熔融制样-X射线荧光光谱法测定不锈钢除尘灰中铁铬镍

来源期刊：冶金分析2011年第5期

论文作者：刘伟 王珺

文章页码：27 - 30

关键词：熔融制样； X射线荧光光谱法； 不锈钢除尘灰； 铁； 铬； 镍

Key words：sample preparation by fusion； X-ray fluorescence spectrometry； stainless steel dedust ash； iron； chromium； nickel

摘    要：采用玻璃熔片法制样,以人工合成样品制作校准曲线,建立了不锈钢除尘灰中Fe、Cr和Ni的X射线荧光光谱分析方法。对样品熔片的制备和分析结果的可靠性进行考察。结果表明,采用铂-黄坩埚(w(Pt)∶w(Au)=95%∶5%)熔样,以硝酸铵和过氧化钠作氧化剂,溴化铵作脱模剂,四硼酸锂作熔剂并控制稀释比为1∶30,按照四硼酸锂、硝酸铵、试样、过氧化钠、四硼酸锂的顺序将它们平铺在坩埚中,然后在600℃下熔融10 min,取出后加入溴化铵,再在熔融机中熔融15 min,则得到表面光洁、无可见晶斑的玻璃熔片,并且坩埚不被腐蚀。用本文拟定的测定条件对熔片中的铁、铬、镍进行X射线荧光光谱法测定并进行结果对照,表明本法测得值与湿法测定值一致,铁、铬、镍测定结果的相对标准偏差分别为0.30%、0.87%、1.4%。

Abstract: The X-ray fluorescence spectrometric determination of iron,chromium and nickel in stainless steel dedust ash was established with sample preparation by glass fusion piece method.The calibration curve was plotted using artificially synthesized samples.The preparation of sample fusion piece and the reliability of analytical results were investigated.The results showed that the fusion pieces with finishing surface and without visible crystal spot could be obtained under the following conditions: the sample was fused in platinum-gold crucible(w(Pt)∶w(Au)=95 %∶5 %);the ammonium nitrate and sodium peroxide were used as oxidant;the ammonium bromide was used as release agent;the lithium tetraborate was the flux;the dilution ratio was 1∶30;the reagents were laid in the crucible in the order of lithium tetraborate,ammonium nitrate,sample,sodium peroxide and lithium tetraborate;the mixture was fused at 600 ℃ for 10 min;then,ammonium bromide was added;the mixture was finally fused in fusion machine for 15 min.Moreover,the crucible was not corroded.The iron,chromium and nickel in fusion piece were determined by X-ray fluorescence spectrometry under the selected conditions.The results were compared.It showed that the results found by this method were consistent with those obtained by wet method.The relative standard deviations(RSDs) for iron,chromium and nickel were 0.30%,0.87% and 1.4%,respectively.