熔融制样-X射线荧光光谱法快速测定富钛料中主次成分

以Li₂B₄O₇为熔剂,Li₂CO₃作助熔剂,NH₄I作脱模剂,熔融法制备样品,建立了X射线荧光光谱法测定富钛料中SiO₂、Al₂O₃、CaO、MgO、MnO、TiO₂、TFe的分析方法。试验表明,采用高温预氧化处理,解决了高钛渣样品中低价钛对铂黄金坩埚的腐蚀问题;在最佳试样量为0.4 g、稀释比(m_样品:m_熔剂)为1∶15、脱模剂使用量为20 mg时熔样效果最佳。采用经验系数法对基体效应进行校正后,测定富钛料样品中各成分的相对标准偏差(RSD,n=10)在0.06%~0.84%之间。用标准物质和实际样品验证,测定结果与标准物质认定值和实际样品化学分析方法测定值相符,能够满足日常分析的要求。

X-ray fluorescence spectrometric determination of major and minor components in titanium-rich material with fusion sample preparation

A determination method for SiO₂,Al₂O₃,CaO,MgO,MnO,TiO₂ and TFe in Ti-rich materials by X-ray fluorescence spectrometry was established with Li₂B₄O₇ as flux,Li₂CO₃ as cosolvent and NH₄I as release agent for sample fusion preparation. Tests showed that the high-temperature pre-oxidation treatment prevented the low-valence titanium in the high titanium slag sample from corroding the platinum-gold crucible; and the sample fusion was optimum with optimum sample dosage of 0.4 g,dilution ratio (m_sample∶m_flux) of 1∶15 and release agent dosage of 20 mg. After the matrix effect was corrected with empirical coefficient method,the relative standard deviations for the determination of each component in titanium-rich material samples were 0.06%-0.84%. Certified reference materials and actual samples were used for verification and the results were consistent with the certified values and those obtained by chemical analytical methods,so it could meet the requirements of routine analysis.