微波消解–分光光度法测定陶瓷原料中二氧化钛

采用微波消解–二安替比林甲烷分光光度法测定陶瓷原料中二氧化钛的含量。探讨了样品消解用酸的种类、检测波长、显色时间和显色剂用量对测定结果的影响。试验结果表明,以HNO_3–HF–H_2O_2溶解样品,395 nm为检测波长,显色20 min,显色液用量为12 m L时测试结果满意。测定钛的线性范围为0~2.0μg/m L,线性相关系数r~2=0.999 5,方法检出限为0.56μg/g。用该法对4种标准物质进行分析验证,测定结果与推荐值相符,测定结果的相对标准偏差为0.64%~2.28%(n=6),加标回收率为95.3%~104%。用该方法和国标方法对乐山和眉山地区陶瓷原料样品进行分析比对,经t检验证明,两种方法测定结果无显著性差异。该方法快速、准确,适合陶瓷原料中二氧化钛的检测。

Determination of Titanium Dioxide in Raw Materials of Ceramics by Microwave Digestion-Spectrophotometry

A method to determine titanium dioxide in raw materials of ceramics by microwave digestiondiantipylmethane(DAPM) spectrophotometry was established.The determination conditions were optimized which including the species of digestion acid,detection wavelength,reaction time and the dosage of chromogenic reagent.The results showed that as samples were dissolved by HNO3-HF-H2O2,395 nm as the wavelength,coloration time of 20 min and 12 mL of DAPM,the detection results were satisfied.The linear range of titanium detection was 0-2.0 μ g/mL,the correlationg coefficient (r2) was 0.999 5.The detection limit of the method was 0.56 μ g / g.The method was used to determine titanium dioxide in certified reference materials,and the results were consistent with the certified values,the relative standard deviation was 0.64％-2.28％(n=6).The recoveries ranged from 95.3％ to 104％.Ceramic raw material samples of Meishan and Leshan were detected by the method and national standard method,t test indicated that there was no significant difference between the results of two methods.This method is quick and accurate,it is suitable for the determinatin of titanium dioxide in raw materials of ceramics.