微波常压碱熔-过氧化氢光度法测定氧化焙烧钒钛球团中二氧化钛  

Microwave heating atmospheric alkali fusion-hydrogen peroxide spectrophotometric determination of titanium dioxide in oxidized and calcined vanadium-titanium pellets

作　　者：杨朝帅[1] 余亚美[1] 邱红绪 

机构地区：[1]河北省地矿局唐山实验测试所,河北唐山063000

出　　处：《冶金分析》2015年第4期19-24,共6页Metallurgical Analysis

摘　　要：建立了微波常压碱熔融法分解样品结合光度法测定氧化焙烧钒钛球团中二氧化钛含量的分析方法。实验以台式微波化学实验炉为热源,过氧化钠和氢氧化钠的混合物作为熔剂,试样在480 W微波功率下加热14min被充分分解。用硫-磷混合酸将碱熔融物酸化,大量的铁基体与磷酸络合,从而消除其干扰。分取部分试液在硫酸介质中以过氧化氢为显色剂显色,采用标准曲线法确定试样中二氧化钛的量。在0~40μg/mL范围内建立二氧化钛校准曲线,其线性相关系数r≥0.999 8。以氟化物褪色参比溶液可消除共存的钒、铬等干扰元素的影响。经不同实验室用X射线荧光光谱法（XRF）和滴定法对实际样品进行比对分析,实验方法的测定结果与其他方法相吻合,相对标准偏差（RSD）在0.22%~0.82%之间,结果满足工业生产的需要。The analysis method of titanium dioxide content in oxidized and calcined vanadium-titanium pellet by hydrogen peroxide spectrometry after microwave alkali fusion at atmospheric pressure was established. The desktop microwave chemical experiment furnace was used as heat source ,and the mixture of sodium peroxide and sodium hydroxide was used as the flux for fusion. The sample was fully decomposed after digestion for 14 min under microwave power of 480 W. The alkali fusion matters were acidified with sulfuric acid-phosphoric acid. Much iron matrix would be eomplexed with phosphoric acid, eliminating the interfer- ence. Partial sample solution was colored in sulfuric acid medium using hydrogen peroxide as coloring a- gent. The content of titanium dioxide in sample was obtained by standard curve method. The calibration curve of titanium dioxide in range of 0-40 /,g/mL was established,and the linear correlation coefficient was no less than 0. 999 8. The influence of coexisting vanadium and chromium could be eliminated by fluoride fading reference solution. The actual samples were also analyzed by X-ray fluorescence spectrometry （XRF） and titration method in various laboratories. The determination results of proposed method were consistent with those obtained by other methods,and the relative standard deviation （RSD） was between 0.22% and 0.82%. The results could meet the requirements of industrial production.

关 键 词：微波加热 常压碱熔 过氧化氢 光度法 氧化焙烧钒钛球团 二氧化钛 

分 类 号：TF802[冶金工程—有色金属冶金] O657.3[理学—分析化学]