【引用本文】 刘彤彤, 钱银弟, 黄登丽, . 磷酸沉淀分离-电感耦合等离子体质谱法测定化探样品中的痕量银[J]. 岩矿测试, 2021, 40(5): 650-658. doi: 10.15898/j.cnki.11-2131/td.202105060058
LIU Tong-tong , QIANG Yin-di , HUANG Deng-li . Determination of Trace Silver in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry with Phosphoric Acid Precipitation Separation[J]. Rock and Mineral Analysis, 2021, 40(5): 650-658. doi: 10.15898/j.cnki.11-2131/td.202105060058

磷酸沉淀分离-电感耦合等离子体质谱法测定化探样品中的痕量银

1. 甘肃省有色金属地质勘查局张掖矿产勘查院, 甘肃 张掖 734000;

2. 甘肃省有色金属地质勘查局兰州矿产勘查院, 甘肃 兰州 730030

收稿日期: 2021-05-06  修回日期: 2021-06-29 

基金项目: 甘肃省地质勘查基金项目(202004-Y01)

Determination of Trace Silver in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry with Phosphoric Acid Precipitation Separation

1. Zhangye Geo-Mine Survey Institute, Non-Ferrous Metal Geological Exploration Bureau of Gansu Province, Zhangye 734000, China;

2. Lanzhou Geo-Mine Survey Institute, Non-Ferrous Metal Geological Exploration Bureau of Gansu Province, Lanzhou 730030, China

Received Date: 2021-05-06
Revised Date: 2021-06-29

摘要:应用电感耦合等离子体质谱法(ICP-MS)分析化探样品中的痕量银,通常在标准模式下用干扰校正法或动能歧视模式进行测定。银的两个稳定同位素均受锆和铌的氧化物或氢氧化物的质谱干扰,对于干扰元素锆、铌含量较高而银含量低的样品,测定误差较大,需要将干扰元素与银分离。本方法采用硝酸、氢氟酸、高氯酸消解样品,浓盐酸复溶提取,加入磷酸使大部分溶出的干扰元素锆、铌转化为难溶的磷酸盐化合物,通过沉淀与待测元素银分离。ICP-MS测定时以103Rh为内标,用90Zr16O+同质量数的同位素106Pd间接校正91Zr16O+90Zr16O1H+107Ag的质谱干扰。经国家一级标准物质验证,分析结果在标准值的允许误差范围内,相对标准偏(n=12)为4.3%~12.1%,方法检出限(3SD)为0.0072μg/g。本方法适合土壤、水系沉积物及岩石等化探样品中痕量银的分析。样品处理中引入的磷酸不影响其他常规元素,可用同一份消解液进行测定。

关键词: 痕量银, 电感耦合等离子体质谱法, 化探样品, 磷酸盐沉淀

Determination of Trace Silver in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry with Phosphoric Acid Precipitation Separation

KEY WORDS: trace silver, inductively coupled plasma-mass spectrometry, geochemical samples, phosphate precipitation

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磷酸沉淀分离-电感耦合等离子体质谱法测定化探样品中的痕量银

刘彤彤, 钱银弟, 黄登丽