摘要
采用具有操作简单、消解完全等优点的微波消解样品,利用磺基水杨酸光度法测定陶瓷原料中三氧化二铁含量;探讨了消解所用酸的种类、显色波长、显色时间和显色剂用量的影响,结果表明以HCl-HNO_3-HF-H_2O_2溶矿,420 nm为显色波长,10 min显色,5 mL磺基水杨酸显色液为条件时陶瓷原料中所含高含量的杂质离子对Fe_2O_3的测定基本没有影响测试效果;使用4种陶瓷原料国家标准物质GBW03116、GBW03134、GBW03115、GBW03122进行分析验证,测定值与推荐值相符,RSD为1.04~3.47%,相对误差绝对值≤4.21%,加标回收率在92.0~106.1%,|△lgC|≤0.019;对乐山和眉山地区陶瓷原料样品进行分析并与常规消解国标方法进行比对实验,测定结果采用t检验法证明两种方法无显著性差异。新建立的方法为快速、准确检测陶瓷原料中Fe_2O_3提供了一条新的途径。
A new method to determine the content of Fe203 in raw materials of ceramics by Sulfosalicylic acid- VIS Spectrophotometry which has many advantages such as operating simply, dissolving completely is presented in this paper. The influence of species and dosage of digestion reagent, wavelength, reaction time and the dosage of Sulfosalicylic acid were investigated. The results showed that samples were dissolved by HCl-HNO3-HF-H2O2, 420 nm as the wavelength and 5 mL of sulfosalicylic acid. The method has been validated by determination of Fe203 in national standard reference materials of GBW03116, GBW03134, GBW03115 and GBW03122. The results were in agreement with certified values and the RSD was 1.04- 3.47%. The relative error was less than 4.21%. The recovery ratio was ranging from 92.0% to 106.1% and the ｜△lgc｜was less than 0.019. Compared with the traditional digestion method that analytical ceramic raw material samples of Meishan and Leshan, there is no significant difference between the two methods by Student＇ s t test. This new method provide a new way for quick and accurate to determine the content of Fe2O3 in raw materials of ceramics.
出处
《中国陶瓷》
CSCD
北大核心
2017年第6期41-45,共5页
China Ceramics
关键词
微波消解
分光光度法
陶瓷原料
FE2O3
Microwave Digestion
VIS Spectrophotometry
Raw materials of ceramics
Fe203
