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中国无机分析化学:2023,13(11):1197-1203
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电感耦合等离子体质谱(ICP-MS)法测定地质样品中Cu和Zn的干扰研究
(1.湖南省地质实验测试中心;2.湖南省郴州生态环境监测中心;3.赛默飞世尔科技有限公司)
Determination of interference studies of copper and zinc in geological samples by inductively coupled plasma-mass spectrometry
YU Lian-ling1,2,3,2,4,2, WANG Gan-zhen1, XU Xiao-hua1, LI Li-yun3, PEN Jun1, GAO Liang4
(1.Hunan Province Geological Testing Institute;2.China;3.Hunan Chenzhou Ecological Environment Monitoring Center;4.ThermoFisher Technology Limited Company)
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投稿时间:2023-02-20    修订日期:2023-03-24
中文摘要: 电感耦合等离子体质谱法(ICP-MS)标准模式测定地质样品中Cu和Zn时,样品溶液中Ti在高温下易形成TiO+和 TiOH+离子产生重叠干扰,使测定值偏离真值而影响测定结果。采用氢氟酸-高氯酸-硝酸消解、王水复溶样品,通过多级在线校正46Ti16O+,消除TiO+和 TiOH+离子重叠干扰,研究了单质Ti与46Ti16O+、质荷比63、64、65、66离子间存在的关系,建立了一种电感耦合等离子体质谱(ICP-MS)法测定地质样品中Cu和Zn的分析方法。实验结果表明:单质Ti对Cu和Zn产生的干扰值与其质量浓度呈非简单的正相关性,TiO+产生的干扰离子质荷比65离子强度比63高,质荷比64离子强度比66 高; 46Ti16O+对质荷比63、66离子干扰增量值与单质Ti质量浓度变化无关;62Ni对46Ti16O+产生同量异位素重叠干扰,测定值须校正来自62Ni的贡献。ICP-MS测定地质样品中Cu和Zn时应选择测量同位素63Cu和66Zn,其检出限(n=7)分别为0.35 μg/g和0.63 μg/g。经有证标准物质验证,测定值与认定值吻合,准确度(RE)<8.6%,精密度(RSD,n=6)<5%。本方法适用于ICP-MS测定地质样品中Cu和Zn的质谱干扰消除,满足地质分析要求。
Abstract:When inductively coupled plasma mass spectrometry (ICP-MS) is used to determine the Cu and Zn concentrations in geological samples, the measurement results are seriously disturbed, and the measured values deviate from the valid values, presumably because the relatively high geochemical abundance of Ti easily forms oxide particles (TiO) under high-temperature conditions. In this paper, an on-line correction method has developed by digestion of hydrofluoric acid-perchloric acid-nitric acid, reconstitution of aqua regia system treatment, and use of 103Rh as an internal standard to establish to eliminate the overlapping interference of Ti oxide. Experimental research of the effects of Ti on the isotopes 63Cu, 65Cu, and isotopes 64Zn, 66Zn, and the impact between TiO and Ni. The results illustrate that: (1) The overlap interference of Ti oxide to 65Cu is more severe than 63Cu, 64Zn is more rigorous than 66Zn, and the increase of interference value is not a simple positive correlation with the change of Ti concentration. (2) The ion count of 62TiO is similar to the 63Cu and 66Zn, and the interference increment value, which is helpful to correct the interference, is not related to the change in the concentration of the Ti element. (3) An ectopic interference to 62TiO is from the 62Ni. The interference value produced by 62TiO must be corrected for the contribution from the single element Ni. By on-line correction of the interference caused by TiO, it is more reasonable for ICP-MS to determine the isotopes of 63Cu and 66Zn, which significantly improves the accuracy and precision of Cu and Zn, reduces the detection limit and expands the linear range. The detection limit of 63Cu and 66Zn is 0.352μg/g and 0.628μg/g, respectively. The method accuracy is <5%, and the precision (RSD, n=7) is <5%. It is verified by the national level geochemical standard materials that the measured value is identical with the identified value.
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基金项目:中央引导地方科技发展专项资金(2018KT5001);湖南省地质院科研基金(HNGSTP202214)
引用文本:
禹莲玲,王干珍,徐小华,李丽云,彭君,高亮.电感耦合等离子体质谱(ICP-MS)法测定地质样品中Cu和Zn的干扰研究[J].中国无机分析化学,2023,13(11):1197-1203.
YU Lian-ling,WANG Gan-zhen,XU Xiao-hua,LI Li-yun,PEN Jun,GAO Liang.Determination of interference studies of copper and zinc in geological samples by inductively coupled plasma-mass spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(11):1197-1203.

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