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建立了液液萃取-分散液液微萃取-气相色谱-质谱联用技术测定纺织废水中痕量偶氮染料的方法。废水中的偶氮染料在碱性条件下经连二亚硫酸钠还原成芳香胺后,先用叔丁基甲醚液液萃取、盐酸反萃进行预浓缩及净化;再以乙腈-氯苯体系进行分散液液微萃取,气相色谱-质谱测定。对前处理条件进行了优化,考察了酸碱度及盐效应对芳香胺萃取效率的影响,结果表明:液液萃取过程中加入30 g NaCl,分散液液微萃取过程中加入1 mL 5 mol/L的NaOH调节体系至碱性才能达到较好的萃取效率。在优化的实验条件下,21种目标物均呈现良好的线性关系,其中13种芳香胺的线性范围为0.05~10 μg/L,7种芳香胺的线性范围为0.05~5 μg/L,2,4-二氨基苯甲醚的线性范围为20~100 μg/L,相关系数为0.996~0.999。20种芳香胺的检出限可达0.05 μg/L,2,4-二氨基苯甲醚检出限为20 μg/L。印染、机织、印花等实际废水加标试验表明,方法的回收率为75.6%~115.1%。该方法富集倍数高,检出限低,适用于纺织废水中痕量禁用偶氮染料的检测。 相似文献
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A method for the simultaneous determination of 17 phenolic compounds in infant textile products, including phenol,o-phenylphenol,alkylphenols and bisphenols,was established using gas chromatography-mass spectrometry(GC-MS). The samples were extracted by 0.1 mol/L KOH solution,derived with acetic anhydride. The derivatives were extracted with ethyl acetate,separated by HP-5MS column,and determined by gas chromatography-mass spectrometry with ion mode scanning. Under the optimized conditions,the method had a good linear relationship in the range of 0.5-6.25 mg/L(R2>0.9990),the recoveries ranged from 80% to 110%, the relative standard deviations were 1.0%-8.6%,and the limit of quantification was 1.0 mg/kg. The method can achieve the simultaneous detection of 17 phenolic compounds in infant textile products. © 2023, Youke Publishing Co., Ltd. All rights reserved. 相似文献
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