摘要
为提高电感耦合等离子体发射光谱(ICP-OES)法测定水泥熟料中铬的准确度,研究选取了Cr 205.560 nm、Cr 267.716 nm和Cr 283.563 nm三条谱线,根据水泥熟料中主量元素(铁、铝、钙和镁)含量,设计不同浓度单元素干扰实验,结果表明:铁对Cr 283.563 nm谱线测定有较大的正干扰,钙对三条谱线均有较大的负干扰,两者导致的相对误差(RE)均在±10%以上,其他一般为负干扰,RE在±10%以内。进一步线性回归分析发现,除铝外,其他干扰元素的干扰大小与浓度呈强线性相关性。通过多元素复合干扰实验发现干扰导致的RE约为-18%~11%,同单元素干扰加和结果比较,两者相差约为8%~10%。实际样品检测结果表明,实际干扰同多元素复合干扰实验基本相同,Cr 283.563 nm谱线测定结果误差可能更小,三条谱线的实际样品加标回收率大致相当,约为80%,经回收率修正,Cr 205.560 nm和Cr 267.716 nm谱线结果满意,而Cr 283.563 nm谱线误差较大。以多元素复合干扰实验溶液作为基体,采用基体匹配法测定可基本消除干扰影响。以钙溶液作为基体的简化基体匹配法同样有效,但仅可选用Cr 205.560 nm和Cr 267.716 nm谱线。从实际干扰问题出发,通过系统分析问题,找到干扰的原因,并据此提出消除干扰方法,提高了测定铬的准确度,也为检测人员解决相关干扰问题提供借鉴。
To improve the accuracy of determination of chromium in cement clinker by ICP-OES,spectral lines of Cr 205.560 nm,Cr 267.716 nm and Cr 283.563 nm were selected in this study.According to the main elements(Fe,Al,Ca and Mg)of cement clinker content,single element interference tests with different concentrations were carried out.The results show that iron has a large positive interference for Cr 283.563 nm,calcium has a large negative interference for all three lines,the relative errors(RE)of them are more than±10%,RE of the other are within±10%,generally negative interference.Further linear regression analysis shows that there is a strong linear correlation between the interference and the concentration of interference elements except aluminum.It is found that the RE caused by interference is about-18%—11%by multi-element composite interference test,which is about 8%—10%different from the sum result of single element interference.The actual sample detection results show that the actual interference is basically the same as the multi-element composite interference test.The error of the determination results using Cr 283.563 nm spectral line may be smaller,and the recoveries of the three spectral lines are similar,about 80%.After the recovery correction,the spectral lines of Cr 205.560 nm and Cr 267.716 nm are satisfactory,while Cr 283.563 nm is low.The matrix interference can be eliminated by matrix matching method with multi-element composite interference test solution as matrix.The simplified matrix matching method with calcium solution as matrix is also effective,but only Cr 205.560 nm and Cr 267.716 nm can be used for spectral line.In this study,the interference was systematically studied and found the reason,a method to eliminate the interference was put forward,which improved the accuracy of determination of chromium,and provided a reference to solve related problems.
作者
刘德金
田荣
吴思聪
车敏
黄勇
LIU Dejin;TIAN Rong;WU Sicong;CHE Min;HUANG Yong(Chongqing Chemical Industry Construction Engineering Quality Surveillance,Chongqing 400020,China;Chongqing Cement Quality Supervision and Inspection,Chongqing 400020,China;Chongqing School,University of Chinese Academy of Sciences,Chongqing 400714,China;Chongqing Institute of Green and Intelligent Technology,Chinese Academy of Sciences,Chongqing 400714,China)
出处
《中国无机分析化学》
CAS
北大核心
2022年第4期45-50,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
中国科学院西部之光资助项目(E0296105)。
关键词
ICP-OES
水泥熟料
铬
电离干扰
光谱干扰
干扰校正
固体废物
ICP-OES
cement clinker
chromium
ionization interference
spectral interference
interference correction
solid waste
