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    在线膜萃取-离子色谱法测定乙酸正丁酯中无机阴离子的含量

    In-line Membrane Extraction-IC Determination of Inorganic Anions in n-Butyl Acetate

    • 摘要: 用去离子水作为萃取溶剂,通过中空纤维萃取了乙酸正丁酯中的无机阴离子,并用离子色谱法测定了Cl-、NO2-、Br-和NO3-的含量。选择如下萃取条件:① 搅拌速率:450 r·min-1;② 萃取流量:30 μL·min-1;③ 萃取时间:30 min。按优化的条件操作,Cl-、NO2-、Br-和NO3-的质量浓度在一定范围内呈线性,其检出限(3S/N)依次为0.002,0.006,0.100,0.004 mg·L-1。按方法对含Cl-和Br-各1.00 mg·L-1及NO2-和NO3-各0.20 mg·L-1的混合溶液进行测定,测定值的相对标准偏差(n=6)依次为6.4%,7.9%,12%,7.4%。对纯乙酸正丁酯样品进行分析,并做加标回收试验,Cl-、NO2-、Br-和NO3-的平均回收率依次为89%,115%,115%和103%。

       

      Abstract: Inorganic anions (including Cl-, NO2-, Br-, and NO3-) in sample of n-butyl acetate was extracted by de-ionized water, passing through the hollow fibre membrane, and determined by IC. Optimized conditions were given as follows: ① rate of agitation: 450 r·min-1; ② flow-rate of extraction: 30 μL·min-1; ③ time of extraction: 30 min. When operated under the optimum conditions, linear relationships between values of response signals and mass concentration of the 4 anions were obtained in definite ranges and detection limits (3S/N) found for the 4 anions were 0.002, 0.006, 0.100, 0.004 mg·L-1 respectively. Mixed solutions containing 1.00 mg·L-1 for each of Cl- and Br-, and 0.20 mg·L-1 for each of NO2- and NO3- were analyzed by the proposed method to test for precision, values of RSD′s (n=6) found were 6.4%, 7.9%, 12% and 7.4% respectively. A sample of pure n-butyl acetate was analyzed by this method and recovery was tested by standard addition method, giving results of average recovery of 89%, 115%, 115% and 103% for Cl-, NO3-, Br- and NO3- respectively.

       

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