Determination of trace silver in geochemical samples by inductively coupled plasma mass spectrometry after sample dissolution with aqua regia
LIU Tongtong1, HUANG Dengli2
1. Zhangye Geo-mine Survey Institute of Non-ferrous Metal Geological Exploration Bureau of Gansu Province,Zhangye 734000, China; 2. Lanzhou Geo-mine Survey Institute of Non-ferrous Metal Geological Exploration Bureau of Gansu Province, Lanzhou 730030, China
Abstract：Determination of silver content has important significance for prospecting indicator and mineral resource prediction in the field of geochemistry. The sample was dissolved with aqua regia in water bath. Zirconium and niobium were separated by phosphoric acid precipitation method. 107Ag was selected as the determination isotope, and 103Rh was used as internal standard. The analysis method of trace silver in geochemical samples by inductively coupled plasma mass spectrometry (ICP-MS) was established with interference factor method. The optimization experiments of addition amount of 0.05 mol/L phosphoric acid showed that 5 mL of 0.05 mol/L phosphoric acid could convert the dissolved zirconium and niobium to insoluble phosphate compounds, realizing the separation of zirconium and niobium from the testing element, i.e., silver. 106Pd, which had same mass number with 90Zr16O+, was used to indirectly correct the interference of 107Ag by 91Zr16O+ and 90Zr16O1H+. Compared to the direct correction method of interference factor of zirconium oxide, it improved the determination error caused by parameter change of oxide ratio in instrumental running process. Under the optimized experimental conditions, the linear correlation coefficients of calibration curves were higher than 0.999. The limit of detection and limit of quantification was 0.006 6 μg/g and 0.022 μg/g, respectively. Total 13 certified reference materials (including 6 stream sediments, 3 rocks and 4 soils) were analyzed according to the experimental method. The logarithmic differences (ΔlgC) between determination results and certified values were calculated according to DZ/T 0130.4-2006 The specification of testing quality management for geological laboratories. The results indicated that the requirements of DZ/T 0130.4-2006 could be satisfied. Six geochemical samples were selected and determined according to the experimental method, and then compared with the alternating current (AC) arc emission spectroscopy (ES). The results showed that the measurement results of experimental method and ES method had no significant difference. The relative standard deviations (RSD, n=12) of determination results were between 2.6% and 12.4%, which could meet the precision requirements of DZ/T 0130.4-2006. The proposed method was applicable for the analysis of trace silver in geological samples with silicon dioxide content not more than 77% (mass fraction).
刘彤彤, 黄登丽. 王水溶样-电感耦合等离子体质谱法测定化探样品中痕量银[J]. 冶金分析, 2021, 41(7): 61-66.
LIU Tongtong, HUANG Dengli. Determination of trace silver in geochemical samples by inductively coupled plasma mass spectrometry after sample dissolution with aqua regia. , 2021, 41(7): 61-66.
