硝化后熔融制样法——X射线荧光光谱同时测定锰矿中主、次元素  

Method of Fused Sample Preparation after Nitrify—Determination of Primary and Minor Elements in Manganese Ore by X-Ray Fluorescence Spectrometry

作　　者：宋义[1] 郭芬[1] 谷松海[1] 

机构地区：[1]天津出入境检验检疫局化矿实验室,天津塘沽300456

出　　处：《光谱学与光谱分析》2007年第2期404-407,共4页Spectroscopy and Spectral Analysis

摘　　要：采用X射线荧光光谱法同时测定锰矿中Mn,SiO2,Fe,P,Al2O3,CaO,MgO和S等8个组分。因锰矿熔融制样过程中产生气泡现象严重,影响到测定的准确性和重现性,文章提出了先加硝酸破坏锰矿样品中的有机物,然后用12∶22混合熔剂在1000℃熔融制样的方法,解决了锰矿熔融制样过程中有机物挥发产生大量的气泡导致熔剂飞溅的问题,消除了试样的粒度效应和矿物效应,同时也解决了硫元素在制样过程中容易挥发的难题。对熔剂、熔融时间、硝酸加入量等制样条件进行了选择,并采用可变理论α系数法校正基体的吸收增强效应,扩大了测定线形范围,进行了方法的精密度及准确度试验。与化学法对比,本法测定锰矿中各组分的定量分析结果令人满意,方法准确、快速、简便。Eight components, i.e. Mn, SlOe, Fe, P, AlcOa, CaO, MgO and S, in manganese ore were determined by X-ray fluorescence spectrometer. Because manganese ore sample releases a lot of air bubbles during fusion which effect accuracy and reproducibility of determination, nitric acid was added to the sample to destroy organic matter before fusion by the mixture flux at 1 000℃. This method solved the problem that the flux splashed during fusion because organic matter volatilized brought out a lot of air bubbles, eliminated particle size effects and mineral effect, while solved the problem of volatilization of sulfur during fu- sion. The experiments for the selection of the sample preparation conditions, i.e. fusion flux, fusion time and volume of HNOa, were carried out. The matrix effects on absorption and enhancement were corrected by variable theoretical alpha coefficient to expand the range of determination. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.

关 键 词：X射线荧光光谱 锰矿 硝化后熔融制样 制样 

分 类 号：O657.3[理学—分析化学]