Simultaneous Determination of Silver, Boron, Tin, Molybdenum and Lead in Geological Samples by Atomic Emission Spectrometer with Full Spectrum
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摘要: 掌握地质样品中银锡硼钼铅的含量对于研究成矿规律和地球化学找矿极其重要，目前的分析方法很少能一次性准确高效检出银锡硼钼铅。本文在前人研究基础上建立了应用全谱发射光谱仪固体粉末进样，一次性高效、准确地分析检测地质样品中银锡硼钼铅的方法。采用国家一级标准物质（岩石、土壤和水系沉积物）对合成硅酸盐标准曲线进行第二次拟合以降低基体的干扰；设置元素分析谱线转换值实现元素分析谱线的简单切换，不同的样品含量使用不同的分析谱线，达到分析结果更加接近样品真值的效果，同时扩大了标准曲线线性范围。结果表明：银锡硼钼铅的检出限分别为0.0077μg/g、0.19μg/g、0.68μg/g、0.058μg/g、0.49μg/g，方法精密度在3.23%~9.39%之间。应用本方法分析土壤、水系沉积物、岩石国家一级标准物质的测定值与其认定值相符，△logC值的绝对值均小于0.10；实际样品和外控样的一次测试结果合格率分别为92%~98%、100%。本方法简单，分析速度快，避免了样品稀释带来的污染，使用多条分析谱线测定国家标准物质，相比传统发射光谱法使用单分析谱线的测定值更加接近认定值，检出限优于《地质矿产实验室测试质量管理规范》的规定值。Abstract:
BACKGROUNDThe contents of silver, tin, boron, molybdenum, and lead in geological samples are extremely important for studying the metallogenic regularity and for geochemical prospecting. Current analytical methods rarely determine silver, tin, boron, molybdenum, and lead simultaneously. OBJECTIVESTo establish a method to simultaneously determine silver, tin, boron, molybdenum and lead in geological samples. METHODSTo eliminate the matrix interference, first-class standard materials (rock, soil and water sediments) were used for linear fitting of the synthetic silicate standard materials curve. By setting analytical line conversion values, different analytical line can be used for samples with different contents. RESULTSThe detection limits of silver, tin, boron, molybdenum, and lead were 0.0077μg/g, 0.19μg/g, 0.68μg/g, 0.058μg/g, 0.49μg/g, respectively. The precisions of the method were 3.23%-9.39%. The measured value of national first class standard materials including soil, water sediments and rock by this method was in accordance with standard values, with an absolute value of △logC < 0.10. The qualified rates of actual sample were 92%-98%, and the qualified rate of the inspection sample was 100%. CONCLUSIONSThis method is easy to apply and can be used to analyze samples rapidly. It can also be used to avoid contamination during sample dilution. Compared with traditional atomic emission spectrometry that uses a single analytical spectrum line, this method can be used to obtain a value which is closer to the standard value of national standard materials. The detection limit of this method is much lower than the standard value of the specification of testing quality management for geological laboratories. -
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表 1 分析谱线、参考线、分析谱线转换值和测试范围
Table 1. Table 1 Analytical line, reference line, conversion value and the measurement range of the method
待测元素 工作谱线(nm) 参考线(nm) 转换值(μg/g) 测试范围(μg/g) Ag 328.068 326.9494 - 0~0.5 338.289 326.9494 0.5 0.5~10 Sn 283.999 270.9626 8.5 8.5~100 317.502 326.9494 - 0~8.5 B 249.678 270.9626 80 80~500 249.773 270.9626 - 0~80 Mo 313.2594 326.9494 10 10~100 317.0347 326.9494 - 0~10 Pb 266.3166 270.9626 Δ Δ 280.1990 270.9626 30 30~600 283.3069 270.9626 - 0~30 注：“Δ”表示不使用该线，“-”表示在小于转换值使用该线。 