[1] 岩石矿物分析编委会.岩石矿物分析:第3分册[M].4版.北京:地质出版社,2011:639-647. [2] 薛静,安帅,汪寅夫,等.王水水浴消解-电感耦合等离子体质谱法测定土壤中的硒[J].岩矿测试,2020,39(5):720-725. XUE Jing,AN Shuai,WANG Yinfu,et al.Determination of selenium in soil by inductively coupled plasma-mass spectrometry with aqua regia digestion in water bath[J].Rock and Mineral Analysis,2020,39(5):720-725. [3] 王佳翰,冯俊,王达成,等.电感耦合等离子体质谱法测定地球化学样品中钼镉钨铀锡[J].冶金分析,2017,37(6):20-25. WANG Jiahan,FENG Jun,WANG Dacheng,et al.Determination of molybdenum,cadmium,tungsten,uranium and tin in geochemical samples by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2017,37(6):20-25. [4] 边朋沙,李晓敬,申玉民,等.电感耦合等离子体质谱法测定地质样品中痕量碲[J].冶金分析,2018,38(6):25-30. BIAN Pengsha,LI Xiaojing,SHEN Yumin,et,al.Determination of trace telluriun in geological sample by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2018,38(6):25-30. [5] 邢智,漆亮.P507萃淋树脂分离-电感耦合等离子体质谱法快速测定化探样品中的银[J].岩矿测试,2013,32(3):398-401. XING Zhi,QI Liang.Separation with P507 levextrel resin for rapid determination of Ag in geochemical exploration samples by ICP-MS[J].Rock and Mineral Analysis,2013,32(3):398-401. [6] 邢智,漆亮.P507负载泡塑分离-电感耦合等离子体质谱法同时测定化探样品中银钨钼[J].岩矿测试,2014,33(4):486-490. XING Zhi,QI Liang.Simultaneous determination of Ag,W and Mo in geochemical exploration samples by ICP-MS using P507 loaded foam for separation[J].Rock and Mineral Analysis,2014,33(4):486-490. [7] 孙朝阳,戴雪峰,代小吕,等.氨水分离-电感耦合等离子体质谱法测定化探样品中的银[J].岩矿测试,2015,34(3):292-296. SUN Chaoyang,DAI Xuefeng,DAI Xiaolü,et al.Determination of silver in samples for geochemical exploration by inductively coupled plasma-mass spectrometry after ammonia complexation[J].Rock and Mineral Analysis,2015,34(3):292-296. [8] 杨艳明.电感耦合等离子体质谱法测定水系沉积物中银铜砷锑铋镉[J].冶金分析,2019,39(7):58-64. YANG Yanming.Determination of silver,copper,arsenic,antimony,bismuth and cadmium in stream sediment by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2019,39(7):58-64. [9] 周丽萍,李中玺.王水提取-电感耦合等离子体质谱法同时测定地质样品中微量银,镉,铋[J].分析试验室,2005,24(9):20-25. ZHOU Liping,LI Zhongxi.Determination of silver,cadmium and bismuth in geological samples by inductively coupled plasma mass spectrometry with aqua regia treatment[J].Chinese Journal of Analysis Laboratory,2005,24(9):20-25. [10] 范凡,温宏利,屈文俊,等.王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟[J].岩矿测试,2009,28(4):333-336. FAN Fan,WEN Hongli,QU Wenjun,et al.Determination of arsenic,antimony,bismuth,silver,cadmium and indium in geological samples by inductively coupled plasma-mass spectrometry with aqua regia sample digestion[J].Rock and Mineral Analysis,2009,28(4):333-336. [11] 于亚辉,闫红岭,陈浩凤,等.电感耦合等离子体质谱法测定地球化学样品中的银[J].理化检验(化学分册),2016,52(7):834-846. YU Yahui,YAN Hongling,CHEN Haofeng,et al.Determination of silver in geochemical samples by inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2016,52(7):834-846. [12] 刘静波,张更宇.全自动消解电感耦合等离子体质谱仪测定环境土壤中铍钡铊银[J].分析试验室,2018,37(2):207-212. LIU Jingbo,ZHANG Gengyu.Determination of Be,Ba,Tl and Ag in environmental soil by inductively coupled plasma mass spectrometry with automatic digestion instrument[J].Chinese Journal of Analysis Laboratory,2018,37(2):207-212. [13] 徐进力,邢夏,唐瑞玲,等.动能歧视模式ICP-MS测定地球化学样品中14种痕量元素[J].岩矿测试,2019,38(4):394-402. XU Jinli,XING Xia,TANG Ruiling,et al.Determination of 14 trace elements in geochemical samples by ICP-MS using kinetic energy discrimination mode[J].Rock and Mineral Analysis,2019,38(4):394-402. [14] 无机化学丛书编委会.无机化学丛书 第8卷:钛分族,钒分族,铬分族[M].北京:科学出版社,1995:133-135.
