摘要
用电感耦合等离子体原子发射光谱法(ICP-AES)测定铬铁中铬磷硅存在的问题是一些高碳铬铁、氮化铬铁等试样难以用酸溶解,在碱熔基体中,大量的易电离元素钠的存在使得测定困难,铬铁中高含量铬和微量的磷、硅等同时测定尤为困难。ICP-AES法同时测定铬铁中铬磷硅是一种新颖的方法。通过试验研究,确定了利用氢氧化钠-过氧化钠混合熔剂熔样的样品处理方法。在用ICP进行测试时,不同谱线所受到的干扰不同。推荐选择Cr 267.716 nm、Cr 206.158 nm、P 213.617 nm、Si 251.611 nm、Si 288.158 nm为分析线;对于干扰,采用基体匹配和两点校正法消除,方法的线性相关系数在0.995以上,磷的测试精密度在5.0%,铬、硅在1.0%以下;铬、硅检出限在0.006%以下,磷为0.002%。准确度试验表明,分析结果与推荐值和手工分析结果间的分析误差在试验允许的误差范围内。
The existing problem of the determination of chromium phosphorus silicon in ferrochromium by inductively coupled plasma emission spectrometry（ ICP-AES） is that some samples,such as high carbon ferrochrome,ferrochrome nitride,etc,is difficult to be dissolved by acid. In the alkali fusion matrix,a large number of easily ionized elements sodium makes it difficult to determine,the simultaneous determination of high content of chromium and trace amounts of phosphorus and silicon is particularly difficult. The simultaneous determination method of chromium,phosphorus,silicon in ferrochromium by inductively coupled plasma atomic emission spectrometry（ ICP-AES） is a novel method. Through the experimental research,the treatment method of samples by melting in mixed flux of sodium hydroxide and sodium peroxide was determined. In the test by ICP-AES,the interference received is different on each line. Cr267. 716 nm,Cr 206. 158 nm,P 213. 617 nm,Si 251. 611 nm,Si 288. 158 nm as the analysis line are recommended. For the interference,it is eliminated by using matrix matching and two-point correction method,the linear correlation coefficient of the method was above 0. 995,the precision of phosphorus determination was 5. 0%,the precisions of chromium and silicon were below 1. 0%,the detection limit was below 0. 006% for chromium and silicon,and 0. 002% for phosphorus. Accuracy tests showed that the analysis error between this method and recommendation or manual analysis results was within the allowable range.
出处
《材料开发与应用》
CAS
2015年第5期14-19,共6页
Development and Application of Materials
