Determination of Trace Silver in Geochemical Samples by Inductively Coupled Plasma-Mass Spectrometry with Phosphoric Acid Precipitation Separation
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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+对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。
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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
要点(1) 通过磷酸沉淀法将大部分干扰元素铌、锆与待测元素银分离，可消除ICP-MS的质谱干扰。
(2) 采用106Pd间接校正91Zr16O+、90Zr16O1H+对107Ag的质谱干扰。
(3) 建立了四酸消解，磷酸沉淀法处理样品，ICP-MS测定地质样品中痕量银的分析方法。
HIGHLIGHTS(1) The phosphate precipitation method separated most of the interfering elements of niobium and zirconium from the analyzed element silver, which eliminated the mass spectrum interference in the determination of silver by ICP-MS.
(2) 106Pd was used to correct the interference of 91Zr16O+ and 90Zr16O1H+ on 107Ag.
(3) A method for the determination of trace silver in geochemical samples by ICP-MS was developed with four acid dissolution andphosphate precipitation.
Abstract:BACKGROUNDStandard mode with interference correction or kinetic energy discrimination mode is commonly used for the determination of trace silver in geochemical samples by inductively coupled plasma-mass spectrometry (ICP-MS). Interference of both stable isotopes of silver occurs in the mass spectrum of the oxides or hydroxides of zirconium and niobium. Moreover, for samples with a higher content of interfering elements and a lower content of silver, the determination accuracy is low, requiring separation of the interfering element from silver in the solution.OBJECTIVESTo develop a method for the determination of trace Ag in geochemical samples.METHODSCommon sample digestion methods and chemical separation (ion exchange separation) were introduced in detail and were discussed in this paper.RESULTSAs proved by first grade standard materials, the result was consistent with standard recommended values, with the relative standard deviation of 4.3%-12.1% (n=12). The detection limit (3SD) of the method was 0.0072μg/g.CONCLUSIONSThis method is suitable for the determination of trace silver in soil, stream sediment and rock samples. The introduction of phosphoric acid does not affect the determination of other conventional elements, and the same digestion solution can be used to determine Ag and other elements.
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图 1 0.05mol/L磷酸加入体积与锆、铌的离子计数
Figure 1. 0.05mol/L phosphoric acid addition and the ion counting of Zr and Nb
表 1 方法精密度
Table 1 Precision tests of the method
标准物质编号 银含量(μg/g) RSD (%) 12次测定值 平均值 GBW07105
(岩石)0.037 0.047 0.037
0.041 0.047 0.041
0.039 0.033 0.036
0.046 0.041 0.0340.040 12.1 GBW07307a
(水系沉积物)1.25 1.15 1.27
1.24 1.17 1.16
1.15 1.24 1.26
1.15 1.17 1.261.20 4.3 GBW07430
(土壤)0.129 0.123 0.131
0.152 0.126 0.136
0.142 0.162 0.151
0.161 0.130 0.1500.141 9.7 
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表 2 标准物质分析结果
Table 2 Analytical results of Ag in certified reference materials
样品类型 标准物质编号 银含量标准值(μg/g) 银含量测定值(μg/g) ΔlgC 水系沉积物 GBW07310 0.27±0.02 0.25 -0.040 GBW07311 3.2±0.4 3.35 0.019 GBW07312 1.15±0.11 1.08 -0.026 GBW07302a 0.040±0.011 0.049 0.088 GBW07304a 0.22±0.03 0.20 -0.037 GBW07305a 0.63±0.06 0.66 0.019 土壤 GBW07401 0.35±0.05 0.34 -0.018 GBW07402 0.054±0.007 0.050 -0.033 GBW07408 0.060±0.009 0.064 0.028 GBW07423 0.076±0.013 0.080 0.022 GBW07424 0.083±0.010 0.079 -0.021 GBW07430 0.14±0.02 0.13 -0.039 岩石 GBW07105 0.040±0.008 0.047 0.070 GBW07106 0.062±0.007 0.056 -0.044 GBW07107 0.047±0.009 0.042 -0.049
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表 3 本方法测定实际样品中银的分析结果与相关方法比对结果
Table 3 Comparison of the analytical results of Ag in real samples determined by this method and alternating current arc emission spectrometry
样品编号 银含量测定值(μg/g) 相对偏差(%) 本文方法 交流电弧发射光谱法 T-1 0.051 0.055 -7.55 T-2 0.038 0.030 23.5 T-3 0.327 0.321 1.85 T-4 0.094 0.104 -10.1 T-5 0.193 0.210 -8.44 T-6 2.260 2.250 0.44 T-7 0.917 0.895 2.43 T-8 0.402 0.384 4.58 T-9 0.262 0.234 11.3 T-10 0.045 0.040 11.8
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