碘量法测定氯乙酰氯生产废酸液中S2O2-3和SO2-3的含量
Iodometric Determination of S2O2-3 and SO2-3 in Waste Acid Liquor Produced in Preparation of Chloroacetyl Chloride
摘 要
采用碘量法测定氯乙酸氯化法生产氯乙酰氯产生的废酸液中S2O32-和SO32-的含量。在室温,pH 4~5的条件下直接进行碘量法滴定,测得S2O32-和SO32-的总量;以废酸液中所含SO32-物质的量的3倍加入甲醛,(30±1) ℃恒温条件下反应15 min以掩蔽SO32-的干扰,用碘量法测得S2O32-的含量,通过计算差值得到SO32-的含量。加标回收率在99.2%~102%之间,测定值的相对标准偏差(n=10)在0.10%~0.20%之间。
废酸液
氯乙酰氯
Iodometry
Waste acid liquor
Chloroacetyl chloride
Abstract
Iodometry was applied to the determination of S2O32- and SO32- in waste acid liquor obtained from the production of chloroacetyl chloride. The total content of S2O32- and SO32- was determined directly by iodometry at pH 4-5 and room temperature. Formaldehyde amounting to triple times of the amount of SO32- in the sample was added and the mixture was reacted at (30±1) ℃ for 15 min to mask SO32-. Then the content of S2O32- was determined by iodometry. The content of SO32- in the sample was obtained by taking the difference of the 2 values. Test for recovery was made by standard addition method, giving results the range of 99.2%-102% with RSD′s (n=10) in the range of 0.10%-0.20%.
中图分类号 O655.2 DOI 10.11973/lhjy-hx201602018
所属栏目 工作简报
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收稿日期 2015/2/21
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备注张筱岑(1987-),男,江苏泰兴人,硕士,主要从事化验工作。
引用该论文: ZHANG Xiao-cen,YUAN Cun-guang. Iodometric Determination of S2O2-3 and SO2-3 in Waste Acid Liquor Produced in Preparation of Chloroacetyl Chloride[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(2): 200～203
张筱岑,袁存光. 碘量法测定氯乙酰氯生产废酸液中S2O2-3和SO2-3的含量[J]. 理化检验－化学分册, 2016, 52(2): 200～203
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参考文献
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【2】吕咏梅.氯乙酰氯合成技术进展与市场分析［J］.现代农药, 2003,2(4):27-30.
【3】潘国龙,柯鹏,李巨滔,等.氯乙酰氯生产工艺概述［J］.贵州化工, 1994(1):32-34.
【4】WITTER A E, JONES A D. Comparison of methods for inorgaic sulfur speciation in a petroleum production effluent［J］. Environmental Toxicology and Chemistry, 1998,17(11):2176-2184.
【5】王孝镕.硫离子、亚硫酸根和硫代硫酸根的分光光度测定［J］.烟台师范学院学报(自然科学版), 1986(2):18-22.
【6】吴雄伟,吕伟,吴介达.离子色谱法快速测定保险粉中的亚硫酸根、硫酸根和硫代硫酸根［J］.色谱, 1988,6(5):319-210.
【7】KIRYUSHOV V N, SKVORTSOVA L I. Advantages of masking sulfite ions with dilute formaldehyde solutions in the iodometric analysis of sulfur containing mixtures［J］. Journal of Analytical Chemistry, 2010,65(3):305-307.
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