熔融制样-X射线荧光光谱法测定含碳锆铝耐火材料中氧化锆、氧化铪和氧化铝

目前针对含碳耐火材料的分析方法以化学湿法为主,X射线荧光光谱法(XRF)多适用于普通的耐火材料。实验针对含碳锆铝耐火材料中的氧化锆、氧化铪和氧化铝进行研究,建立了熔融制样-X射线荧光光谱法测定含碳锆铝耐火材料中这3种组分的方法。实验采用硝酸钠和过氧化钠作氧化剂预氧化样品,可消除碳化硅对铂-金坩埚的腐蚀。以四硼酸锂-偏硼酸锂(m∶m=5∶1)混合熔剂熔融,以碘化铵为脱膜剂,试样与熔剂比例为1∶20,在1100℃熔融15min,可制得表面光滑、无气泡、无结晶的均匀玻璃片。实验选择ZrLα、HfLβ和AlKα谱线测定含碳锆铝耐火材料中的氧化锆、氧化铪和氧化铝,曲线回归精度分别为0.162、0.033和0.209;测定结果的相对标准偏差(RSD,n=8)分别为1.7%、4.3%和0.21%;按照实验方法测定含碳锆铝耐火材料样品中氧化锆、氧化铪和氧化铝,与相应国家标准方法比对,结果一致。

Determination of zirconium oxide,hafnium oxide and alumina in carbon-bearing zirconium-aluminum refractory material by X-ray fluorescence spectrometry with fusion sample preparation

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.