Determination of zirconium oxide, hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material by X-ray fluorescence spectrometry with fusion sample preparation
ZHANG Yu1,2, LIU Wei1,2
1. State Key Laboratory of Advanced Stainless Steel Materials, Taiyuan Iron and Steel (Group) Co., Ltd., Taiyuan 030003,China; 2. Technical Center of Shanxi Taiyuan Stainless Steel Co., Ltd., Taiyuan 030003, China
Abstract：At present, the main analysis method for carbon-bearing refractory materials is chemical wet method, and X-ray fluorescence spectrometry (XRF) is mostly suitable for the ordinary refractory materials. Zirconium oxide, hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material were investigated.The determination method of these three components in carbon-bearing zirconium-aluminum refractory material by XRF with fusion sample preparation was established. In experiments, the samples were pre-oxidized using sodium nitrate and sodium peroxide as the oxidant to eliminate the corrosion of silicon carbide on the Pt-Au crucible. The mixture of lithium tetraborate and lithium metaborate (m∶m=5∶1) was used as flux and ammonium iodide was selected as the release agent. The ratio between sample and flux was 1∶20. After fusion at 1100℃ for 15min, the uniform glass beads with smooth surface and without bubbles and crystals could be prepared. The spectral lines of ZrLα, HfLβ and AlKα were selected to determine the contents of zirconium oxide, hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material in experiments. The regression accuracy of the curves was 0.162, 0.033 and 0.209 respectively. The relative standard deviation (RSD, n=8) of determination results was 1.7%, 4.3% and 0.21% respectively. The contents of zirconium oxide, hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material sample were determined according to the experimental method, and the found results were consistent with those obtained by corresponding national standard methods.
李小明,赵会芹,刘兰英,等. X射线荧光光谱法测定稳定氧化锆中主、次量元素[J].山东冶金,2005,27(3):48-49.LI Xiao-ming,ZHAO Hui-qin,LIU Lan-ying,et al.Determination of primary and secondary elements in stabilized zirconia by XRF[J].Shandong Metallurgy,2005,27(3):48-49.
[5]
宋霞,王静.锆刚玉质耐火材料的X射线荧光光谱分析法[J].光谱实验室,2006,23(6):1314-1317.SONG Xia,WANG Jing.XRF analysis of zircaloy refractories[J].Chinese Journal of Spectroscopy Laboratory,2006,23(6):1314-1317.
[6]
王本辉,郭红丽,胡坚.X射线荧光光谱法测定氧化锆质耐火材料中主次成分[J].冶金分析,2010,30(1):39-42.WANG Ben-hui,GUO Hong-li,HU Jian.Determination of primary and secondary components in zirconia refractories by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(1):39-42.
