熔融制样-X射线荧光光谱法测定锰铁中锰硅磷

来源期刊：冶金分析2011年第6期

论文作者：李京

文章页码：51 - 53

关键词：X射线荧光光谱法； 熔融制样； 锰铁； 锰； 硅； 磷

Key words：X-ray fluorescence spectrometry； fusion sample preparation； ferromanganese； manganese； silicon； phosphorus

摘    要：锰铁试样以水和硝酸于铂黄坩埚中溶解并蒸干,加入Co元素为Mn元素内标,以四硼酸锂为熔剂、溴化钾为脱模剂,熔融制作玻璃熔片,在X射线荧光光谱仪上测定锰、硅和磷的含量。本法采用少量水浸润试样并滴加硝酸溶解的试样前处理方法,可保证溶解反应温和且不致试样扑溅损失,有效避免了锰铁熔融过程中坩埚腐蚀问题。同时采用大稀释比、内标法减少了基体干扰。对不同生产单位的标准样品进行测定,测定值与认定值相吻合,各元素测定结果的相对标准偏差(n=11)为0.25%~1.9%。

Abstract: The ferromanganese sample was dissolved in a platinum-gold crucible with water and nitric acid and evaporated to dryness.Then,manganese,silicon and phosphorus in sample were determined by X-ray fluorescence spectrometry with sample fusion preparation using Co as internal standard for Mn,Li₂B₄O₇ as flux and KBr as release agent.In this study,the sample got wet with a little water first and then dissolved by dripping nitric acid,which could not only guaranteed the mild dissolution reaction without loss of sample due to splashing,but also effectively avoided the corrosion of crucible in the fusion of ferromanganese samples.Meanwhile,the large dilution ratio and internal standard method were used to reduce matrix interference.The proposed method has been applied to the determination of certified reference materials from different production units.The determination results were consistent with the certified values,and the relative standard deviations (RSD,n=11) were 0.25%-1.9%.