ICP-OES法测定磷铁中硅、锰、钛、钒、铬元素  

Determination of silicon,manganese,titanium,vanadium,and chromium in phosphorus iron by ICP-OES

作　　者：陈娜 任楠 金婷婷 CHEN Na;REN Nan;JIN Tingting(Test Center of Geological Geophysical and Chemical Exploration Institute,Yunnan Nonferrous Geological Bureau,Kunming 650216,China)

机构地区：[1]云南省有色地质局地质地球物理化学勘查院测试中心,云南昆明650216

出　　处：《中国有色冶金》2024年第2期93-99,共7页China Nonferrous Metallurgy

摘　　要：针对目前电感耦合等离子体发射光谱法(ICP-OES)测定磷铁样品杂质元素含量存在的样品溶解问题,本文采用氢氧化钠+碳酸钠对被检测磷铁进行一次熔样,然后使用电感耦合等离子体发射光谱仪对样品中的硅、锰、钛、钒、铬进行测定。测定结果表明,本文测定各元素检出限为0.0016%~0.0080%,测定下限为0.0064%~0.032%,结果与标准样品各元素含量相对误差RE均小于5%,加标回收率为95.1%~102.4%,相对标准偏差小于5%,且三个实际样品RSD均小于5%,故表明此方法精密度及准确度良好,能够满足检测要求。该方法克服了磷铁样品难溶解的特点,并在短时间内获得理想检测结果,而且测定结果具有很高稳定性、精密度和准确度。本试验方法具有可重复性,流程短、成本低,适用于大批量样品的快速分析,可成为检测磷铁产品的一种更简单、快速、经济的重要手段。In order to solve the problem of sample dissolution in the determination of impurity elements in ferric phosphorus samples by inductively coupled plasma emission spectrometry(ICP-OES),this paper uses sodium hydroxide+sodium carbonate to melt the tested ferric phosphorus samples,and then uses inductively coupled plasma emission spectrometer to determine silicon,manganese,titanium,vanadium and chromium in the samples.The results showed that the detection limit of each element was 0.0016%~0.0080%and the lower limit was 0.0064%~0.032%.The relative error RE of each element content between the results and the standard sample was less than 5%,the recovery rate was 95.1%~102.4%,and the relative standard deviation was less than 5%.RSD of the three actual samples is less than 5%,which indicates that the method has good precision and accuracy,and can meet the detection requirements.The method overcomes the insoluble characteristics of the phosphorus and iron samples,and obtains the ideal detection results in a short time,and the determination results have high stability,precision and accuracy.The test method has the advantages of repeatability,short process and low cost,and is suitable for rapid analysis of large quantities of samples.It can be used as a simple,rapid and economic important means to detect iron phosphorus products.

关 键 词：磷铁 电感耦合等离子体发射光谱法 样品溶解 硅、锰、钛、钒、铬 短流程检测 低成本分析 

分 类 号：TF03[冶金工程—冶金物理化学]