熔融制样-X射线荧光光谱法测定硅锰合金中硅锰磷  

Determination of silicon,manganese,phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：刘伟[1] 曹吉祥[1] 郭云涛[1] 戴学谦[1] 

机构地区：[1]山西太钢不锈钢股份有限公司技术中心,山西太原030003

出　　处：《冶金分析》2015年第8期51-54,共4页Metallurgical Analysis

摘　　要：采用硅锰及锰铁的标准样品,以一定比例人工合成校准样品,绘制校准曲线,建立了X射线荧光光谱法(XRF)测定硅锰合金中硅、锰、磷的方法,各元素的检出限分别为0.015 3%、0.018 9%、0.002 9%。为避免硅锰合金样品对铂金坩埚的腐蚀问题,选用碳酸锂和过氧化钠分步氧化硅锰合金试样,讨论了熔剂、氧化剂的选择及预氧化的操作方式。试验结果表明:将试样与四硼酸锂熔剂以1∶30的质量比混合,加入5滴400g/L溴化铵溶液做脱模剂,制得试样在熔剂中分散均匀的玻璃片,能同时适用于高低含量组分的测定。当硅、锰、磷质量分数分别为24.58%、65.20%、0.190%时,10次测量结果的相对标准偏差(RSD)分别为0.29%、0.14%和0.92%。方法用于硅锰合金样品中硅、锰、磷的测定,与湿法测定值吻合较好,能满足常规分析要求。The calibration samples were artificially synthesized using the standard samples of silicon-manganese and manganese-iron in according to a certain proportion.The calibration curves were prepared,and the determination method of silicon,manganese and phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry(XRF)was established.The detection limit of silicon,manganese and phosphorus was 0.015 3%,0.018 9% and 0.002 9%,respectively.In order to avoid the corrosion of silicon-manganese alloy sample to the platinum-gold crucible,the silicon-manganese alloy sample was oxidized successively with lithium carbonate and sodium peroxide.The selection of flux and oxidizing agent as well as the operation method of pre-oxidization were discussed.The results indicated that the sample could be uniformly dispersed in flux when the mass ratio between sample and lithium tetraborate was 1∶30and five drops of 400g/L ammonium bromide solution was used as releasing agent.Meanwhile,it was simultaneously applicable for the determination of high and low content components.The relative standard deviation(RSD,n=10)was 0.29%,0.14% and 0.92% when the content of silicon,manganese and phosphorus was 24.58%,65.20% and 0.190%,respectively.The proposed method was applied to the determination of silicon,manganese and phosphorus in silicon-manganese alloy,and the found results were consistent with those obtained by the wet method.It could meet the requirements of routine analysis.

关 键 词：熔融制样 X射线荧光光谱法 硅锰合金 预氧化 硅 锰 磷 

分 类 号：TG115.33[金属学及工艺—物理冶金]