4-氨基偶氮苯在乙腈-盐双水相系统中的萃取  

Extraction of 4-aminoazobenzene by acetonitrile-salt aqueous two-phase system

作　　者：丁力进 孙峰[1,2] 顾伟 DING Lijin;SUN Feng;GU Wei(Suzhou Institute of Inspection on Fiber,Suzhou,Jiangsu 215128,China;National Silk and Garment Quality Supervision Testing Center,Suzhou,Jiangsu 215128,China)

机构地区：[1]苏州市纤维检验所,江苏苏州215128 [2]国家丝绸及服装产品质量监督检验中心,江苏苏州215128

出　　处：《纺织学报》2018年第7期100-104,共5页Journal of Textile Research

摘　　要：为解决纺织品中的4-氨基偶氮苯萃取时间长,乙醚挥发以及污染环境和结果不准确等问题,以乙腈-无机盐-水双水相系统,建立了一种环保高效的4-氨基偶氮苯前处理方法。经由无机盐分相能力差异,分析乙腈与几种常见盐构成双水相系统中各成分之间配比、有机相加入量、水相中氢氧化钠的质量分数对有机相的萃取率和4-氨基偶氮苯回收率的影响,筛选出4-氨基偶氮苯萃取的最优系统。结果表明:乙腈/碳酸钾系统为4-氨基偶氮苯萃取的最佳系统;当2%氢氧化钠溶液体积为10 mL,乙腈体积为4 mL,无水碳酸钾质量为4.0 g时,效果最优,线性范围为0~20 mg/kg,相关系数为0.999 9,检出限为0.036 mg/kg;4-氨基偶氮苯的回收率在89.71%~101.60%之间,其相对标准偏差为1.40%~3.86%;乙腈萃取率在96.25%~101.00%之间,其相对标准偏差为0.63%~1.27%。In order to solve the problems of long extraction time,volatilization of ether,environment pollution and poor result accuracy during the extraction of 4-aminoazobenzene, the acetonitrile-salt aquatic two phase system was established,and an environment-friendly and efficient sample treatment method was developed for detection of 4-aminoazobenzene in textiles. Based on phase capability difference of inorganic salts,several common salts on the phase separation in acetonitrile-water were examined. According to the extraction rate,mass fraction of Na OH,dosage of organic,researched recovery ratio of acetonitrile and 4-aminoazobenzene,the optimum system for extraction of 4-aminoazobenzene was screened. The results show that acetonitrile-potassium carbonate is the optimum system,which is composed of 2% sodium hydroxide solution 10 mL,acetonitrile 4 mL and anhydrous potassium carbonate 4. 0 g. The linear range is 0-20 mg/kg with correlation coefficient of 0. 999 9. Limit of detection is 0. 036 mg/kg. Recovery rate of 4-aminoazobenzene is 89. 71%-101. 6%,relative standard deviation（ RSD） is 1. 40%-3. 86%. Extraction rate of acetonitrile is 96. 25%-101. 00%,RSD is0. 63%-1. 27%.

关 键 词：4-氨基偶氮苯 双水相 回收率 萃取率 乙腈 碳酸钾 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程] O656.31[轻工技术与工程—纺织科学与工程]