X射线荧光光谱法测定石灰石中多组分含量

doi:10.13228/j.issn.1000-7571.2014.09.008

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摘要采用粉末压片法制样,建立了X射线荧光光谱法测定石灰石中10种组分(CaO、SiO₂、MgO、Fe₂O₃、Al₂O₃、MnO、TiO₂、K₂O、Na₂O、SrO)含量的方法。通过试验确定石灰石样品粒度达到74 μm以下,3.00 g样品称样量,30 t压力压片的制样条件。试验发现,压片时利用硼酸镶边和硼酸衬底,不另外添加粘结剂可解决样品粘结问题;利用经验α系数法校正基体效应,校正后校准曲线的离散度较小,有效地消除了重叠谱线干扰。各组分的检出限在0.47~188.08 μg/g之间。对石灰石试样进行精密度考察,各组分含量的相对标准偏差(RSD)在0.042%~5.7%范围内;对石灰石标准样品进行分析,各组分的测定值与认定值相符。方法满足进出口商品检验工作对效率和准确度的要求。

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关键词 ： X射线荧光光谱法, 石灰石, 压片制样, 多组分

Abstract：Ten components in limestone (CaO, SiO₂, MgO,Fe₂O₃, Al₂O₃, MnO, TiO₂, K₂O, Na₂O, SrO) were determined by X-ray fluorescence spectrometry with pressed powder pellet. Through experiment, it was determined that the sample should be prepared under the pressure of 30 t with 3.00 g of limestone sample, whose granularity was below 74 μm. It was found that, by using boric acid for edge and substrate during sample pressing, the sample bonding problem could be solved without bonding agent; By using empirical α coefficient method for correcting matrix effect, the dispersion of the calibration curve after correction was relatively small, which indicated the interference from overlapping lines was effectively eliminated. The detection limit of the testing components was in the range of 0.47-188.08 μg/g. Precision test was conducted on limestone sample. The relative standard deviation (RSD) was within 0.042%-5.7%. The limestone certified reference material was analyzed by the proposed method, and the results were consistent with the certified values. The proposed method could satisfy the requirements for efficiency and accuracy of entry-exit inspection.

Key words： X-ray fluorescence spectrometry limestone pressed powder pellet multi-components

收稿日期: 2014-02-19

ZTFLH:	O657.34
	P619.26+3

通讯作者: 徐金龙(1976-),男,高级工程师,硕士,主要从事化矿金检测分析及质量控制工作;E-mail:xujinlongccc@163.com E-mail: lvshansheng@126.com

作者简介: 吕善胜(1982-),男,工程师,主要从事X射线荧光光谱分析工作;E-mail:lvshansheng@126.com

引用本文:

吕善胜,徐金龙,田琼,洪武兴,史亚晓. X射线荧光光谱法测定石灰石中多组分含量[J]. 冶金分析, 2014, 34(9): 39-42. LÜ Shan-sheng, XU Jin-long,TIAN Qiong, HONG Wu-xing, SHI Ya-xiao. Determination of multi-components in limestone by X-ray fluorescence spectrometry. , 2014, 34(9): 39-42.

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http://47.93.29.245/Jweb_yjfx/CN/10.13228/j.issn.1000-7571.2014.09.008 或 http://47.93.29.245/Jweb_yjfx/CN/Y2014/V34/I9/39

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