Determination of silicon, manganese, phosphorus, copper, tungsten in ferrotungsten alloy by X-ray fluorescence spectrometry with fusion sample preparation
LIU Wei1,2, CAO Ji-xiang1,2, ZHANG Yu1,2
1. State Key Laboratory of Advanced Stainless Steel Materials, Taiyuan Iron & Steel (group) Co., Ltd., Taiyuan 030003, China; 2. Technology Center, Shanxi Taiyuan Stainless Steel Co., Ltd., Taiyuan 030003, China
Abstract：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.
时军波.X射线荧光光谱法测定钨铁合金(粉末)中的钨、铁、硅、锰、铜[J].化学分析计量,2000(4):20-21.SHI Jun-bo.Determination of multi-elements(W,Fe,Si,Mn,Cu) in ferrotungsten by XRF method[J].Chemical Analysis and Meterage,2000(4):20-21.
[7]
吉昂,陶光仪,卓尚军,等.X射线荧光光谱分析[M].北京:科学出版社,2003:201-204.
[8]
宋鹏心,张健,杨志强,等.离心浇铸制样X-射线荧光光谱法测定钨铁中钨[J].冶金分析,2013,33(4):48-51.SONG Peng-xin,ZHANG Jian,YANG Zhi-qiang,et al.Determination of tungsten in ferrotungsten by X-ray fluorescence spectrometry with centrifugal casting sample preparation[J].Metallurgical Analysis,2013,33(4):48-51.
[9]
鲍希波,石毓霞,赵靖,等.熔融制样-X射线荧光光谱法测定硅铁合金中主次元素[J].冶金分析,2010,30(5):14-18.BAO Xi-bo,SHI Yu-xia,ZHAO Jing,et al.X-ray fluorescence spectrometry for the determination of major and minor elements in ferro-silicon alloy with fusion sample preparation[J].Metallurgical Analysis,2010,30(5):14-18.
[10]
Coedo A G,Dorado T,Padilla I,et al.X-ray fluorescence determination of major and minor elements in ferrotitanium,ferroniobium and ferrovanadium from compressed pellets and fusion beads[J].X-Ray Spectrometry,2002,31:424-431.
[11]
Giles H L,Holmes GM.The X-ray fluorescence analysis of ferroniobium by a fusion method[J].X-ray Spectrometry,1978,7(1):2-4.
[12]
刘伟,曹吉祥,郭云涛,等.熔融制样-X射线荧光光谱法测定硅锰合金中硅锰磷[J].冶金分析,2015,35(8):51-54.LIU Wei,CAO Ji-xiang,GUO Yun-tao,et al.Determination of silicon, manganese, phosphorus in silicon manganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(8):51-54.
