固体粉末进样交流电弧法测定区域地球化学调查样品中痕量银、硼、锡、铅
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摘要
采用固体粉末进样交流电弧法测定区域地球化学调查样品中的痕量银、硼、锡、铅。对实验条件进行了优化,激发电流为14 A,曝光时间为40 s。选择内标元素为锗,银、硼、锡、铅的分析线波长分别为328.07,249.77,283.99,283.31 nm;内标线波长分别为303.91,270.96,270.96,270.96 nm。分别在含量0.05~3,10~140,1~50,10~100μg/g范围内,银、硼、锡、铅含量的对数与分析线、内标线的黑度差呈良好的线性关系,相关系数分别为0.998 2,0.998 8,0.999 6,0.999 0,检出限分别为0.01,1.1,0.2,0.7μg/g。用所建方法对土壤成分分析标准物质GBW07446,GBW 07453和水系沉积物成分分析标准物质GBW 07302a,GBW 07303a,GBW 07304a进行测试,银、硼、锡、铅的测定值与标准值的对数差分别为–0.007~0.024,–0.031~–0.013,0.000~0.029,0.002~0.028,测定结果的相对标准偏差分别为7.3%~9.3%,6.0%~9.9%,6.5%~9.0%,6.5%~9.9%(n=12)。该方法操作简单、快速,环境友好,适合于区域地球化学调查样品中痕量银、硼、锡、铅的分析。
Solid powder sample AC arc method was applied to the determination of trace Ag, B, Sn and Pb in regional geochemical survey samples. The optimized conditions found were as follows: excitation current was 14 A, exposure time was 40 s. The internal standard element was Ge. The wavelength of the analytical lines of Ag, B, Sn, Pb was 328.07, 249.77, 283.99, 283.31 nm, and the internal line wavelength was 303.91, 270.96, 270.96, 270.96 nm, respectively. Logarithm of Ag, B, Sn, Pb mass fraction was linear with the difference of blackness in the range of 0.05–3,10–140, 1–50, 10–100 μg/g, respectively, the correlation coefficients were 0.998 2, 0.998 8, 0.999 6, 0.999 0, and detection limits were 0.01,1.1,0.2,0.7μg/g, respectively. Certified reference materials for the chemical composition of soil(GBW 07446, GBW 07453) and stream sediment(GBW 07302 a, GBW 07303 a, GBW 07304 a) were tested by the method. The logarithmic difference of results and the certified values for Ag,B,Sn, Pb was –0.007–0.024, –0.031– –0.013, 0.000–0.029, 0.002–0.028, respectively, and the relative standard deviations were 7.3%–9.3%, 6.0%–9.9%, 6.5%–9.0%, 6.5%–9.9%(n=12), respectively. The method is simple, rapid and environmentally friendly, it is suitable for the analysis of trace Ag, B, Sn and Pb in regional geochemical survey samples.
Solid powder sample AC arc method was applied to the determination of trace Ag, B, Sn and Pb in regional geochemical survey samples. The optimized conditions found were as follows: excitation current was 14 A, exposure time was 40 s. The internal standard element was Ge. The wavelength of the analytical lines of Ag, B, Sn, Pb was 328.07, 249.77, 283.99, 283.31 nm, and the internal line wavelength was 303.91, 270.96, 270.96, 270.96 nm, respectively. Logarithm of Ag, B, Sn, Pb mass fraction was linear with the difference of blackness in the range of 0.05–3,10–140, 1–50, 10–100 μg/g, respectively, the correlation coefficients were 0.998 2, 0.998 8, 0.999 6, 0.999 0, and detection limits were 0.01,1.1,0.2,0.7μg/g, respectively. Certified reference materials for the chemical composition of soil(GBW 07446, GBW 07453) and stream sediment(GBW 07302 a, GBW 07303 a, GBW 07304 a) were tested by the method. The logarithmic difference of results and the certified values for Ag,B,Sn, Pb was –0.007–0.024, –0.031– –0.013, 0.000–0.029, 0.002–0.028, respectively, and the relative standard deviations were 7.3%–9.3%, 6.0%–9.9%, 6.5%–9.0%, 6.5%–9.9%(n=12), respectively. The method is simple, rapid and environmentally friendly, it is suitable for the analysis of trace Ag, B, Sn and Pb in regional geochemical survey samples.
