X射线荧光光谱法测定地质样品中的硫和氟
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摘要
采用粉末压片制样-X射线荧光光谱法研究地质样品中硫(S)和氟(F)元素的快速测定方法。通过分级过筛实验优化确定样品粒度,探讨样品粒度对测定结果的影响,并进行实际样品和标准物质验证。结果显示,样品粒度为85μm时,经实际样品和标准物质验证,测定结果与化学值和标准认定值相符,且相对标准偏差(RSD)均小于2%。方法具有准确度高、检出限好、测试范围宽、简便快速等优点,能确保样品分析结果的准确性,实现了地质样品中S和F的快速测定。
The rapid determination method of sulphur and fluorine in geological samples by X-ray fluorescence spectrometry with pressed powder preparation was studied.The particle size of the sample was optimized by the sieving experiment,and the effect of the sample particle size on the determination results was discussed.The results show that verified by actual samples and standard substances,the measured results were consistent with the chemical values and the standard values,and the relative standard deviation(RSD)was less than 2%,when the sample size was 85μm.The method has the advantages of high accuracy,good detection limit,wide test range,simple and rapid,etc.,which can ensure the accuracy of sample analysis results and realize the rapid determination of S and F in geological samples.
The rapid determination method of sulphur and fluorine in geological samples by X-ray fluorescence spectrometry with pressed powder preparation was studied.The particle size of the sample was optimized by the sieving experiment,and the effect of the sample particle size on the determination results was discussed.The results show that verified by actual samples and standard substances,the measured results were consistent with the chemical values and the standard values,and the relative standard deviation(RSD)was less than 2%,when the sample size was 85μm.The method has the advantages of high accuracy,good detection limit,wide test range,simple and rapid,etc.,which can ensure the accuracy of sample analysis results and realize the rapid determination of S and F in geological samples.
引文
[1]全国国土资源标准化技术委员会.硅酸盐岩石岩石化学分析方法第12部分:氟量测定:GB/T14506.12-2010[S].北京:中国标准出版社,2010.
[2]贺攀红,荣耀,连福龙,等.X射线荧光光谱法快速测定地质样品中的钼[J].分析测试技术与仪器(Analysis and Testing Technology and Instruments),2012,18(4):):213-216.
[3]周伟,曾梦,王建,等.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试((Rock and Mineral Analysis),2018,37(3):298-305.
[4]李迎春,周伟,王健,等.X射线荧光光谱法测定高锶高钡的硅酸盐样品中的主量元素[J].岩矿测试(Rock and Mineral Analysis),2013,32(2):249-253.
[5]袁家义,白雪冰,王卿,等.X射线荧光光谱法测定地质样品中的氯和硫[J].岩矿测试(Rock and Mineral Analysis),2004,23(3):225-227.
[6]王祎亚,詹秀春,潘兴涛,等.粉末压片-X射线荧光光谱法测定地质样品中痕量硫的矿物效应佐证实验及其应用[J].冶金分析(Metallurgical Analysis),2010,30(1):7-11.
[7]沈春春.探析痕量硫的X射线荧光光谱法测定[J].化工时刊(Chemical Industry Times),2016,30(5):29-31.
[8]吴超超,马秀艳,邢文清,等.熔融制样-X射线荧光光谱法测定萤石中主次组分[J].冶金分析(Metallurgical Analysis),2017,37(4):42-47.
[9]唐梦奇,刘顺琼,袁焕明,等.粉末压片制样-波长色散X射线荧光光谱法测定进口铜矿石中的氟[J].岩矿测试(Rock and Mineral Analysis),2013,32(2):254-257.
[10]袁建,夏晨光,刘高辉,等.X射线荧光光谱法测定高氟地质样品中氟、钙等元素[J].铀矿地质(Uranium Geology),32(3):175-179.
[11]张勤,李国会,潘守忠,等.X射线荧光光谱法测定土壤和水系沉积物等样品中碳、氮、氟、氯、硫、溴等42种主次和痕量元素[J].分析实验室(Chinese Journal of Analysis Laboratory),2008,27(11):51-57.
[12]全国国土资源标准化技术委员会地质矿产实验室测试分技术委员会.地质矿产实验室质量管理规范第2部分:岩石矿物分析试样制备:DZ/T0130-2006[S].北京:中国标准出版社,2006.
[2]贺攀红,荣耀,连福龙,等.X射线荧光光谱法快速测定地质样品中的钼[J].分析测试技术与仪器(Analysis and Testing Technology and Instruments),2012,18(4):):213-216.
[3]周伟,曾梦,王建,等.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试((Rock and Mineral Analysis),2018,37(3):298-305.
[4]李迎春,周伟,王健,等.X射线荧光光谱法测定高锶高钡的硅酸盐样品中的主量元素[J].岩矿测试(Rock and Mineral Analysis),2013,32(2):249-253.
[5]袁家义,白雪冰,王卿,等.X射线荧光光谱法测定地质样品中的氯和硫[J].岩矿测试(Rock and Mineral Analysis),2004,23(3):225-227.
[6]王祎亚,詹秀春,潘兴涛,等.粉末压片-X射线荧光光谱法测定地质样品中痕量硫的矿物效应佐证实验及其应用[J].冶金分析(Metallurgical Analysis),2010,30(1):7-11.
[7]沈春春.探析痕量硫的X射线荧光光谱法测定[J].化工时刊(Chemical Industry Times),2016,30(5):29-31.
[8]吴超超,马秀艳,邢文清,等.熔融制样-X射线荧光光谱法测定萤石中主次组分[J].冶金分析(Metallurgical Analysis),2017,37(4):42-47.
[9]唐梦奇,刘顺琼,袁焕明,等.粉末压片制样-波长色散X射线荧光光谱法测定进口铜矿石中的氟[J].岩矿测试(Rock and Mineral Analysis),2013,32(2):254-257.
[10]袁建,夏晨光,刘高辉,等.X射线荧光光谱法测定高氟地质样品中氟、钙等元素[J].铀矿地质(Uranium Geology),32(3):175-179.
[11]张勤,李国会,潘守忠,等.X射线荧光光谱法测定土壤和水系沉积物等样品中碳、氮、氟、氯、硫、溴等42种主次和痕量元素[J].分析实验室(Chinese Journal of Analysis Laboratory),2008,27(11):51-57.
[12]全国国土资源标准化技术委员会地质矿产实验室测试分技术委员会.地质矿产实验室质量管理规范第2部分:岩石矿物分析试样制备:DZ/T0130-2006[S].北京:中国标准出版社,2006.