中国地质学会岩矿测试技术专业委员会、国家地质实验测试中心主办

固体进样-发射光谱法同时测定地球化学样品中铜铅锌镍

马景治, 曲少鹏, 李光一, 董学兵, 吴萌, 吴俊, 李策, 董学林. 固体进样-发射光谱法同时测定地球化学样品中铜铅锌镍[J]. 岩矿测试, 2022, 41(6): 1007-1016. doi: 10.15898/j.cnki.11-2131/td.202202230030
引用本文: 马景治, 曲少鹏, 李光一, 董学兵, 吴萌, 吴俊, 李策, 董学林. 固体进样-发射光谱法同时测定地球化学样品中铜铅锌镍[J]. 岩矿测试, 2022, 41(6): 1007-1016. doi: 10.15898/j.cnki.11-2131/td.202202230030
MA Jingzhi, QU Shaopeng, LI Guangyi, DONG Xuebing, WU Meng, WU Jun, LI Ce, DONG Xuelin. Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique[J]. Rock and Mineral Analysis, 2022, 41(6): 1007-1016. doi: 10.15898/j.cnki.11-2131/td.202202230030
Citation: MA Jingzhi, QU Shaopeng, LI Guangyi, DONG Xuebing, WU Meng, WU Jun, LI Ce, DONG Xuelin. Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique[J]. Rock and Mineral Analysis, 2022, 41(6): 1007-1016. doi: 10.15898/j.cnki.11-2131/td.202202230030

固体进样-发射光谱法同时测定地球化学样品中铜铅锌镍

  • 基金项目:
    国家重点研发计划项目(2021YFC2903002);湖北省地质局科技项目(KJ2021-17)
详细信息
    作者简介: 马景治,硕士,工程师,从事地质样品中无机元素分析方法研究。E-mail:cugedu@163.com
    通讯作者: 董学林,博士,高级工程师,从事地质样品测试技术及环境污染物检测工作。E-mail:dongxlin109@126.com
  • 中图分类号: O657.31

Simultaneous Determination of Copper, Lead, Zinc and Nickel in Geochemical Samples by Emission Spectrometry with Solid Sampling Technique

More Information
  • 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。

  • 加载中
  • 图 1  元素蒸发曲线

    Figure 1. 

    图 2  累计光强随曝光时间的变化趋势

    Figure 2. 

    图 3  单次和双次分析性能比较

    Figure 3. 

    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
    下载: 导出CSV

    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
    下载: 导出CSV

    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)

    Cu
    0.55  0.94  0.89  0.67
    0.60  0.80  0.52  0.88
    0.63  0.86  0.95  0.77
    0.15 0.45 1.00

    Pb
    3.13  2.51  3.81  3.19
    3.68  2.94  2.78  3.21
    2.19  2.75  3.54  2.66
    0.49 1.46 2.00

    Zn
    3.33  1.56  1.68  2.00
    3.16  1.63  2.82  3.95
    3.07  1.77  2.84  3.02
    0.80 2.40 4.00

    Ni
    2.04  1.97  0.27  1.78
    2.11  1.57  1.89  1.66
    2.27  2.09  2.08  2.08
    0.53 1.58 2.00
    下载: 导出CSV

    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
    下载: 导出CSV
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出版历程
收稿日期:  2022-02-23
修回日期:  2022-04-01
录用日期:  2022-04-30
刊出日期:  2022-11-28

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