Investigation of problems associated with the determination of iodine in glacial acetic acid samples using flow injection analysis-inductively coupled plasma-mass spectrometry†

K. L. Ackley, J. Day, K. Sutton, J. Caruso
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引用次数: 9

Abstract

Determination of iodine in glacial acetic acid is a major concern of acetic acid manufacturers and consumers. The use of ICP-MS for iodine determinations in acetic acid is hindered by memory effects that produce an elevated background signal necessitating long rinse times between samples. In this work, different analysis methods are employed in an attempt to minimize memory and matrix effects allowing for the accurate determination of iodine in glacial acetic acid using ICP-MS. Ammonium hydroxide solutions (3.7 and 7.4 M) were better at reducing the elevated iodine signal present after the introduction of an acetic acid sample than water or 0.3 M nitric acid. Memory effects were decreased when the sample was introduced by flow injection rather than constant sample aspiration. Peak areas generated by flow injection decreased significantly with increasing ammonium hydroxide concentration in the carrier solution. Iodine determinations made with 1.7 M ammonium hydroxide as the carrier solution were higher than determinations made with 3.7 M ammonium hydroxide as the carrier solution for the same samples, however, the percentage difference between the two determinations varied widely from sample to sample. All samples were analyzed by the method of standard additions in an attempt to compensate for matrix effects. This work illustrates the importance of the carrier solution in the determination of iodine in glacial acetic acid samples.Introduction
流动注射分析-电感耦合等离子体质谱法测定冰醋酸样品中碘的相关问题研究
冰醋酸中碘的测定是冰醋酸生产商和消费者关心的主要问题。ICP-MS用于醋酸中碘的测定受到记忆效应的阻碍,记忆效应会产生升高的背景信号,需要在样品之间长时间冲洗。在这项工作中,采用不同的分析方法,以尽量减少记忆和基质效应,允许使用ICP-MS准确测定冰醋酸中的碘。氢氧化铵溶液(3.7 M和7.4 M)比水或0.3 M硝酸更能降低引入乙酸样品后出现的升高的碘信号。当采用流动注射而不是恒定吸样方式引入样品时,记忆效应降低。随着载体溶液中氢氧化铵浓度的增加,流动注射产生的峰面积显著减小。在相同的样品中,以1.7 M氢氧化铵为载体溶液测定的碘含量高于以3.7 M氢氧化铵为载体溶液测定的碘含量,但两者测定的百分比差异因样品而异。所有样品都用标准添加的方法进行分析,试图补偿基体效应。这项工作说明了载体溶液在测定冰醋酸样品中碘的重要性。介绍
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