/min – 200 °C (0 min) Purge flow : 3 mL/min Det. Temp. : 280 ˚C Discharge Gas : 50 mL/min (He) Inj. Volume : 200 μL (gas-tight syringe) Fig. 2 Analysis of Trace SF6 (0.1 ppm) in the Atmosphere Fig. 3 Linearity of SF6 in the Atmosphere (0.1 to 50 ppm) Fig. 4 Analysis of SF6 Decomposition Gases (CF4: 310 ppm, SOF2: 107 ppm) Nexis is a trademark of Shimadzu Corporation or its affiliated companies in Japan and/or other countries. SF 6 H 2 O 2 0.5 1.0 1.5 2.0 2.5 min 0 10 20 30 40 50 Concentration (ppm) 0 100000 200000 300000 400000 500000 600000 700000 800000 900000 1000000 1100000 1200000 Area (μV·sec) R 2 = 0.9998 2.5 5.0 7.5 10.0 12.5 min CF 4 SOF 2 Air CO 2 SF 6
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