熔融制样-X射线荧光光谱法测定石灰石中5种组分  

Determination of five components in limestone by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：曲月华[1] 王翠艳[2] 王一凌[1,3] 张慤 

机构地区：[1]鞍钢股份公司技术中心,辽宁鞍山114009 [2]鞍山师范学院化学系,辽宁鞍山114000 [3]辽宁科技大学化工学院,辽宁鞍山114051 [4]沈阳广播电视大学理工学院,辽宁沈阳110003

出　　处：《冶金分析》2013年第12期29-33,共5页Metallurgical Analysis

摘　　要：以标准样品及人工配制校准样品共同绘制校准曲线,无需对石灰石中的碳酸盐进行烧损校正,直接采用无水四硼酸锂熔剂熔融石灰石样品,以X射线荧光光谱法测定石灰石中CaO、MgO、SiO2、Al2O3、Fe2O3含量.探讨确定样品与熔剂的稀释比例为1∶ 10;预熔温度为900℃,时间为80 s、熔融温度为1 100℃,熔融时间为300 s;无须进行烧失量及基体干扰校正,可直接测定石灰石中5种主要成分.对石灰石测定成分进行了精密度考察,结果的相对标准偏差（n=10）在0.28％～4.9％之间.采用方法对石灰石标准样品及实际样品进行测定,结果与认定值或其他方法的测定值相吻合.The certified reference material sample and artificial calibration sample were used to plot the calibration curve, and the limestone sample was directly fused with anhydrous lithium tetraborate as flux without ignition loss correction for the carbonate in limestone. Consequently, CaO, MgO, SiO2, Al2 O3 and Fe2O3 contents in the limestone were determined by X-ray fluorescence spectrometry. Ex- periments conditions were obtained as follows：the dilution ratio of sample to flux was 1 ： 10, the pre- fusion temperature was 900 ℃ for 80 s and the fusion temperature was 1 100 ℃ for 300 s; five main components in the limestone could be determined directly without loss on ignition and matrix interfer- ence correction. The precision tests was carried out for the determination of components and the relative standard deviation （n=10） was in the range of 0. 28%-4. 9%. This met plied to the determination of limestone certified reference materials and actual samples. in limestone hod was ap- e resultswere consistent with the certified values or those obtained by other methods.

关 键 词：X射线荧光光谱法 石灰石 矿物元素 熔融制样 烧失量 

分 类 号：O657.34[理学—分析化学]