Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique
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摘要:
快速检测地球化学样品中铜铅锌镍的含量可及时了解重金属污染情况，方便有效治理。本文采用固体进样技术，建立了交流电弧直读原子发射光谱同时测定地球化学样品中铜、铅、锌、镍的方法。以氟化钠、氧化铝、二氧化硅、碳粉为缓冲剂，锗为内标元素，优选了各元素分析线对，曝光时间分别为25s。采用国家一级标准物质对合成硅酸盐标准曲线进行校正从而降低基体干扰；同时选择灵敏线和次灵敏线两条分析谱线，不仅提高了准确度也扩大了元素可测定的线性范围；采用两次平行分析计算平均值进一步提高分析精度。方法检出限为铜0.45μg/g，铅1.46μg/g，锌2.40μg/g，镍1.58μg/g；精密度为铜1.36%~6.25%，铅1.17%~8.06%，锌1.64%~9.68%，镍0.91%~5.31%。采用该方法对土壤、沉积物、岩石国家一级标准物质进行分析，测定值与标准值一致，|△logC|均≤0.05，实际样品和外部质控样品测试合格率均在90%以上。本方法主要特点体现在：固体进样技术操作简单，相比酸溶处理后测定更加环保，同时避免了由试剂空白、器皿等带来的污染；采用两次摄谱计算平均强度，相比文献报道的单次分析的结果更加准确，分析精度更高，各项指标优于DZ/T 0130.5—2006中多目标地球化学调查（1：250000）规范要求。
Abstract:BACKGROUND The fast detection of Cu, Pb, Zn and Ni in geochemical samples helps to determine the level of heavy metal pollution, thus assisting in the employment of efficient treatments.
OBJECTIVES To establish a method for the simultaneous determination of Cu, Pb, Zn and Ni in geochemical samples by AC Arc direct reading atomic emission spectrometry with solid sampling technique.
METHODS With sodium fluoride, alumina, silicon dioxide and carbon powder as buffer agents and germanium as the internal standard element, the element analysis line pairs were optimized, and the exposure time was also optimized at 25s. The standard curve of synthetic silicate was corrected using national first-class reference materials (soil, rock and sediment), so as to reduce the interference of the matrix. Sensitive line and hyposensitive line were selected to enhance the accuracy as well as expand the measurable linear range of elements. Average value of two parallel analyses was adopted for further improved analytical precision.
RESULTS The detection limits of Cu, Pb, Zn and Ni were 0.45μg/g, 1.46μg/g, 2.40μg/g and 1.58μg/g, respectively. The precision ranges of the method were 1.36%-6.25% for Cu, 1.17%-8.06% for Pb, 1.64%-9.68% for Zn and 0.91%-5.31% for Ni. Measured values with this method for the national first-class reference materials of soil, sediment and rock were consistent with the certified values (|△logC| ≤ 0.05), qualification rates of the actual samples and external quality control samples were all above 90%.
CONCLUSIONS With simple operation, direct solid sampling technique is applied. The method reported here is more environmentally friendly compared to the acid dissolving method, sample contamination caused by reagent blank and vessels used is avoided at the same time. The average results of twice spectral acquisitions are calculated, which is more accurate and precise than the single analysis reported in the literature. All indicators of this method are better than the requirements of regulation (1:250000) DZ/T 0130.5-2006.
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Key words:
- geochemical samples /
- heavy metal elements /
- solid sampling /
- emission spectrometry
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表 1 分析谱线、内标线和方法测试范围
Table 1. Analytical lines, internal standard lines and measurement range of the method
元素 分析线
(nm)Ge内标线
(nm)测定范围
(μg/g)Pb 266.316 270.963 10~1000 Cu 282.437 270.963 50~1000 Cu 327.393 326.949 2~50 Zn 334.501 326.949 5~1000 Ni 341.476 326.949 2~200 
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表 2 标准曲线校正前后准确度结果比对
Table 2. Comparison of accuracy results for before and after calibration of standard curve
标准物质编号 Cu含量标准值
(μg/g)校正前 校正后 Pb含量标准值
(μg/g)校正前 校正后 Cu含量测定值
(μg/g)△logC Cu含量测定值
