Determination of Boron, Germanium, Bromine, Molybdenum, Tin, Iodine and Tungsten in Geochemical Survey Samples by ICP-MS with Alkali Fusion-Cation Exchange Resin Separation
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摘要:
多目标地球化学填图是多目标区域地球化学调查中重要的区域性基础性工作之一，为了更好地反映出地球化学背景变化，要求分析方法具有更高的准确度、精密度以及更低的检出限。地球化学调查样品中的硼锗溴钼锡碘钨主要采用单独或分组熔矿的方法进行制备和测定，操作流程长且涉及6种测定方法。本文基于前人研究，对以上7种元素的分析方法进行系统总结，采用过氧化钠-氢氧化钠碱熔，分取溶液加入柠檬酸，利用阳离子交换树脂，静态交换2~3h，除去溶液中大量的阳离子减少基体干扰，利用电感耦合等离子体质谱法（ICP-MS）测定硼锗溴钼锡碘钨含量。结果表明：7种元素的检出限分别为0.66、0.096、0.78、0.11、0.15、0.29、0.27μg/g，相对标准偏差（RSD，n=11）在2.1%~7.5%之间，均小于10%。该方法操作简便、快速，应用成本低，并且整合了相关6种分析配套方法，应用于测定厚覆盖区地球化学调查样品，精密度和准确度均满足《多目标区域地球化学调查规范（1：250000）》（DZ/T 0258-2014）要求。
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关键词:
- 地球化学调查样品 /
- 过氧化钠-氢氧化钠碱熔 /
- 柠檬酸 /
- 阳离子交换树脂 /
- 电感耦合等离子体质谱法
Abstract:BACKGROUND Multi-target geochemical mapping is one of the most important basic regional tasks in multi-target regional geochemical surveys. In order to better reflect changes in the geochemical background, analytical methods are required to have higher accuracy and precision, and lower detection limits. Elements B, Ge, Br, Mo, Sn, I, and W in geochemical survey samples are mainly prepared and determined by smelting ore individually or in groups. The analysis procedure is long and involves 6 methods.
OBJECTIVES In order to integrate 6 supporting analysis methods, optimize analysis conditions, and improve the accuracy and precision of the method.
METHODS The mixed reagent of sodium peroxide and sodium hydroxide was used for alkali fusion. Citric acid was added to the solution. Cation exchange resin was used for static exchange for 2-3 hours to remove a large amount of cations in the solution and reduce matrix interference. B, Ge, Br, Mo, Sn, I, and W were determined using inductively coupled plasma mass spectrometry.
RESULTS The detection limits of B, Ge, Br, Mo, Sn, I, and W were 0.66, 0.096, 0.78, 0.11, 0.15, 0.29, and 0.27μg/g, respectively. Relative standard deviation (RSD, n=12) was between 2.1% and 7.5%, which were all less than 10%.
CONCLUSIONS The method is simple, rapid and low-cost, and its precision and accuracy meet the requirements of 《Specification of multi-purpose regional geochemical survey (1:250000)》 (DZ/T 0258-2014). It can quickly and accurately determine B, Ge, Br, Mo, Sn, I, W in geochemical survey samples in a thick coverage area.
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表 1 不同模式Mo和W的测定结果
Table 1. Analytical results of Mo and W determined with different modes
标准物质编号 元素 标准值(μg/g) 碰撞模式测定值(μg/g) 普通模式测定值(μg/g) GBW07404 Mo 2.6±0.3 2.58 2.74 W 6.2±0.5 6.06 6.32 GBW07424 Mo 0.52±0.04 0.51 0.58 W 1.66±0.10 1.69 1.75 GBW07364 Mo 1.7±0.1 1.65 1.58 W 0.97±0.11 0.95 1.08 GBW07366 Mo 1.56±0.20 1.63 1.66 W 15.5±0.8 15.2 16.7 