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表 2 转换值的使用对实验结果的影响
Table 2. Effect of conversion values on the analytical results of the method
待测元素 项目 GBW07427 GBW07304a GBW07301 GBW07303 GBW07448 GBW07457 GBW07105 GBW07107 GBW07307a GBW07358 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC 元素含量测定值（μg/g） △lgC Ag 认定值 0.067 - 0.22 - 0.048 - 0.59 - 0.05 - 0.13 - 0.04 - 0.047 - 1.2 - 0.14 - 多线测定 0.072 0.031 0.23 0.011 0.046 -0.019 0.56 -0.022 0.056 0.050 0.12 -0.028 0.046 0.064 0.043 -0.038 1.2 0.003 0.135 -0.014 328.068nm测定值 0.072 0.031 0.23 0.011 0.046 -0.019 0.55 -0.032 0.056 0.050 0.12 -0.028 0.046 0.064 0.043 -0.038 1.3 0.023 0.135 -0.014 338.289nm测定值 0.078 0.065 0.16 -0.148 0.026 -0.260 0.56 -0.022 0.061 0.087 0.11 -0.054 0.044 0.042 0.025 -0.280 1.2 0.003 0.129 -0.037 Snm测定值 认定值 3.3 - 4 - 3.1 - 3.4 - 2.3 - 8.7 - 2 - 2 - 2.5 - 2.5 - 多线测定 3.52 0.028 3.95 -0.005 3.22 0.017 3.47 0.009 2.97 0.111 8.88 0.009 2.53 0.102 2.16 0.033 2.36 -0.025 2.17 -0.061 317.502nm测定值 3.52 0.028 3.95 -0.005 3.22 0.017 3.47 0.009 2.97 0.111 9.24 0.026 2.66 0.124 2.16 0.033 2.36 -0.025 2.17 -0.061 283.999nm测定值 3.74 0.054 2.94 -0.134 3.47 0.049 3.33 -0.009 2.93 0.105 8.88 0.009 2.66 0.124 2.34 0.067 2.18 -0.060 2.17 -0.061 B 认定值 46 - 91 - 4.6 - 33 - 51 - 64 - 3.5 - 154 - 195 - 53 - 多线测定 51.7 0.051 87.1 -0.019 4.49 -0.010 37.0 0.049 48.7 -0.020 68.8 0.032 3.77 0.033 152 -0.006 202 0.016 57.9 0.038 249.773nm测定值 51.7 0.051 77.6 -0.069 4.49 -0.010 37.0 0.049 48.7 -0.020 68.8 0.032 3.77 0.033 137 -0.051 204 0.019 57.9 0.038 249.678nm测定值 52.5 0.057 87.1 -0.019 4.92 0.029 36.3 0.041 48.6 -0.021 81.5 0.105 4.77 0.135 152 -0.006 202 0.016 57.6 0.037 Mo 认定值 0.48 - 1.6 - 0.74 - 92 - 0.61 - 1.18 - 2.6 - 0.35 - 0.82 - 0.94 - 多线测定 0.49 0.011 1.63 0.007 0.67 -0.044 90.6 -0.007 0.63 0.012 1.02 -0.065 2.61 0.001 0.35 0.006 0.76 -0.031 0.91 -0.016 313.2594nm测定值 0.49 0.011 1.63 0.007 0.67 -0.044 79.2 -0.065 0.63 0.012 1.02 -0.065 3.33 0.108 0.35 0.006 0.76 -0.031 0.91 -0.016 317.0347nm测定值 0.45 -0.026 1.03 -0.190 0.63 -0.072 90.6 -0.007 0.55 -0.043 0.87 -0.130 2.61 0.001 0.57 0.213 0.67 -0.088 0.87 -0.033 Pb 认定值 21.6 - 68 - 24 - 40 - 18.7 - 61 - 7.2 - 8.7 - 555 - 210 - 多线测定 21.7 0.002 65.8 -0.014 27.5 0.060 38.7 -0.015 19.4 0.016 50.7 -0.080 7.83 0.036 7.77 -0.049 630 0.055 203 -0.015 283.3069nm测定值 21.7 0.002 58.3 -0.067 27.5 0.060 34.7 -0.061 19.4 0.016 50.1 -0.086 7.83 0.036 7.77 -0.049 474 -0.069 183 -0.060 280.199nm测定值 23.2 0.032 65.8 -0.014 28.0 0.067 38.7 -0.015 20.2 0.034 50.7 -0.080 8.34 0.064 9.99 0.060 630 0.055 203 -0.015
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表 3 方法检出限
Table 3. Detection limits of the method
待测元素 分次测定值(μg/g) 标准偏差(μg/g) 检出限(μg/g) Ag 0.017 0.016 0.019 0.02 0.021 0.016 0.003 0.0077 0.021 0.015 0.017 0.021 0.024 0.018 Sn 0.26 0.27 0.15 0.36 0.25 0.29 0.062 0.19 0.19 0.30 0.23 0.33 0.21 0.20 B 1.74 2.2 1.72 2.09 2.19 1.54 0.230 0.68 1.87 2.02 1.68 2.08 2.10 1.68 Mo 0.16 0.16 0.17 0.13 0.13 0.13 0.019 0.058 0.16 0.13 0.14 0.15 0.19 0.14 Pb 1.17 1.48 0.96 1.23 1.37 1.16 0.160 0.49 1.15 1.32 1.17 1.02 0.94 1.29
