【引用本文】 禹莲玲, 郭斌, 柳昭, 等. 电感耦合等离子体质谱法测定高锡地质样品中的痕量镉[J]. 岩矿测试, 2020, 39(1): 77-84. doi: 10.15898/j.cnki.11-2131/td.201906270094
YU Lian-ling , GUO Bin , LIU Zhao , et al. Trace Cadmium in Geological Samples with High Content of Tin Determined by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2020, 39(1): 77-84. doi: 10.15898/j.cnki.11-2131/td.201906270094

电感耦合等离子体质谱法测定高锡地质样品中的痕量镉

湖南省地质测试研究院, 湖南 长沙 410007

收稿日期: 2019-06-27  修回日期: 2019-08-19 

基金项目: 中央引导地方科技发展专向资金项目《湖南省地质测试研究院大型仪器科研设备购置项目》(2018KT5001)

作者简介: 禹莲玲,硕士,工程师,岩矿测试分析方向。E-mail:yull2010@yeah.net。。

Trace Cadmium in Geological Samples with High Content of Tin Determined by Inductively Coupled Plasma-Mass Spectrometry

Hunan Province Geological Testing Institute, Changsha 410007, China

Received Date: 2019-06-27
Revised Date: 2019-08-19

摘要:应用电感耦合等离子体质谱法(ICP-MS)测定地质样品中的痕量镉,存在多种质谱干扰,通常采用在线或离线方程进行校正,当样品中含锡较高时,采用传统固定系数校正方程,易导致测定结果有明显偏离,甚至结果出现负数。本文针对含高锡的地质样品,应用ICP-MS测定其中的镉,采用氢氟酸-高氯酸-硝酸敞开酸溶消解、硝酸浸提体系处理样品,通过测定111Cd、113Cd、114Cd同位素,研究了干扰元素Sn、In、Zr、Mo对镉测定的影响。结果表明镉与干扰源浓度变化呈非简单的正相关性。①同质异位素Sn或In产生的干扰增值Δ(114Cd/114Sn或113Cd/113In)随干扰源浓度增大逐渐变大,114Sn对114Cd的干扰系数在0.0271~0.0222,113In对113Cd的干扰系数在0.0670~0.0412;②Zr和Mo在测定条件下形成氧化物和多原子复合离子物质对Cd均产生不同程度的质谱干扰。通过测定与样品中干扰源浓度相近的单一标准溶液产生的Cd干扰值,经在线修正干扰系数(γ),建立了精确的校正方程。该方法经标准物质验证,准确度高,相对标准偏差在6.57%~9.94%(n=7),方法检出限为0.03mg/kg,达到了地质分析检测要求,为高锡地质样品中的痕量镉分析提供了依据。

关键词: 地质样品, , , 氢氟酸-高氯酸-硝酸酸溶, 在线修正, 电感耦合等离子体质谱法

Trace Cadmium in Geological Samples with High Content of Tin Determined by Inductively Coupled Plasma-Mass Spectrometry

KEY WORDS: geological samples, tin, cadmium, hydrofluoric acid-perchloric acid-nitric acid dissolution, on-line correction, inductively coupled plasma-mass spectrometry

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电感耦合等离子体质谱法测定高锡地质样品中的痕量镉

禹莲玲, 郭斌, 柳昭, 赵昕, 戴长文, 彭君