二硫化碳、1,3-丁二烯、苯乙烯及丙烯睛(ACN)分析方法驗證

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Title:	二硫化碳、1,3-丁二烯、苯乙烯及丙烯睛(ACN)分析方法驗證 Methods Validation for Compounds of Carbon Disulfide, 1,3-Butadiene, Styrene and Acrylonitrile
Authors:	王文忻;賴俊雄
Contributors:	中國醫藥學院 research report
Keywords:	二硫化碳;1,3-丁二烯;苯乙烯;丙烯？;分析方法驗證;Carbon Disulfide;1,3-Butadiene;Styrene;Acrylonitrile;Method Validation
Date:	2000-09
Issue Date:	2010-09-06 23:25:34 (UTC+8)
Abstract:	現行的CS/sub 2/分析方法，主要是以活性碳管連接乾燥管進行採樣，分析時，以1mL甲苯進行活性碳中的CS/sub 2/脫附，使用氣相層析儀-火焰光度偵檢器(GC-FPD)進行檢測。現行CS/sub 2/分析方法，在使用上有若干缺失，如：低濃度時之脫附效率偏低，脫附溶劑甲苯易造成分析人員之暴露與健康危害，脫附溶劑造成樣品的稀釋，檢量線線性範圍窄(約10倍範圍)，採樣泵及連接管線配戴，會影響勞工的正常作業習慣，脫附溶劑具健康危害等。由於被動式採樣器具有質量輕、體積小不需動力、不妨礙勞工作業習慣等優點，適合針對作業環境個人採樣，而熱脫附分析方法具有高靈敏性、無須前處理、無需使用溶劑及避免干擾、吸附劑可重複使用。因此本研究將驗證被動式採樣及熱脫附技術，以氣相層析儀/質譜儀(GC/MS)進行分析，建立分析條件，檢量線範圍(0.67至103.4μg)，分析精密度測試。熱脫附方法係參考美國EPA之TO-17熱脫附方法，使用Perkin-Elmer ATD-400的自動熱脫附(ATD)設備。被動式採樣管中之吸附劑選擇，則參考英國HSE(Health and Safety Executive)MDHS 80建議之Spherocarb吸附劑。於動態標準氣體產生設備中測試採集效率及採樣分析方法之精密度及準確度。ABS製造業以丙烯@@、1,3-丁二烯、苯乙烯三種化合物為主要原料，需使用裱敷抗聚合物TBC(4-tert-buty1 catechol)之活性碳管，及HP-FFAP層析管柱執行此三種化合物同步分析；並特別針對注射器、偵檢器及管柱的溫度設定，做最佳化的探討。 The current sampling and analysis method for carbon disulfide for Time Weighted Average (TWA) exposure assessment issued by both Labor of Council Affairs, Taiwan is using sampling method of charcoal tube connecting with active pump followed by solvent desorption and gas chromatography flame photometry detector analysis. There are several drawbacks in this methods, named a few, desorption efficiency decreasing at concentration below 0.25 mg/mL, sample dilution, narrow linear dynamic range, disturbing worker's operation routine, hazardous solvent consumption. The passive sampling method is convenient to use with light weight sampler, no extra power required, and no interference on worker's operation . The passive sampling is highly accepted by worker in the workplace. The thermal desorption method is having advantage on no solvent consumption, no sample dilution, reusability of solid sorbent. The analysis method of thermal desorption interfaced with gas chromatography mass spectrometry (GC/MS) analysis is desirably to validate. The USEPA TO-17 method and HSE (London) MDHS 80 are two methods employed, in that, the Perkin-Elmer ATD-400 (automatic thermal description) is used and Spherocarb is applied as a solid sorbent. The validation of passive sampling method is conducted in a dynamic standard gas generator system. The analytical conditions and calibration standards are established. The accuracy and precision of both sampling and analysis are evaluated. 1,3-butadiene, acrylonitrile and styrene are three major chemicals used in ABS production industry. The analysis of these coexisted compounds are a challenge to the laboratory. The TBC (4-tert-buty1 catechol) coated charcoal is required for the sample collection in order to prevent polymerization of three compounds. The HP-FFAP is employed as the GC separation column. The optimum temperature condition for injector, oven and detector is studied in the separation system.
Appears in Collections:	[China Medical University] Research reports

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