直读发射光谱法测定银硼钼锡铅的载体缓冲剂研究
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摘要
研究推荐以Al_2O_3、K_2S_2O_7、SiO_2、BaCO_3、NaF、S、CaCO_3、Fe_2O_3为主要组分的载体缓冲剂,通过与地球化学样品中待测元素发生热化学反应生成氟化物、硫化物确保其蒸发浓集率,与样品基体生成难以挥发的硅铝酸盐降低其干扰程度。在此基础上建立了直读光谱快速测定Ag、B、Mo、Sn、Pb的单电极载体蒸馏法,采用国家一级标准物质校准工作曲线及分析结果的量值溯源,检出限分别为Ag 0.006μg/g、B 0.84μg/g、Mo 0.08μg/g、Sn 0.19μg/g、Pb 0.59μg/g,待测元素结果的精密度≤8.14%、准确度≤0.089,满足多目标地球化学调查、生态地球化学评价等要求。
Carrier buffer with Al_2O_3,K_2S_2O_7,SiO_2,BaCO_3,Na F,S,CaCO_3,Fe_2O_3 as its main composition,as is recommended by the study,ensures the vaporization concentration of target elements by having thermochemical reaction with them that produces fluoride and sulfide,and mitigates the interference of the sample matrix by reacting with it and producing aluminosilicate.Based on that,the experiment established single electrode distillation method with direct reading emission spectrometry rapidly determining Ag,B,Mo,Sn and Pb,uses national GradeⅠnational reference material to calibrate the working curve,and carried out tracibility of values.The method has a detection limit of 0.006 μg/g for Ag,0.84 μg/g for B,0.08 μg/g for Mo,0.19 μg/g for Sn and 0.59 μg/g for Pb,the precision of determination results is ≤8.14 % and the accuracy≤0.089,meeting the requirement of multi-target geochemical investigation and ecological geochemical evaluation.
Carrier buffer with Al_2O_3,K_2S_2O_7,SiO_2,BaCO_3,Na F,S,CaCO_3,Fe_2O_3 as its main composition,as is recommended by the study,ensures the vaporization concentration of target elements by having thermochemical reaction with them that produces fluoride and sulfide,and mitigates the interference of the sample matrix by reacting with it and producing aluminosilicate.Based on that,the experiment established single electrode distillation method with direct reading emission spectrometry rapidly determining Ag,B,Mo,Sn and Pb,uses national GradeⅠnational reference material to calibrate the working curve,and carried out tracibility of values.The method has a detection limit of 0.006 μg/g for Ag,0.84 μg/g for B,0.08 μg/g for Mo,0.19 μg/g for Sn and 0.59 μg/g for Pb,the precision of determination results is ≤8.14 % and the accuracy≤0.089,meeting the requirement of multi-target geochemical investigation and ecological geochemical evaluation.
引文
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[2]叶家瑜,张蕾.多目标地球化学勘查样品分析方法配套方案[J].地质通报,2006,25(6):241-244.
[3]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铅[J].岩矿测试,2006,25(4):323-326.
[4]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,2004:78-85.
[5]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.
[6]叶晨亮.发射光谱法快速测定银锡铜铅锌钼铍[J].岩矿测试,2004,23(3):238-240.
[7]张文华,张芳.发射光谱法测定碳酸盐岩石样品中8个痕量元素[J].岩矿测试,1995,14(1):37-40.
[8]姚建贞,郝志红,唐瑞玲,等.固体发射光谱测定地球化学样品中的高含量锡[J].光谱学与光谱分析,2013,33(11):3 124-3 127.
[9]俞晓峰,李锐,寿淼钧,等.E5000型全谱直读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.
[10]郝志红,姚建贞,唐瑞玲,等.直流电弧全谱直读原子发射光谱法测定地球化学样品中痕量硼钼银锡铅的方法研究[J].光谱学与光谱分析,2015,35(2):527-533.
[11]赵质远.Prodigy-直流电弧法直接测定地质样品中银锡硼等痕量元素[J].岩矿测试,2012,31(5):922-923.
[12]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.