Determination of 18 Components in Titanium Ores by X-Ray Fluorescence Spectrometry with Sample Preparation of Tablet Compression Method and Fusion Tablet Method
摘 要
为了克服基体效应和矿物效应对钛矿石样品中18种主、痕量组分测定的干扰,采用压片机在1 500 kN压力下将样品压制成片,用X射线荧光光谱法(XRF)测定压片中的10种痕量组分(磷、镓、铬、钒、硫、铷、锶、锰、锌和锆);按质量比20∶1将混合熔剂(四硼酸锂和偏硼酸锂的质量比为2∶1)和样品混合,在1 050℃条件下熔融制样,用XRF测定熔融片中的8种主量组分(三氧化二铁、二氧化钛、二氧化硅、三氧化二铝、氧化钙、氧化镁、氧化钾和氧化钠)。采用6种标准物质混合配制24个具有一定含量梯度的校准样品,用于绘制校准曲线。以经验系数法校正谱线重叠效应,用理论α系数法、康普顿散射内标法校正基体效应,用钴内标法校正铁的基体吸收效应。结果表明:经过综合校正公式校正后,18种组分的校准曲线的线性相关系数均大于0.996 0。3个未知样品的测定结果和文献中报道的碱熔法的相一致。10种痕量组分的检出限(3s)为1.2~21 mg·kg-1,8种主量组分的检出限(3s)为0.015%~0.66%。方法用于分析标准物质的10个平行样,得到痕量组分测定值的相对标准偏差(RSD)为0.21%~11%;主量组分测定值的RSD为0.22%~0.99%。
Abstract
In order to overcome the interference of matrix effect and mineral effect on determination of 18 major and trace components in titanium ore samples, the samples were pressed into tablet at 1 500 kN for analysis of 10 trace components (phosphorus, gallium, chromium, vanadium, sulfur, rubidium, strontium, manganese, zinc and zirconium) by XRF, and the mixture flux (composed of lithium tetraborate and lithium metaborate at a mass ratio of 2:1) together with the sample at a mass ratio of 20:1 were mixed and melted to a fused bead at 1 050℃ for analysis of 8 major components (iron trioxide, titanium dioxide, silica oxide, aluminum trioxide, calcium oxide, magnesium oxide, potassium oxide and sodium oxide) by XRF. 24 calibration samples in a certain content gradient were prepared by using a mixture of six standard materials, thus to make the calibration curves. Spectral line overlap was corrected by empirical coefficient method. Matrix effect was corrected by theoretical α coefficient method and compton scattering internal standard method. The matrix absorption effect of iron was corrected by cobalt internal standard method. The results showed that after correction of comprehensive correction formula, the linear correlation coefficients of 18 components were all greater than 0.996 0. Three unknown samples were determined by this method, giving results consistent with alkali melting method. Detection limits (3s) of 10 trace and 8 major components were 1.2-21 mg·kg-1 and 0.015%-0.66% respectively. 10 parallel samples of standard material were analyzed by the above method, giving results of RSDs (n=10) of trace components in the range of 0.21%-11% and of major components in the range of 0.22%-0.99%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202011009
所属栏目 工作简报
基金项目 典型矿产标准物质研制(2016YFF020110309)
收稿日期 2019/12/25
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备注李小莉,教授级高级工程师,主要从事X射线荧光光谱分析及分析方法的建立
引用该论文: LI Xiaoli,LIU Bin,XU Jinli,PAN Hanjiang,PAN Yanshan. Determination of 18 Components in Titanium Ores by X-Ray Fluorescence Spectrometry with Sample Preparation of Tablet Compression Method and Fusion Tablet Method[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(11): 1188~1192
李小莉,刘斌,徐进力,潘含江,潘宴山. 压片法和熔融片法制样-X射线荧光光谱法测定钛矿石中的18种组分[J]. 理化检验-化学分册, 2020, 56(11): 1188~1192
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参考文献
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【2】袁家义,吕振生,姜云.X射线荧光光谱熔融制样法测定钛铁矿中主次量组分[J].岩矿测试, 2007,26(2):158-162.
【3】朱忠平,李国会.熔融制样-X射线荧光光谱法测定钛铁矿中主次组分[J].冶金分析, 2013,33(6):32-36.
【4】罗明荣,陈文静.X射线荧光光谱法测定还原钛铁矿中11种组分[J].冶金分析, 2012,32(6):24-29.
【5】SIYANBOLA W O, FASASI A Y, FUNTUA I I, et al. Elemental composition of rutile from south-western Nigeria using X-ray techniques[J]. Nuclear Instruments and Methods in Physics Research B:Beam Interactions with Materials and Atoms, 2004,215(1):240-245.
【6】宫嘉辰,白小叶,姜炳南.熔融制样X射线荧光光谱法测定钒钛磁铁矿中12种组分[J].冶金分析, 2019,39(2):66-70.
【7】DUCHESNE J C, BOLOGNE G. XRF major and trace element determination in Fe-Ti oxide minerals[J]. Geologica Belgica, 2009,12(3/4):205-212.
【8】王卿,赵伟,张会堂,等.过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铁矿中铬磷钒[J].岩矿测试, 2012,31(6):971-974.
【9】MORIKAWA H, LIDA Y, ISHZUKA T, et al. Determination of impurities in titanium oxide by ICP-AES[J]. Kagaku Gernal, 1987,36:306-310.
【10】吴天良,庞书南,苏丽.ICP-AES测定金红石中的二氧化锆、三氧化二铁、二氧化硅含量[J].光谱实验室, 27(4):1294-1296.
【11】李蓉,王劲榕.ICP-AES法测定金红石及钛铁矿中锆[J].云南冶金, 2013,42(5):98-100.
【12】秦军荣,樊勇.ICP-AES法测定钛铁矿中SiO2,Al2O3[J].湖南有色金属, 2015,31(2):71-72.
【13】郑永凤,王玉清.ICP-AES法测定金红石、钛铁矿、钛铀矿中13个元素[J].分析测试通报, 1985,4(1):13-17.
【14】赵楠楠,黄慧萍,李艳玲,等.电感耦合等离子体质谱法测定金红石单矿物中的痕量稀土元素[J].理化检验-化学分册, 2012,28(7):781-784.
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