熔融制样-波长色散X射线荧光光谱法测定高硫高磷铜磁铁矿中主次成分  

Determination of major and minor components in high-sulfur and high-phosphorus copper magnetite by wavelength dispersion X-ray fluorescence spectrometry with fusion sample preparation

作　　者：褚宁[1] 蒋晓光[1] 张彦甫[1] 

机构地区：[1]鲅鱼圈出入境检验检疫局,辽宁营口115007

出　　处：《冶金分析》2015年第12期10-16,共7页Metallurgical Analysis

基　　金：工信部行业标准计划项目(2013-0346T-YS)

摘　　要：铜磁铁矿属富铜、高硫、高磷的磁铁矿矿物,以测量灼烧减量后的灼烧基试料质量作为试料量,建立了熔融制样-波长色散X射线荧光光谱法测定铜磁铁矿中铜、铁、硅、铝、钙、镁、钛、锰和磷含量的分析方法。以四硼酸锂-偏硼酸锂混合熔剂（m∶m=12∶22）为熔剂,控制试料与熔剂稀释比为1∶10,以220mg/mL硝酸锂溶液为氧化剂,50mg/L碘化铵溶液为脱模剂,于1 050℃熔融20min,制备的试料片透彻、玻璃化程度高。以磁铁矿标准物质为基体,并添加铜和磷标准溶液作为标准试料,解决了铜磁铁矿没有标准物质的问题。各待测组分校准曲线的相关系数在0.989 0-0.999 9之间;方法检出限为0.001 7%-0.30%;各待测组分的相对标准偏差（RSD,n=11）在0.15%-4.7%之间。对与铜磁铁矿基体组分相近的含铜铁矿石标准物质进行测定,测定值与认定值基本一致;采用不同实验方法对不同含量水平的铜磁铁矿样品进行测定,测定值与滴定法、重量法、电感耦合等离子体原子发射光谱法（ICP-AES）、原子吸收光谱法（AAS）和分光光度法的测量结果基本相符。8个实验室对8个不同含量水平的铜磁铁矿样品进行了协同试验,结果表明方法的重复性和再现性良好。The copper magnetite belonged to the rich-copper,high-sulfur and high-phosphorus magnetic ore.Using the mass of burned sample after measurement of loss on ignition as sample mass,an analysis method of copper,iron,silicon,aluminum,calcium,magnesium,titanium,manganese and phosphorus in copper magnetite was established by wavelength dispersion X-ray fluorescence spectrometry with fusion sample preparation.The lithium tetraborate-lithium metaborate mixture（m∶m=12∶22）was used as flux.The dilution ratio between sample and flux was controlled at 1∶10.The lithium nitrate solution（220mg/mL）and ammonium chloride solution（50mg/L）was used as oxidizer and release agent,respectively.The sample was fused at 1 050 ℃for 20 min.The prepared specimens were transparent with high vitrification degree.The certified reference material of magnetite was used as matrix to prepare reference material of copper magnetite by adding the standard solution of sulfur and phosphorus which solved the problem of copper magnetite without certified reference material.The correlation coefficients of calibration curves of testing components were between 0.989 0and 0.999 9.The detection limit of method was 0.0017%-0.30%.The relative standard deviations（RSD,n=11）were between 0.15%and 4.7%.The certified reference material of copper-bearing iron ore with similar composition to copper magnetite matrix was determined by the proposed method,and the results were consistent with the certified values.The copper magnetite samples with different content level were determined by the proposed method,and the results were basically consistent with those obtained by titrimetry,gravimetry,inductively coupled plasma atomic emission spectrometry（ICP-AES）,atomic absorption spectrometry（AAS）and spectrophotometry.The synergism tests of eight copper magnetite samples with different content level in eight laboratories were conducted.The results indicated that the repeatability and reproducibility of the proposed method was good.

关 键 词：波长色散X射线荧光光谱法 熔融制样 铜磁铁矿 高硫 高磷 主次成分 

分 类 号：O657.34[理学—分析化学]