两步法熔融制样-X射线荧光光谱法测定硅钙钡合金中9种主次量元素  

Determination of Nine Major and Minor Elements in Si-Ca-Ba Alloy by X-Ray Fluorescence Spectrometry with Two-Step Fusion Sample Preparation

作　　者：於利慧 YU Lihui(Pangang Group Research Institute Co.,Ltd.,Panzhihua 617000,China;Sichuan Pan Testing Technology Co.,Ltd.,Panzhihua 617000,China)

机构地区：[1]攀钢集团研究院有限公司,攀枝花617000 [2]四川攀研检测技术有限公司,攀枝花617000

出　　处：《理化检验（化学分册）》2021年第9期840-844,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：以两步法熔融制样,建立了X射线荧光光谱法(XRFS)测定硅钙钡合金中5种主量元素(Si、Ca、Ba、Al、Fe)和4种次量元素(P、Mn、Cu、Cr)含量的方法。将以6∶0.5∶0.2的质量比混合的Li_(2)B_(4)O_(7)、Li_(2)CO_(3)、样品和1.0~2.0 g NH_(4)NO_(3)一起包裹在滤纸中,放入预先用石墨粉垫底的瓷坩埚中,在程序升温条件下进行第一步熔融。冷却后,将熔球转移至铂-金坩埚中,加入0.5~1.0 g脱模剂NH_(4)I,在马弗炉中进行第二步熔融,于1 100℃熔融10~15 min,冷却成型后即得玻璃样片,供XRFS分析。以有证标准样品和内控标准样品熔融制备校准用标准样品系列,以经验α系数法建立的校正公式进行基体效应校正。结果显示:校准曲线的相关系数在0.950 0以上,方法用于实际样品分析,所得9种元素测定值的相对标准偏差(n=10)均小于4.0%,测定值与采用其他文献方法所得的测定结果吻合。A method for the determination of the contents of five major elements(Si, Ca, Ba, Al, Fe) and four minor elements(P, Mn, Cu, Cr) in Si-Ca-Ba alloy was established by X-ray fluorescence spectrometry(XRFS) with two-step fusion sample preparation. Li_(2)B_(4)O_(7), Li_(2)CO_(3) and samples with the mass ratio of 6∶0.5∶0.2 and ammonium nitrate(1.0-2.0 g) were wrapped in filter paper and put into a porcelain crucible with graphite powder as the bottom in advance. The first step of melting was made under the condition of programmed temperature. After cooling, the molten ball was transferred to a Pt-Au crucible, 0.5-1.0 g of NH_(4)I as release agent was added, and the second step of melting was made in a muffle furnace at 1 100 ℃ for 10-15 min. After cooling and forming, the glassy slice of sample obtained was used for XRFS analysis. Standard sample series for calibration were prepared by melting certified standard samples and internal control standard samples, and the matrix effect was corrected by the correction formula established by empirical α coefficient method. The results showed that correlation coefficients of the calibration curves were more than 0.950 0. The proposed method was used for the analysis of actual samples, RSDs(n=10) of the determined values of nine elements were less than 4.0%, and the determined values were consistent with those obtained by the methods described in literatures.

关 键 词：熔融制样 两步法 X射线荧光光谱法 主次量元素 硅钙钡合金 

分 类 号：O657.34[理学—分析化学]