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表 2 标准物质中各元素测定结果
Table 2. Analytical results of each element in standard samples
标准物质编号 元素 标准值(μg/g) 测定平均值(μg/g) ΔlgC RSD (%) GBW07978 B 39±3 35.9 -0.040 3.9 Ge 1.39±0.06 1.47 0.024 2.1 Br 8.5±0.5 7.99 -0.027 4.3 Mo 0.68±0.03 0.64 -0.026 7.5 Sn 3.4±0.2 3.28 -0.016 3.2 I 3.49±0.15 3.61 0.015 2.3 W 2.1±0.3 1.95 -0.032 4.6 GBW07980 B 85±4 80.8 -0.022 4.2 Ge 2.3±0.3 2.57 0.048 2.8 Br 3.3±0.3 3.68 0.047 5.9 Mo 12.2±0.6 13.5 0.044 6.3 Sn 411±36 398.2 -0.014 4.1 I 3.42±0.17 3.35 -0.009 3.1 W 164±9 179.0 0.038 4.4 GBW07309 B 54±6 58.4 0.034 3.2 Ge 1.3±0.2 1.37 0.023 2.2 Br 1.2±0.3 1.28 0.028 3.9 Mo 0.64±0.11 0.68 0.026 5.8 Sn 2.6±0.4 2.71 0.018 2.6 I 0.63±0.09 0.57 -0.043 4.1 W 1.8±0.2 1.69 -0.027 6.3 GBW07384 B 10.4±1.0 9.61 -0.034 2.7 Ge 1.79±0.10 1.71 -0.020 5.4 Br 3.7±0.5 3.82 0.014 6.3 Mo 2.59±0.15 2.88 0.046 3.9 Sn 5.19±0.41 4.87 -0.028 3.2 I 2.95±0.36 3.14 0.027 4.2 W 4.73±0.27 4.87 0.013 3.5
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表 3 加标回收实验结果
Table 3. Recovery tests of the method
样品编号 元素 测定值(μg/g) 加标量(μg/g) 加标后测定值(μg/g) 加标回收率(%) S1 B 29.3 30 58.2 96.3 Ge 1.52 2 3.42 95.0 Br 3.31 4 7.44 103.3 Mo 0.77 1 1.68 91.0 Sn 4.33 4 7.94 90.3 I 0.96 1 1.89 93.0 W 1.98 2 4.12 107.0 S2 B 27.2 30 56.6 98.0 Ge 1.44 2 3.63 109.5 Br 5.24 5 9.77 90.6 Mo 0.71 1 1.65 94.0 Sn 12.3 10 21.6 93.0 I 1.64 2 3.66 101.0 W 2.08 2 3.93 92.5 S3 B 9.78 10 18.9 91.2 Ge 1.47 2 3.32 92.5 Br 5.09 5 9.53 88.8 Mo 0.93 1 2.09 116.0 Sn 2.89 4 6.56 91.8 I 3.32 4 7.76 111.0 W 1.58 2 3.97 119.5 S4 B 9.55 10 21.1 115.5 Ge 1.43 2 3.52 104.5 Br 4.84 5 10.7 117.2 Mo 0.93 1 1.92 99.0 Sn 3.65 4 8.21 114.0 I 2.45 2 4.73 114.0 W 1.43 2 3.74 115.5 S5 B 15.4 20 33.1 88.5 Ge 1.43 2 3.28 92.5 Br 4.89 5 9.76 97.4 Mo 0.83 1 1.77 94.0 Sn 3.67 4 7.98 107.8 I 3.21 4 7.69 112.0 W 1.36 2 3.7 117.0
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表 4 本文方法与文献相同和不同方法的对比
Table 4. Comparison of analytical results of elements determined with the same method and different methods in the literatures
分析元素 前处理方法 分析方法 检出限(μg/g) RSD (%) B Ge Br Mo Sn I W 7种元素(本文方法) 碱熔 ICP-MS 0.66 0.096 0.78 0.11 0.15 0.29 0.27 2.1~7.5 B、Ge、Mo、Sn、I、W[14] 碱熔 ICP-MS 0.57 0.092 - 0.13 0.11 0.22 0.3 0.99~5.9 B、Ge、Sn、I[24] 碱熔 ICP-MS 0.92 0.09 - - 0.29 0.1 - 1.49~4.94 B、Sn[2] - 原子发射光谱 3.6 - - - 0.63 - - 6.0~12.0 Mo、W[31] 碱熔 极谱 - - - 0.141 - - 0.104 3.37~4.06 Mo、W[32] 碱熔-离子交换 ICP-OES - - - 11 - - 15 1.1~2.3 Ge[33] 酸溶 AFS - 0.037 - - - - - 4.0~7.1 Br、I[8] 酸溶 ICP-MS - - 0.21 - - 0.15 - 1.2~5.0 I[34] 酸溶 ICP-MS - - - - - 0.012 - 4.88~9.19 Br[7] 粉末压片 XRF - - 0.61 - - - - 3.1~4.7
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表 5 实际样品测定结果
