{"title":"Field-portable solid-phase microextraction/fast GC system for trace analysis†","authors":"Tadeusz Górecki, Janusz Pawliszyn","doi":"10.1002/(SICI)1520-6521(1997)1:5<277::AID-FACT3>3.0.CO;2-R","DOIUrl":null,"url":null,"abstract":"<p>A commercially available SRI gas chromatograph (model 9300B) has been adapted to enable the use of solid phase microextraction (SPME) as the sample preparation and introduction technique for fast GC separations in the field. SPME utilizes a small-diameter fused silica fiber coated with a polymeric stationary phase for extraction of organic analytes from aqueous or gaseous matrices. The analytes extracted are thermally desorbed in the injector of a gas chromatograph. Modifications to the instrument included a new injector and modifications to the PID detector. The injector enables very fast fiber heating rates (∼4000 °C/s), which produce narrow injection bands suitable for fast GC. Separation of BTEX (100 ppb each compound) within 15 s has been demonstrated with FID and PID detection. The precision of the results was very good. Separation of purgeables (trichlorofluoromethane, 1,1-dichloroethene, dichloromethane, 1,1-dichloroethane, trichloromethane, tetrachloromethane, trichloroethene, 1,2-dichloropropane, 2-chloroethyl vinyl ether, 1,1,2-trichloroethane, tetrachloroethene, dibromochloromethane, chlorobenzene; 200 ppb each compound) was accomplished in 2 min with good precision with the use of a dry electrolytic conductivity detector (DELCD). The instrument was tested in the field in the analysis of trichloroethylene in soil extracts. PID was used for detection because its dynamic range is better as compared to DELCD. Almost 500 samples were analyzed in 10 days without major problems. © 1997 John Wiley & Sons, Inc. Field Analyt Chem Technol 1: 277–284, 1997</p>","PeriodicalId":100527,"journal":{"name":"Field Analytical Chemistry & Technology","volume":"1 5","pages":"277-284"},"PeriodicalIF":0.0000,"publicationDate":"1998-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/(SICI)1520-6521(1997)1:5<277::AID-FACT3>3.0.CO;2-R","citationCount":"37","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Field Analytical Chemistry & Technology","FirstCategoryId":"1085","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/%28SICI%291520-6521%281997%291%3A5%3C277%3A%3AAID-FACT3%3E3.0.CO%3B2-R","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
引用次数: 37
Abstract
A commercially available SRI gas chromatograph (model 9300B) has been adapted to enable the use of solid phase microextraction (SPME) as the sample preparation and introduction technique for fast GC separations in the field. SPME utilizes a small-diameter fused silica fiber coated with a polymeric stationary phase for extraction of organic analytes from aqueous or gaseous matrices. The analytes extracted are thermally desorbed in the injector of a gas chromatograph. Modifications to the instrument included a new injector and modifications to the PID detector. The injector enables very fast fiber heating rates (∼4000 °C/s), which produce narrow injection bands suitable for fast GC. Separation of BTEX (100 ppb each compound) within 15 s has been demonstrated with FID and PID detection. The precision of the results was very good. Separation of purgeables (trichlorofluoromethane, 1,1-dichloroethene, dichloromethane, 1,1-dichloroethane, trichloromethane, tetrachloromethane, trichloroethene, 1,2-dichloropropane, 2-chloroethyl vinyl ether, 1,1,2-trichloroethane, tetrachloroethene, dibromochloromethane, chlorobenzene; 200 ppb each compound) was accomplished in 2 min with good precision with the use of a dry electrolytic conductivity detector (DELCD). The instrument was tested in the field in the analysis of trichloroethylene in soil extracts. PID was used for detection because its dynamic range is better as compared to DELCD. Almost 500 samples were analyzed in 10 days without major problems. © 1997 John Wiley & Sons, Inc. Field Analyt Chem Technol 1: 277–284, 1997
现场便携式固相微萃取/快速气相色谱系统痕量分析†
一种市售的SRI气相色谱仪(型号9300B)已经过改造,可以使用固相微萃取(SPME)作为样品制备和引入技术,在现场进行快速GC分离。SPME利用小直径熔融二氧化硅纤维,涂有聚合物固定相,用于从水或气体基质中提取有机分析物。提取的分析物在气相色谱仪的进样器中热解吸。对仪器的修改包括一个新的进样器和对PID检测器的修改。该注入器可实现非常快的纤维加热速率(~ 4000°C/s),从而产生适合快速GC的窄注入带。用FID和PID检测,可以在15 s内分离BTEX(每种化合物100 ppb)。结果的精度很好。分离可净化物(三氯氟甲烷、1,1-二氯乙烯、二氯甲烷、1,1-二氯乙烷、三氯甲烷、四氯甲烷、三氯乙烯、1,2-二氯丙烷、2-氯乙基乙烯醚、1,1,2-三氯乙烷、四氯乙烯、二溴氯甲烷、氯苯;使用干式电解电导率检测器(DELCD),在2分钟内以良好的精度完成了每种化合物200 ppb的检测。该仪器在土壤萃取物中三氯乙烯的分析中进行了现场试验。采用PID进行检测,其动态范围优于DELCD。在10天内分析了近500个样本,没有出现重大问题。©1997 John Wiley &儿子,Inc。化学工程学报(自然科学版),1997,19 (3):387 - 394
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