ICP-MS Simultaneous Determination of Iodine and Copper, Lead, Zinc, Manganese and Iron in Surface Water Sample with Iodine Oxidized by Sodium Hypochlorite
摘 要
取地表水样90.0 mL置于100 mL容量瓶中,用硝酸及氢氧化钠溶液调节其酸度至pH 7~9之间,加水至96 mL,加入0.6%(质量分数)次氯酸钠溶液1 mL,放置2 h使碘完全氧化至非挥发性碘酸盐,再加入硝酸3 mL酸化使溶液总体积至100.0 mL。这一处理实现了采用电感耦合等离子体质谱法同时测定碘与水样中铜、铅、锌、锰、铁的含量。在质谱分析中,测定207Pb和127I使用标准(STD)模式,其余元素均采用动能歧视(KED)模式。经试验,选用钬作为测定碘的内标。所测定6种元素的质量浓度在一定范围内与其相应的信号强度之间呈线性关系。另按规定方法对空白样品进行测定,计算得到6种元素的检出限(3s)依次为0.096,0.071,0.062,0.065,0.044,0.19 μg·L-1。以地表水实际样品为基体,各加入上述6种元素的标准溶液,按方法分析并进行回收试验,测得回收率在83.2%~116%之间。测定值的相对标准偏差(n=5)在2.4%~7.3%之间。同一样品经本方法和国家标准方法对所涉及的6种元素进行测定,两方法的结果基本一致。
Abstract
90.0 mL of surface water sample was taken and its acidity was adjusted to pH 7-9. Water was added to make its volume to 96 mL, 1 mL of 0.6% (mass fraction) NaOCl solution was added and the solution was set aside for 2 h to have the iodine completely oxidized to iodate. 3 mL of HNO3 acid were then added to made its total volume to 100.0 mL. By this treatment, iodine was transformed to the non-volatile state, and could be determined together with Cu, Pb, Zn, Mn and Fe in the same acidic sample solution by ICP-MS. In the MS analysis, STD mode was used for determination of 207Pb and 127I, while KED mode was used for determination of the 4 remainder. Holmium was found to be a suitable internal standard for determination of iodine. Linear relationships between values of signal intensity and mass concentrations of the 6 elements were kept in definite ranges. Detection limits (3s) found by running blank determinations for 12 times, were given as follows:0.096 (I), 0.071 (Cu), 0.062 (Pb), 0.065 (Zn), 0.044 (Mn), 0.19 (Fe) μg·L-1. Tests for recovery were made by addition of standard solutions of the 6 elements to surface water samples as matrixes, results of recovery found were in the range of 83.2%-116%. Values of RSDs (n=5) found were ranged from 2.4% to 7.3%. A same surface water sample was analysed simultaneously by the present method and the method given in the standards of HJ 778-2015 and GB/T 5750.6-2006, and the results obtained by these methods were in consistency.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201907018
所属栏目 专题报道(电感耦合等离子体质谱法)
基金项目
收稿日期 2019/1/30
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备注王佳翰,工程师,硕士,主要从事水质、岩矿分析工作,wangjiahanhao@163.com
引用该论文: WANG Jiahan,FENG Jun,YANG Xiujiu,ZHANG Yafeng. ICP-MS Simultaneous Determination of Iodine and Copper, Lead, Zinc, Manganese and Iron in Surface Water Sample with Iodine Oxidized by Sodium Hypochlorite[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(7): 840~845
王佳翰,冯俊,杨秀玖,张亚峰. 次氯酸钠氧化碘-电感耦合等离子体质谱法同时测定地表水样品中的碘及铜、铅、锌、锰、铁的含量[J]. 理化检验-化学分册, 2019, 55(7): 840~845
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参考文献
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【3】MOXON R E D, DIXON E J. Semi-automatic method for the determination of total iodine in food[J]. The Analyst, 1980,105(1249):344-352.
【4】RODGERS K, POOLE D B. The estimation of iodine in biological materials:A modification of the method of Ellis & Duncan[J]. Biochemical Journal, 1958,70(3):463-471.
【5】AL-AMMAR A, REITZNEROVÁ E, BARNES R M. Thorium and iodine memory effects in inductively-coupled plasma mass spectrometry[J]. Fresenius' Journal of Analytical Chemistry, 2001,370(5):479-482.
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【8】李冰,史世云,何红蓼,等.电感耦合等离子体质谱法同时测定地质样品中痕量碘溴硒砷的研究Ⅱ.土壤及沉积物标准物质分析[J].岩矿测试, 2001,20(4):241-246.
【9】高运川,高勤芬,孙明星,等.电感耦合等离子体-质谱同时测定煤、焦中砷、溴、碘[J].分析化学, 2007,35(8):1175-1178.
【10】沈璐佳,董亚红.电感耦合等离子体质谱法同时测定矿泉水中痕量溴和碘[J].中国无机分析化学, 2012,2(4):31-34.
【11】赵秋香,汪模辉,刘赛红.电感耦合等离子体质谱仪同时测定地下水中的溴和碘[J].光谱实验室, 2009,26(6):1519-1522.
【12】JUDPRASONG K, JONGJAITHET N, CHAVASIT V. Comparison of methods for iodine analysis in foods[J]. Food Chemistry, 2016,193:12-17.
【13】VANHOE H, VAN ALLEMEERSCH F, VERSIECK J, et al. Effect of solvent type on the determination of total iodine in milk powder and human serum by inductively coupled plasma mass spectrometry[J]. The Analyst, 1993,118(8):1015-1019.
【14】TAKAYANAGI K. The oxidation of iodide to iodate for the polarographic determination of total iodine in natural waters[J]. Talanta, 1986,33(5):451-454.
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【16】樊祥,陈迪,张润何,等.微波消解-电感耦合等离子体质谱法测定乳制品中总碘[J].理化检验-化学分册, 2015,51(1):119-121.
【17】周相武,汪晓军,刘姣,等.次氯酸钠溶液的氧化性研究[J].氯碱工业, 2006(8):28-30.
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