Table 5. Analytical results of real samples
样品编号 元素 测定值(μg/g) RSD (%) 样品编号 元素 测定值(μg/g) RSD (%) S1 B 30.23 3.08 S6 B 25.1 1.65 Ge 1.25 2.24 Ge 1.43 2.09 Br 3.77 1.32 Br 5.72 5.70 Mo 0.91 5.98 Mo 1.04 2.98 Sn 4.21 9.44 Sn 4.13 9.21 I 1.22 3.56 I 3.28 3.65 W 2.15 6.05 W 1.54 4.03 S2 B 27.5 8.67 S7 B 22.4 4.67 Ge 1.46 1.76 Ge 1.31 2.98 Br 4.37 1.14 Br 5.03 5.88 Mo 0.71 8.28 Mo 0.88 4.98 Sn 10.2 1.93 Sn 4.02 7.83 I 1.25 4.28 I 3.09 3.60 W 2.65 7.95 W 1.83 8.21 S3 B 8.97 2.67 S8 B 28.8 3.64 Ge 1.28 9.76 Ge 1.60 1.82 Br 6.04 8.92 Br 6.77 3.46 Mo 0.84 6.33 Mo 0.76 3.03 Sn 3.09 2.65 Sn 3.62 2.26 I 3.61 1.23 I 3.33 2.60 W 1.48 7.21 W 2.50 4.32 S4 B 12.5 4.28 S9 B 21.1 7.35 Ge 1.56 2.09 Ge 1.63 4.74 Br 4.65 4.67 Br 6.13 9.22 Mo 0.75 3.82 Mo 0.82 3.54 Sn 3.72 6.01 Sn 3.45 2.09 I 3.11 2.65 I 3.52 3.18 W 1.32 2.78 W 3.04 6.03 S5 B 13.8 6.02 S10 B 26.2 7.32 Ge 1.16 3.02 Ge 1.47 2.44 Br 4.21 4.88 Br 9.02 8.87 Mo 0.79 4.50 Mo 0.97 6.52 Sn 3.89 2.89 Sn 4.06 4.59 I 3.40 1.04 I 3.48 3.85 W 1.27 5.01 W 2.63 6.77
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表 6 本法与标准方法的准确度和精密度对比
Table 6. Comparison of accuracy and precision between this method and the standard method
元素 GBW07978 GBW07980 标准值(μg/g) 本方法(n=11) 对比方法(n=11) 标准值(μg/g) 本方法(n=11) 对比方法(n=11) 测定值(μg/g) ΔlgC RSD (%) 测定值(μg/g) ΔlgC RSD (%) 测定值(μg/g) ΔlgC RSD (%) 测定值(μg/g) ΔlgC RSD (%) B 39±3 35.9 -0.04 3.9 40.2 0.013 5.3 85±4 80.8 -0.022 4.2 92.4 0.036 3.8 Ge 1.39±0.06 1.47 0.024 2.1 1.44 0.015 0.8 2.3±0.3 2.57 0.048 2.8 2.19 -0.021 1.3 Br 8.5±0.5 7.99 -0.027 4.3 8.76 0.013 2.2 3.3±0.3 3.68 0.047 5.9 3.45 0.019 1.3 Mo 0.68±0.03 0.64 -0.026 7.5 0.67 -0.006 3.6 12.2±0.6 13.5 0.044 6.3 11.3 -0.032 2.1 Sn 3.4±0.2 3.28 -0.016 3.2 3.54 0.018 3.8 411±36 398.2 -0.014 4.1 426 0.016 4.4 I 3.49±0.15 3.61 0.015 2.3 3.41 -0.01 1.7 3.42±0.17 3.35 -0.009 3.1 3.69 0.033 3.7 W 2.1±0.3 1.95 -0.032 4.6 2.29 0.038 5.0 164±9 179 0.038 4.4 158.3 -0.015 5.2 B 54±6 58.4 0.034 3.2 57.3 0.026 4.4 10.4±1.0 9.61 -0.034 2.7 9.67 -0.032 4.2 Ge 1.3±0.2 1.37 0.023 2.2 1.28 -0.007 0.6 1.79±0.10 1.71 -0.02 5.4 1.85 0.014 2.4 Br 1.2±0.3 1.28 0.028 3.9 1.32 0.041 6.8 3.7±0.5 3.82 0.014 6.3 3.46 -0.029 1.9 Mo 0.64±0.11 0.68 0.026 5.8 0.61 -0.02 1.7 2.59±0.15 2.88 0.046 3.9 2.52 -0.012 0.9 Sn 2.6±0.4 2.71 0.018 2.6 2.47 -0.022 3.2 5.19±0.41 4.87 -0.028 3.2 5.47 0.023 2.9 I 0.63±0.09 0.57 -0.043 4.1 0.67 0.027 2.8 2.95±0.36 3.14 0.027 4.2 2.89 -0.009 1.6 W 1.8±0.2 1.69 -0.027 6.3 1.96 0.037 6.8 4.73±0.27 4.87 0.013 3.5 4.56 -0.016 3.9 注：B、Sn为DZ/T 0279—2016的第11部分，采用粉末进样，交流电弧-发射光谱法测定；Ge、Mo分别为DZ/T 0279—2016的第16、07部分，采用酸溶ICP-MS法测定；Br为DZ/T 0279—2016的第10部分，采用粉末压片XRF法测定；I为DZ/T 0279—2016的第24部分，采用半熔ICP-MS法测定；W为DZ/T 0279—2016的第30部分，采用碱熔ICP-MS法测定。
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