高碳铬铁EDXRF分析中的制样条件优化  

Optimization of Measurement Conditions of High Carbon Ferrochrome Based on EDXRF Technology

作　　者：李欣倩 冯海涛[1,2] 李波 高丹丹[1,2] 张波 董亚萍[1,2] 李武 LI Xin-qian;FENG Hai-tao;LI Bo;GAO Dan-dan;ZHANG Bo;DONG Ya-ping;LI Wu(Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources,Qinghai Institute of Salt Lakes,Chinese Academy of Sciences,Xining,810008,China;Qinghai Technology Research and Development Center of Comprehensive Utilization of Salt Lakes Resources,Xining,810008,China;University of Chinese Academy of Sciences,Beijing,100049,China)

机构地区：[1]中国科学院青海盐湖研究所,中国科学院盐湖资源综合高效利用重点实验室,青海西宁810008 [2]青海盐湖资源综合利用技术研究开发中心,青海西宁810008 [3]中国科学院大学,北京100049

出　　处：《盐湖研究》2021年第2期102-108,共7页Journal of Salt Lake Research

基　　金：国家自然科学基金(U1607103);青海省重大科技专项(2016-GX-A10)资助。

摘　　要：利用能量色散X射线荧光光谱分析技术(EDXRF)检测高碳铬铁,能实现对主次组分的同时测量,且无需对铬铁样品进行化学处理。实验以荧光强度和测试精密度为指标,采用单因素试验考察了粉末压片制样过程中称样量、粘结剂种类与用量、研磨时间、压片压力、保压时间等制样条件对测量结果的影响趋势,并将优化后的条件用于对高碳铬铁的检测。结果表明,使用6 g样品和0.4 g微晶纤维素,研磨时间为3 min,压片压力为40 MPa,保压时间为1 min时制得的样片表面光滑,测定重现性好。精密度和稳定性分析表示,各元素测定结果的相对标准偏差(RSD)均小于0.5%,证明优化制样条件后可以满足利用EDXRF定量分析铬铁主次元素的要求。A method of pressed powder pellet is reported for the simultaneous determination of eight major and minor elements in high-carbon ferrochromium samples by Energy dispersive X-ray fluorescence spectrometry(EDXRF).Single factor experiment was used to optimize sample weight,binder type and dosage,grinding time,tablet pressure and holding time with fluorescence intensity and test precision as indexes.And the optimized conditions were applied to the detection of high carbon ferrochromium.The results showed that the surface of the sample was smooth when 0.4 g microcrystalline cellulose was used,the grinding time was 3 min,the sample weight was 6 g,the pressing pressure was 40 MPa,and the holding time was 1 min.The results of precision and stability showed that the relative standard deviation(RSD)of each element was less than 0.5%,which proved that the optimized sample preparation conditions could meet the requirements of quantitative analysis of primary and secondary elements of ferrochrome by EDXRF.

关 键 词：EDXRF 粉末压片 条件优化 高碳铬铁 

分 类 号：O657.3[理学—分析化学]