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表 4 方法精密度
Table 4. Precision tests of the method
待测元素 项目 GBW07302 GBW07309 GBW07312 GBW07364 GBW07403 GBW07451 GBW07452 GBW07454 GBW07103 Ag 含量平均值(μg/g) 0.060 0.085 1.10 0.13 0.086 0.069 0.072 0.078 0.035 标准偏差 0.0044 0.0040 0.040 0.0070 0.0046 0.0057 0.0047 0.0046 0.0033 RSD(%) 7.33 4.74 3.69 5.37 5.29 8.32 6.56 5.90 9.39 Sn 含量平均值(μg/g) 29.0 2.43 69.6 1.79 2.61 2.15 3.32 2.91 13.5 标准偏差 2.44 0.19 6.08 0.058 0.21 0.13 0.14 0.17 1.10 RSD(%) 7.76 7.93 8.66 3.23 7.62 6.18 4.10 5.91 8.17 B 含量平均值(μg/g) 10.4 55.3 24.0 37.1 22.1 52.0 76.4 50.9 20.7 标准偏差 0.63 2.52 1.66 2.69 1.57 3.83 4.31 3.58 1.66 RSD(%) 6.43 4.56 6.93 7.25 8.06 7.36 5.64 7.04 8.05 Mo 含量平均值(μg/g) 2.16 0.58 7.68 1.53 0.31 0.57 0.59 0.68 3.67 标准偏差 0.095 0.043 0.37 0.11 0.028 0.044 0.034 0.046 0.25 RSD(%) 4.40 7.41 4.79 7.41 9.17 7.77 5.85 6.82 6.94 Pb 含量平均值(μg/g) 40.6 23.4 295 26.1 27.1 25.6 25.8 22.5 33.1 标准偏差 1.82 1.30 19.68 1.50 1.51 1.13 0.86 0.84 1.68 RSD(%) 4.49 5.54 6.66 5.74 5.59 4.42 3.35 3.74 5.09
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表 5 方法准确度
Table 5. Accuracy tests of the method
标准物质编号 项目 Ag Sn B Mo Pb GBW07404 测定值(μg/g) 0.067 4.88 105 2.46 54.4 认定值(μg/g) 0.070 5.70 97.0 2.60 58.5 △logC -0.020 -0.067 0.033 -0.025 -0.032 GBW07405 测定值(μg/g) 3.6 15.5 65.5 4.28 498 认定值(μg/g) 4.4 17.7 53.0 4.60 552 △logC -0.085 -0.056 0.092 -0.032 -0.045 GBW07449 测定值(μg/g) 0.076 1.52 148 3.04 11.5 认定值(μg/g) 0.068 1.80 143 3.20 13.4 △logC 0.047 -0.073 0.015 -0.022 -0.066 GBW07453 测定值(μg/g) 0.090 6.08 81.9 1.12 45.1 认定值(μg/g) 0.092 6.20 83.0 1.10 40.0 △logC -0.008 -0.009 -0.006 0.009 0.052 GBW07457 测定值(μg/g) 0.12 8.63 77.1 1.14 54.0 认定值(μg/g) 0.13 8.70 80.0 1.18 61.0 △logC -0.038 -0.004 -0.016 -0.014 -0.053 GBW07301 测定值(μg/g) 0.046 3.28 4.92 0.68 20.6 认定值(μg/g) 0.048 3.10 4.60 0.74 24.4 △logC -0.023 0.024 0.029 -0.039 -0.073 GBW07303 测定值(μg/g) 0.66 2.93 38.6 95.1 35.7 认定值(μg/g) 0.59 3.40 33.0 92.0 40.0 △logC 0.047 -0.064 0.068 0.015 -0.049 GBW07311 测定值(μg/g) 2.8 343.2 66.5 6.05 644 认定值(μg/g) 3.2 370.0 68.0 5.90 636 △logC -0.051 -0.033 -0.010 0.011 0.006 GBW07302a 测定值(μg/g) 0.041 9.42 7.84 0.97 36.3 认定值(μg/g) 0.040 8.60 9.70 1.10 35.0 △logC 0.015 0.040 -0.092 -0.053 0.016 GBW07307a 测定值(μg/g) 1.2 2.11 176 0.69 511 认定值(μg/g) 1.2 2.50 195 0.82 555 △logC 0.008 -0.073 -0.045 -0.078 -0.036 GBW07103 测定值(μg/g) 0.032 15.3 23.8 3.40 35.1 认定值(μg/g) 0.033 12.5 24.0 3.50 31.0 △logC -0.009 0.087 -0.004 -0.013 0.054 GBW07106 测定值(μg/g) 0.068 1.40 37.4 0.85 10.4 认定值(μg/g) 0.062 1.10 34.0 0.76 7.60 △logC 0.037 0.104 0.042 0.050 0.137 GBW07108 测定值(μg/g) 0.041 1.11 17.9 0.37 18.0 认定值(μg/g) 0.043 0.98 16.0 0.38 18.3 △logC -0.021 0.054 0.050 -0.016 -0.008 GBW07111 测定值(μg/g) 0.054 1.55 3.31 0.60 19.1 认定值(μg/g) 0.066 1.44 3.92 0.47 19.8 △logC -0.086 0.033 -0.073 0.105 -0.015 GBW07122 测定值(μg/g) 0.060 0.88 10.1 0.18 8.82 认定值(μg/g) 0.050 0.80 12.0 0.16 9.00 △logC 0.079 0.042 -0.074 0.060 -0.009
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