引文
[1]张雪梅,张勤.发射光谱法测定勘查地球化学样品中银硼锡钼[J].岩矿测试,2006,25(4):323–326.
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[12]程加伟.发射光谱法测定岩石化探样品中银等10个元素[J].地质实验室,1995,11(1):21–24.
[13]李滦宁,赵淑杰,王烨.发射光谱载体蒸馏法测定地质样品中微量硼铍锡银[J].岩矿测试,2004,23(1):31–36.
[14]张文华,王彦东,吴冬梅,等.交流电弧直读光谱法快速测定地球化学样品中的银、锡、硼、钼、铅[J].中国无机分析化学,2013,3(4):16–19.
[15]俞晓峰,李锐,寿淼钧,等.E5000型全谱直读型电弧发射光谱仪研制及其在地球化学样品分析中应用[J].岩矿测试,2015,34(1):40–47.
[16]叶家瑜,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:298–302.
[17]DZ/T 0130.4–2006地质矿产实验室测试质量管理规范[S].
[2]胡跃波,石亚萍,李蓓,等.交流电弧原子发射光谱法测定地质样品中的微量银[J].理化检验(化学分册):2015,51(10):1 414–1 417.
[3]刘江斌,武永芝.原子发射光谱法快速测定矿石中锡[J].冶金分析,2013,33(3):65–68.
[4]熊艳.深孔电极载体蒸馏光谱法测定化探样品中八个易挥发元素[J].岩矿测试,2007,26(5):425–427.
[5]王辉,马晓敏,郑伟,等.直流电弧原子发射光谱法测定钛和钛合金中微量杂质元素[J].岩矿测试,2014,33(4):506–511.
[6]曹成东,魏轶,刘江斌.发射光谱法同时测定地球化学样品中微量银铍硼锡铋钼[J].岩矿测试,2010,29(4):458–460.
[7]余宇,和振云,毛振才,等.交流电弧发射光谱的不同灵敏度谱线测定锡[J].岩矿测试,2013,32(1):44–47.
[8]刘薇.原子发射光谱法直接测定独居石矿物中钇组稀土元素[J].岩矿测试,2010,29(6):687–690.
[9]丁春霞,王琳,孙慧莹,等.发射光谱法测定生态地球化学调查样品中的银锡硼[J].黄金,2012,33(10):55–58.
[10]杨胜科,张文英.平头电极发射光谱分析法测定化探样品中痕量银的研究[J].西北地质,1995,16(4):81–83.
[11]许晓洁,付军刚,贾喜英.发射光谱法测定化探样品中银锡铅硼[J].西部探矿工程,2002,14(5):74–75.
[12]程加伟.发射光谱法测定岩石化探样品中银等10个元素[J].地质实验室,1995,11(1):21–24.
[13]李滦宁,赵淑杰,王烨.发射光谱载体蒸馏法测定地质样品中微量硼铍锡银[J].岩矿测试,2004,23(1):31–36.
[14]张文华,王彦东,吴冬梅,等.交流电弧直读光谱法快速测定地球化学样品中的银、锡、硼、钼、铅[J].中国无机分析化学,2013,3(4):16–19.
[15]俞晓峰,李锐,寿淼钧,等.E5000型全谱直读型电弧发射光谱仪研制及其在地球化学样品分析中应用[J].岩矿测试,2015,34(1):40–47.
[16]叶家瑜,江宝林.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004:298–302.
[17]DZ/T 0130.4–2006地质矿产实验室测试质量管理规范[S].