摘要
采用盐酸、硝酸、氢氟酸分解试样,冒磷酸和高氯酸烟,如需要可加内标元素钇,加酒石酸溶液,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定钢中钨、钼和铌。在优化仪器工作条件的基础上,综合考虑灵敏度和干扰情况选择最合适的分析线为W 207.911nm、Mo202.030nm、Mo 281.615nm、Nb 309.418nm、Nb 316.340nm,并考察了可能的干扰元素。标准溶液系列与被测样品主体元素进行基体匹配,消除了基体效应的影响。各元素校准曲线线性相关系数均大于0.998,钨、钼、铌的检出限分别为0.037 0、0.037 9和0.062 9mg/L。实验方法适用于钢中质量分数为0.005%~19.0%钨、0.005%~8.0%钼和0.005%~5.0%铌的测定,国内7家获得中国合格评定国家认可委员会认可的钢铁行业实验室之间的精密度试验证明方法具有良好的重复性和再现性。
The sample was decomposed with hydrochloric acid,nitric acid and hydrofluoric acid followed by smoking of phosphoric acid and perchloric acid.The internal standard yttrium and tartaric acid solution could be added if necessary.The contents of tungsten,molybdenum and niobium in steels were determined by inductively coupled plasma atomic emission spectrometry（ICP-AES）.Based on the optimization of instrumental parameters, W 207.911 nm, Mo 202.030 nm, Mo 281.615 nm,Nb 309.418 nm and Nb316.340 nm were selected as the analytical lines by considering the sensitivity and interference.Meanwhile,the possible interference elements were investigated.The influence of matrix effect was eliminated through matrix matching between standard solution series and major elements in tested samples.The linear correlation coefficients of all calibration curves were higher than 0.998.The detection limit of tungsten,molybdenum and niobium was 0.037 0,0.037 9 and 0.062 9 mg/L,respectively.The proposed method was suitable for the determination of tungsten,molybdenum and niobium in steels with mass fraction of 0.005%-19.0%,0.005%-8.0% and 0.005%-5.0%,respectively.The precision tests conducted by seven accredited iron and steel industry laboratories indicated that proposed method had good repeatability and reproducibility.
作者
于媛君
亢德华
杨丽荣
高品
王莹
邓军华
YU Yuan-jun;KANG De-hua;YANG Li-rong;GAO Pin;WANG Ying;DENG Jun-hua(Iron ＆ Steel Research Institute of Ansteel Group,Anshan 114009,China)
出处
《冶金分析》
CAS
CSCD
北大核心
2018年第7期73-79,共7页
Metallurgical Analysis
