熔融制样-X射线荧光光谱法测定钨铁合金中硅锰磷铜钨  

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

作　　者：刘伟[1,2] 曹吉祥[1,2] 张瑜[1,2] LIU Wei;CAO Ji-xiang;ZHANG Yu(State Key Laboratory of Advanced Stainless Steel Materials,Taiyuan Iron & Steel (group) Co.,Ltd.,Taiyuan 030003,China;Technology Center,Shanxi Taiyuan Stainless Steel Co.,Ltd.,Taiyuan 030003,China)

机构地区：[1]太原钢铁(集团)有限公司先进不锈钢材料国家重点实验室,山西太原030003 [2]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》2019年第2期46-50,共5页Metallurgical Analysis

摘　　要：钨铁合金是冶炼高速钢等钨合金钢的加入剂,目前采用化学湿法分析钨、硅、锰、磷和铜的含量,实验流程很长,操作相对繁琐。实验采用碳酸锂和过氧化钠作氧化剂预氧化样品、熔融方法制样,建立了X射线荧光光谱法(XRF)测定钨铁合金中硅、锰、磷、铜、钨5种元素含量的检测方法。绘制校准曲线时,采用钨铁标准样品中加入三氧化钨纯物质及硅、锰、磷、铜标准溶液的方法扩展了校准曲线线性范围。实验表明,以四硼酸锂为熔剂,溴化铵为脱模剂,试样与熔剂比例为1∶30,在1 150℃熔融炉中熔融10min,制得表面光滑、无气孔、无结晶的均匀玻璃片。实验方法用于测定钨铁合金样品中硅、锰、磷、铜、钨,测定结果的相对标准偏差(RSD,n=8)为0.20%～5.2%;按照实验方法测定3个钨铁合金样品中硅、锰、磷、铜、钨,并与相应的国家标准方法进行比对,结果相一致。Ferrotungsten alloy is an additive for the smelting of tungsten-alloy steels such as high-speed steels.At present,the chemical wet method is usually used to analyze the contents of tungsten,silicon,manganese,phosphorus and copper in ferrotungsten.However,this method has the disadvantages of long experimental process and complicated operation.The sample was pre-oxidized by lithium carbonate and sodium peroxide.The determination method of silicon,manganese,phosphorus,copper and tungsten in ferrotungsten alloy by X-ray fluorescence spectrometry(XRF)with fusion sample preparation was established.During the establishment of calibration curves,pure tungsten trioxide as well as standard solution of silicon,manganese,phosphorus and copper was added into the standard sample of ferrotungsten to extend the linear range of calibration curves.The results showed that the uniform glass beads with smooth surface,no pores and no crystallization could be prepared under the following experimental conditions:the lithium tetraborate was used as flux,the ammonium bromide was selected as the releasing agent,the ratio of sample to flux was 1∶30,and the sample was melted in melting furnace at 1150℃for 10min.The proposed method was applied to the determination of tungsten,silicon,manganese,phosphorus and copper in ferrotungsten alloy.The relative standard deviations(RSD,n=8)were between 0.20%and 5.2%.The contents of tungsten,silicon,manganese,phosphorus and copper in three ferrotungsten alloy samples were determined according to the experimental method.The found results were consistent with those obtained by the corresponding national standard methods.

关 键 词：预氧化 熔融制样 X射线荧光光谱法 钨铁合金 主次元素 

分 类 号：TF652[冶金工程—钢铁冶金] O657.34[理学—分析化学]