(μg/g)△logC Pb含量测定值
(μg/g)△logC Pb含量测定值
(μg/g)△logC GBW07403 11.4±1.6 10.6 -0.03 11.5 0.00 26.0±4.0 21.4 -0.08 26.7 0.01 GBW07404 40.0±4.0 47.1 0.07 41.0 0.01 58.0±7.0 55.4 -0.02 61.5 0.03 GBW07423 25.0±3.0 28.7 0.06 26.9 0.03 25.0±3.0 21.6 -0.06 26.9 0.03 GBW07430 32.0±2.0 33.5 0.02 30.7 -0.02 61.0±2.0 59.3 -0.01 65.2 0.03 GBW07448 16.0±0.5 17.0 0.03 17.2 0.03 18.7±0.9 16.9 -0.04 21.6 0.06 GBW07301a 28.0±2.0 30.9 0.04 28.6 0.01 31.0±4.0 25.4 -0.09 31.0 0.00 GBW07307a 22.5±1.0 24.5 0.04 23.5 0.02 555±19 670 0.08 549 0.00 GBW07331 44.0±1.3 44.7 0.01 39.2 -0.05 27.7±1.3 26.3 -0.02 31.9 0.06 GBW07311 79.0±4.0 88.0 0.05 85.4 0.03 636±34 759 0.08 612 -0.02 GBW07360 26.5±1.0 25.2 -0.02 24.1 -0.04 341±15 353 0.02 312 -0.04 标准物质编号 Zn含量标准值
(μg/g)校正前 校正后 Ni含量标准值
(μg/g)校正前 校正后 Zn含量测定值
(μg/g)△logC Zn含量测定值
(μg/g)△logC Ni含量测定值
(μg/g)△logC Ni含量测定值
(μg/g)△logC GBW07403 31.0±4.0 29.2 -0.03 35.7 0.06 12.0±2.7 11.8 -0.01 13.8 0.06 GBW07404 210±19 250 0.08 251 0.08 64.0±7.0 66.2 0.01 66.6 0.02 GBW07423 61.0±5.0 54.5 -0.05 63.0 0.01 33.0±3.0 32.8 0.00 35.0 0.03 GBW07430 100±8 97.2 -0.01 106 0.03 27.4±0.9 27.4 0.00 29.8 0.04 GBW07448 52.0±2.0 45.5 -0.06 53.5 0.01 21.0±1.0 22.5 0.03 24.9 0.07 GBW07301a 90.0±7.0 74.2 -0.08 83.3 -0.03 56.0±7.0 50.6 -0.04 52.1 -0.03 GBW07307a 780±19 934 0.08 829 0.03 22.0±0.6 22.1 0.00 24.5 0.05 GBW07331 77.1±2.7 64.4 -0.08 73.3 -0.02 37.2±1.4 30.9 -0.08 33.2 -0.05 GBW07311 373±21 363 -0.01 352 -0.02 14.3±1.5 15.1 0.02 17.3 0.08 GBW07360 579±17 561 -0.01 523 -0.04 14.4±0.7 12.4 -0.06 12.3 -0.07
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表 3 方法检出限
Table 3. Detection limits of the method
元素 12次平行分析测定值
(μg/g)标准偏差
(μg/g)检出限
(3s, μg/g)1∶25万规范要求DZ/T 0130.5—2006
(μg/g)
Cu0.55 0.94 0.89 0.67
0.60 0.80 0.52 0.88
0.63 0.86 0.95 0.770.15 0.45 1.00
Pb3.13 2.51 3.81 3.19
3.68 2.94 2.78 3.21
2.19 2.75 3.54 2.660.49 1.46 2.00
Zn3.33 1.56 1.68 2.00
3.16 1.63 2.82 3.95
3.07 1.77 2.84 3.020.80 2.40 4.00
Ni2.04 1.97 0.27 1.78
2.11 1.57 1.89 1.66
2.27 2.09 2.08 2.080.53 1.58 2.00
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表 4 方法准确度和精密度
Table 4. Accuracy and precision tests of the method
元素 项目 GBW07402 GBW07403 GBW07404 GBW07423 GBW07426 GBW07361 GBW07311 GBW07360 GBW07365 GBW07366 GBW07104 Cu 平均值(μg/g) 16.0 11.7 42.0 27.5 27.8 4.04 84.0 24.6 23.2 467 54.7 标准值(μg/g) 16.3±1.4 11.4±1.6 40.0±4.0 25.0±3.0 29.0±1.0 3.90±0.60 79.0±4.0 26.5±1.0 22.6±0.8 483±20 55.0±4.0 |△logC| 0.01 0.01 0.02 0.04 0.02 0.01 0.03 0.03 0.01 0.01 0.00 RSD(%) 1.36 1.76 4.50 2.05 6.25 3.18 1.97 1.39 1.53 3.90 2.72 Pb 平均值(μg/g) 20.9 27.2 62.4 27.4 20.2 22.8 615 343 18.7 129 11.4 标准值(μg/g) 20.0±4.0 26.0±4.0 58.0±7.0 25.0±3.0 19.0±2.0 22.0±1.0 636±34 341±15 17.0±1.0 126±5 11.3±1.8 |△logC| 0.02 0.02 0.03 0.04 0.03 0.02 0.01 0.00 0.04 0.01 0.00 RSD(%) 5.44 8.06 4.79 5.69 3.89 5.81 1.22 1.17 3.14 2.09 1.38 Zn 平均值(μg/g) 38.4 33.8 229 62.6 77.2 20.4 348 525 61.5 912 64.9 标准值(μg/g) 42.0±5.0 31.0±4.0 210±19 61.0±5.0 78.0±5.0 19.0±2.0 373±21 579±17 59.0±2.0 874±19 71.0±7.0 |△logC| 0.04 0.04 0.04 0.01 0.00 0.03 0.03 0.04 0.02 0.02 0.04 RSD(%) 5.08 9.68 1.64 6.51 8.81 2.28 7.34 3.52 6.70 3.60 3.60 Ni 平均值(μg/g) 20.9 12.5 67.5 35.4 34.1 5.22 13.7 15.4 24.5 29.4 17.5 标准值(μg/g) 19.4±1.9 12.0±2.7 64.0±7.0 33.0±3.0 32.0±1.0 4.70±0.50 14.3±1.5 14.4±0.7 26.0±2.0 29.0±1.0 17.0±2.0 |△logC| 0.03 0.02 0.02 0.03 0.03 0.05 0.02 0.03 0.03 0.01 0.01 RSD(%) 2.98 1.75 1.43 1.00 0.91 5.31 4.36 3.66 1.14 4.01 3.64
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