首页|高压密闭消解-电感耦合等离子体质谱法测定地球化学样品中6种元素的含量

高压密闭消解-电感耦合等离子体质谱法测定地球化学样品中6种元素的含量

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提出了高压密闭消解-电感耦合等离子体质谱法(ICP-MS)测定地球化学样品中硼、钴、钼、镉、锗、铍等6种元素含量的方法.取样品0.100 0 g于聚四氟乙烯坩埚中,加入3 mL 50%王水(体积比为3∶1∶4的盐酸-硝酸-水混合溶液)和0.5 mL氢氟酸,静置30 min后,于180℃烘箱中高压消解18 h.消解结束后,用水定容至50 mL,采用ICP-MS测定其中6种元素含量.结果表明:硼、钴元素的质量浓度在200 μg ·L-1以内,钼、镉、锗、铍元素的质量浓度在10.0 μg ·L-1以内与对应的谱峰强度与内标谱峰强度比呈线性关系,检出限(3s)为0.005~0.12 mg ·kg-1;方法用于分析国家标准物质,测定值与认定值基本一致,并且测定值的相对标准偏差(n=12)均小于8.0%;方法用于两个实际地球化学样品的分析,其测定结果与DZ/T 0279-2016的基本一致,且相对标准偏差(n=12)均小于5.0%.
Determination of 6 Elements in Geochemical Sample by Inductively Coupled Plasma Mass Spectrometry with High Pressure Sealed Digestion
A method for determination of 6 elements,including boron,cobalt,molybdenum,cadmium,germanium,and beryllium,in geochemical sample by inductively coupled plasma mass spectrometry(ICP-MS)with high pressure sealed digestion was proposed.0.100 0 g of the sample was taken into a polytetrafluoroethylene crucible,and 3 mL of 50%aqua regia(a mixture of hydrochloric acid-nitric acid-water at a volume ratio of 3∶1∶4)and 0.5 mL of hydrofluoric acid were added,settling for 30 min.Then the mixture was performed by high pressure digestion in a 180℃oven for 18 h.After digestion,its volume was made up to 50 mL with water,in which 6 elements were determined by ICP-MS.As shown by the results,linear relationships between the corresponding spectral peak intensity and internal standard spectral peak intensity ratios and mass concentrations were found within 200 μg·L-1 for boron and cobalt elements and 10.0 μg·L-1 for molybdenum,cadmium,germanium,and beryllium elements,with detection limits(3s)of 0.005-0.12 mg·kg-1.The method was used to analyze national standard materials,and the determined values were basically consistent with the certified values,with RSDs(n=12)of the determined values less than 8.0%.The method was also used to analyze two actual geochemical samples,and the determined results were basically consistent with those by DZ/T 0279-2016,with RSDs(n=12)less than 5.0%.

high pressure sealed digestioninductively coupled plasma mass spectrometry(ICP-MS)geochemical sampleelement

辜洋建、陈璐、王玉环、周腾飞、王玲玲、高玉花

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山东省物化探勘查院,济南 250013

地下资源环境高精度探测山东省工程研究中心,济南 250013

山东省地质勘查工程技术研究中心,济南 250013

中国石油大学(华东)地球科学与技术学院,青岛 266580

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高压密闭消解 电感耦合等离子体质谱法(ICP-MS) 地球化学样品 元素

自然资源部滨海城市地下空间地质安全重点实验室开放基金中央高校基本科研业务费专项项目

BHKF2021Z0718CX06019A

2024

理化检验-化学分册
上海材料研究所

理化检验-化学分册

CSTPCD北大核心
影响因子:0.647
ISSN:1001-4020
年,卷(期):2024.60(7)