交流电弧发射光谱法测定铅矿石中锡

doi:10.13228/j.boyuan.issn1000-7571.011898

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摘要准确、快速测定铅矿石中锡,对矿产资源的综合利用具有十分重要的意义。实验采用交流电弧发射光谱法测定铅矿石中锡。以二氧化硅、氟化铝、氟化钠、碳为缓冲剂,锗为内标元素,优选了锡元素分析线对,曝光时间为22 s;采用氧化铅光谱纯物质与合成硅酸盐标准物质按不同比例混合来建立校准曲线,从而降低由基体差异引入的误差;选择干扰少、灵敏度高的Sn I 283.998 nm作为分析线,采用两点差值法背景校正扣除PbⅠ283.306 nm尾峰对SnⅠ283.998 nm的干扰。方法中锡的检出限为0.13 μg/g,定量限为0.43 μg/g。按照实验方法测定铅矿石国家一级标准物质和铅矿石样品中锡,结果的相对标准偏差(RSD,n=12)为3.9%~5.6%,相对误差(RE)为-2.81%~4.63%,精密度和正确度结果均满足地质矿产行业标准DZ/T 0130.3—2006的技术要求。

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	马景治
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	董学林

关键词 ：交流电弧发射光谱法, 铅矿石, 锡, 两点差值法

Abstract：The accurate and rapid determination of tin in lead ore is of great significance to the comprehensive utilization of mineral resources. AC arc emission spectrometry was employed to determine the tin content in lead ore. Silicon dioxide, aluminum fluoride, sodium fluoride and carbon powder were used as buffers, and germanium was selected as the internal standard element. The analytical line pairs of tin were optimized. The exposure time was 22 s. The standard curve was established by mixing the pure lead oxide spectral material and the synthetic silicate standard material in different proportions, so as to reduce the error caused by the matrix difference. Sn Ⅰ 283.998 nm with little interference and high sensitivity was selected as the analytical line. The interference of tail peak of Pb Ⅰ 283.306 nm on Sn Ⅰ 283.998 nm was deducted by background correction of twofic-point difference method. The limit of detection (LOD) was 0.13 μg/g, and the limit of quantification (LOQ) was 0.43 μg/g. The proposed method was used to analyze the tin content in national first-class reference material and actual sample of lead ore. The relative standard deviations (RSD, n=12) of determination results were between 3.9% and 5.6%. The relative error (RE) ranged from -2.81% to 4.63%. The precision and trueness of the method could meet the technical requirements of the geological and mineral industry standard DZ/T 0130.3-2006.

Key words： AC arc emission spectrometry lead ore tin two-point difference method

收稿日期: 2022-05-30

ZTFLH:	O657.31
	TF03+1
	TF041

基金资助:国家重点研发计划项目(2021YFC2903002)

作者简介: 马景治(1989—),男,工程师,硕士,从事地质样品中无机元素分析方法研究;E-mail:cugedu@163.ccom

引用本文:

马景治, 李光一, 董学兵, 李策, 董学林. 交流电弧发射光谱法测定铅矿石中锡[J]. 冶金分析, 2023, 43(2): 39-45. MA Jingzhi, LI Guangyi, DONG Xuebing, LI Ce, DONG Xuelin. Determination of tin in lead ore by AC arc emission spectrometry. , 2023, 43(2): 39-45.

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