内标法与外标法测定餐具洗涤剂中甲醇含量的分析比较.pdfVIP

第45 卷第7 期 日用化学工业 Vol. 45 No.7 2015 年7 月 China Surfactant Detergent Cosmetics July 2015 内标法与外标法测定餐具洗涤剂中 甲醇含量的分析比较 张鹏，卢伟，管磊 (掘州市产品质量监督检验所，在苏 掘州 225ω0) 摘要:对 GB 9985-2000 中内标法测定餐具洗涤剂中甲醇含量的方法进行了改进，并比较了内标法和外标法在测定洗涤 剂中甲醇含量的差异。通过向洗涤剂样品中加入异丁醇内标液，用759毛乙醇定容到一定体积，经 0.45μm 针式微孔滤 膜过滤，DB -FFAP 色谱柱分离，火焰离子化检测器(FID) 检测，内标法和外标法分别计算洗涤剂中甲醇的含量。实验得 到方法的检出限为0.5 mglL ，内标法和外标法的相对标准偏差(RSD) 分别为0.4% -0.9% 和 0.6% -1. 2% ，平均回收 率分别为 I ∞% -102% 和959毛 -999毛。结果表明，采用内标法和外标法的定量方式获得的结果均能满足检测要求，但 内标法的精密度和回收率优于外标法。 关键词:餐具洗涤剂;气相色谱;甲醇;内标法;外标法 中图分类号:TQ649.7 文献标识码:A 文章编号:1001 -1803(2015)07 -0415 -03 DOI: 10. 13218/j. cnki. csdc. 2015. 07. 012 Comparison of analysis methods for determination of methanol content in dishwashing detergent adopting ISTD and ESTD ZHANG Peng ,LU Wei ,GUAN Lei ( Yangzhou Product Quality Inspection Institute ,Yangzhou ,Jiangsu 225000 ,China) Abstract: The method for determination of methanol content in dishwashing detergent adopting ISTD as specified in GB 9985-2000 was improved. Difference hetween ISTD method and ESTD method for determination of methanol content in dishwashing detergent was compared. Via the spiking of isohutanol and dilution wi也 759毛 ethanol up to the specified volume ,then filtered through O. 45μm pinhole memhrane ,the prepared sample solution was separated hy DB - FFAP chromatographic column and detected by FID detector , quantified separately with ISTD and ESTD. Results showed that the detection limit was O. 5 mglL ,the relative standard derivation of ISTD and ESTD were 0.4% - 0.9% and