干洗织物中氯代烃溶剂残留的气相色谱-质谱测定

Method for Determining Chlorinated Solvent Residues in Dry Cleaning Fabrics with Gas Chromatography-Mass Spectrometry

采用固相微萃取和气 质联用技术(GC MS)对干洗衣物中氯代烯烃的残留和释放进行了分析测定。干洗过程使用的有害物质包括四氯乙烯(PCE)、三氯乙烯(TCE)及少量的三氯乙烷,这些挥发性有机物已列入许多国家和地区优先控制的污染物指标。该方法参照欧洲生态纺织品标准100对目标化合物的限量控制,以加标的标准贴衬为样品基质,将样品浸渍在含5%(体积分数)甲醇的饱和NaCl溶液中,于(40±1)℃水浴中超声处理10min后,再将样液用100μmPDMS固相微萃取纤维顶空提取,然后进行GC MS测定。目标化合物在线性范围内(PCE和TCE为0 005mg/kg～5 000mg/kg,三氯乙烷为0 012mg/kg～1 200mg/kg)满足衣物的干洗剂残留安全评定要求,方法的最小检测量(LOQ)低于0 005mg/kg,加标回收率为90 6%～108.7%。

An analytical technique was provided for using headspace solid phase microextraction (SPME) with gas chromatographymass spectrometry (GCMS) to estimates exposure and emissions of chlorinated hydrocarbon residues in dry cleaning fabrics or garments. Hazardous substances used by chlorinated dry cleaning operation include perchloroethylene (PEC), trichloroethylene (TCE) and small amounts of trichloroethane, all known as volatile organic compounds (VOCs) listed in many professional testing criteria and limit values of pollutant control index. A standard fabric matrix was spiked with several chlorinated volatile organic compounds to achieve a theoretical concentration based on koTex Standard 100 levels. Samples were soaked in 5% (volume fraction) methanol saturated NaCl solution with supersonic treatment in a waterbath at (40±1) ℃ for 10 min, and then the solution extracted by headspace SPME with a 100 μm PDMS fiber was analyzed by GCMS. The method gives the applicable range of 0005 mg/kg-5000 mg/kg for PCE and TCE, and 0012 mg/kg-1200 mg/kg for trichloroethane as the safe assessment of fabrics and garments in dry cleaning. The limits of detection for target compounds PCE, TCE and trichloroethane were 0005 mg/kg with average recoveries between 906%-108.7%. 