纺织学报 ›› 2018, Vol. 39 ›› Issue (07): 100-104.doi: 10.13475/j.fzxb.20170707405

• 染整与化学品 • 上一篇    下一篇

4-氨基偶氮苯在乙腈-盐双水相系统中的萃取

  

  • 收稿日期:2017-07-20 修回日期:2018-01-03 出版日期:2018-07-15 发布日期:2018-07-16

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

  • Received:2017-07-20 Revised:2018-01-03 Online:2018-07-15 Published:2018-07-16

摘要:

为解决纺织品中的4-氨基偶氮苯萃取试时间长,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0.9999,检出限为0.036 mg/kg;4-氨基偶氮苯的回收率在89.71%~101.6%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%。

关键词: 4-基偶氮苯, 双水相, 回收率, 萃取率, 乙腈, 碳酸钾

Abstract:

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 NaOH, dosage of organic, researched recovery ratio of acetonitrile and 4- aminoazobenzene,  the optimum system for extraction of 4- aminoazobenzene was screened. The result show acetonitrile-potassium carbonate is the optimum system,  which is 2% sodium hydroxide solution 10 mL, acetonitrile 4 mL and anhydrous potassium carbonate 4.0 g. The liner 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 standarddeviation (RSD) is 1.40%~3.86%. Extraction rate of acetonitrile is  96.25%~101.00%, RSD is 0.63%~1.27%

Key words: 4-aminoazobene, aqueous two phase system, recovery rate, exraction rate,  acetonitrile, potassium carbonate

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