熔融制样-X射线荧光光谱法测定白云石中主次量组分  

Determination of Major and Minor Components in Dolomite by X-Ray Fluorescence Spectrometry after Fusion Sample Preparation

作　　者：廖建容 罗明荣[1] LIAO Jianrong;LUO Mingrong(Atlantic China Welding Consumables,Inc.,Zigong 643000,China)

机构地区：[1]四川大西洋焊接材料股份有限公司检测所,自贡643000

出　　处：《理化检验（化学分册）》2021年第9期845-849,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：建立了熔融制样-X射线荧光光谱法(XRFS)同时测定白云石中氧化钙、氧化镁、二氧化硅、三氧化二铝、三氧化二铁、二氧化钛、氧化钾、氧化钠、五氧化二磷含量的方法。称取混合熔剂(由质量比67∶33的四硼酸锂和偏硼酸锂混合而成) 6.000 0 g,先将一半熔剂倒入铂-金坩埚中,然后加入碘化铵0.2 g和干燥好的样品0.900 0 g,混匀后,再将剩余的混合熔剂覆盖在表面,在1 000℃熔融12 min,得到的玻璃样片供XRFS分析。以标准物质、光谱纯试剂和基准试剂混合熔融制备校准用标准样品系列,以经验α系数法进行基体校正和谱线重叠效应校正。结果显示:校准曲线的相关系数为0.993 8~1.000,检出限为9.31~129.1μg·g^(-1);对实际样品进行单天内重复测定11次和11天的重复测定,测定值的相对标准偏差(RSD)不大于6.0%和10%;对11个平行制备的样品进行单天和11天连续测定(每天1个样品),测定值的RSD不大于7.0%和8.0%;方法用于分析标准物质和实际样品,测定值和认定值或按GB/T 3286-2012所得测定值的误差均在GB/T 3286-2012的允许差范围内。A method for the simultaneous determination of calcium oxide, magnesium oxide, silicon dioxide, aluminum oxide, iron oxide, titanium dioxide, potassium oxide, sodium oxide and phosphorus pentaoxide in dolomite by X-ray fluorescence spectrometry after fusion sample preparation was established. 6.000 0 g of the flux mixture(lithium tetraborate and lithium metaborate with mass ratio of 67∶33) was weighed, half of the flux was poured into a Pt-Au crucible, and ammonium iodide(0.2 g) and the dried sample(0.900 0 g) were added subsequently. After mixing well, the remaining flux was taken and covered on the surface of the above mixture for melting at 1 000 ℃ for 12 min, the glassy slice of sample obtained was analyzed by XRFS. The series of standard samples for calibration were prepared by melting of the mixtures of standard materials, spectral pure reagents and reference reagents, matrix effect and spectral line overlapping effect were corrected by empirical α coefficient method. The results showed that linear correlation coefficients of calibration curves were found beween 0.993 8 and 1.000, with detection limits ranged from 9.31 μg·g^(-1) to 129.1 μg·g^(-1). The actual samples were analyzed by eleven repeated determinations in a single-day and 11 days repeated determinations, RSDs of the determined values was not greater than 6.0% or 10%;single-day and 11 days(1 sample per-day) continuous determinations were made on 11 parallel-prepared samples, RSDs of the determined values was not greater than 7.0% or 8.0%. The proposed method was applied to analyze standard substances and actual samples, errors between the determined values and the certified values or the determined values obtained from GB/T 3286-2012 were all within the allowable error range of GB/T 3286-2012.

关 键 词：熔融制样 X射线荧光光谱法 主次量组分 白云石 

分 类 号：O657.31[理学—分析化学]