熔片制样-波长色散X射线荧光光谱法同时测定铜熔炼渣中15种组分  

Simultaneous determination of 15 components in copper smelting slag by wave-length dispersive X-ray fluorescence spectrometry with fusion sample preparation

作　　者：钟坚海 吴景武 余淑媛 唐梦奇 刘芳美 叶华欣 黄丽 董清木 冯均利 刘明健 ZHONG Jianhai;WU Jingwu;YU Shuyuan;TANG Mengqi;LIU Fangmei;YE Huaxin;HUANC Li;DONG Qingmu;FENG Junli;LIU Mingjian(Technology Center,Xiamen Customs,Xiamen 361026,China;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen 518067,China;Nanning Customs Technology Center,Nanning 530221,China;Zijin Copper Co.,Ltd.,Longyan 364100,China)

机构地区：[1]厦门海关技术中心,厦门361026 [2]深圳海关工业品检测技术中心,深圳518067 [3]南宁海关技术中心,南宁530221 [4]紫金铜业有限公司,龙岩364100

出　　处：《分析试验室》2025年第1期96-101,共6页Chinese Journal of Analysis Laboratory

基　　金：福建省科技计划项目(2021I0032);海关总署科研项目(2022HK060)资助。

摘　　要：铜熔炼渣的基体复杂且含有低价态物质,熔融制样方法的关键在于确保样品的充分熔融和避免坩埚被浸蚀。本实验首先在700℃下采用硝酸钠作为氧化剂对铜熔炼渣进行预氧化,采用X射线衍射仪对预氧化效果进行表征,结果表明铜熔炼渣中铁橄榄石以及铁和铜的硫化物被氧化成CuO,Fe_(2)O_(3)和SiO_(2),说明此时具有很好的氧化效果。进一步采用质量比为12∶22的四硼酸锂和偏硼酸锂(Li_(2)B_(4)O_(7)-LiBO_(2))混合熔剂进行垫底和覆盖,以溴化锂为脱模剂,通过高温熔融获得满足测试要求的均质玻璃片。以采用化学法定值的铜熔炼渣样品、含铜有证标准物质以及上述样品的人工混合样作为校准样品,解决了标准物质缺失的问题。考察了谱线重叠情况和元素间的吸收增强效应,建立了铜熔炼渣中Cu,Fe,SiO_(2),Al_(2)O_(3),S,Mn,CaO,MgO,K_(2)O,Zn,As,Ni,Co,Pb,Sb共15种组分的X射线荧光光谱检测方法。该方法对各元素测定的检出限为5.6~246.8 mg/kg,方法相对标准偏差为0.4%~5.2%,本方法对铜熔炼渣样品的测定值与化学法测定结果一致。The matrix of copper smelting slag is complex and contains low valence substances.The key to the melting sample preparation method is to ensure the full melting of the sample and avoid the erosion of the crucible.In this experiment,the copper smelting slag was pre-oxidized with sodium nitrate as oxidant at 700℃,and the pre-oxidation effect was characterized by X-ray diffractometer.The results showed that fayalite and iron and copper sulfides in copper smelting slag were oxidized to CuO,Fe_(2)O_(3) and SiO_(2),indicating that it had a good oxidation effect.Further,the Li_(2)B_(4)O_(7)-LiBO_(2) mixed flux with a mass ratio of 12∶22 was used as base and cover,and lithium bromide was used as the release agent.Homogeneous glass sheets that meet the test requirements were obtained by high-temperature melting.The copper smelting slag sample with chemical process,the certified reference material containing copper,and the artificial mixed sample of the above samples were used as calibration samples to solve the problem of lack of reference materials.The overlap of spectral lines and the absorption enhancement effect between elements were investigated.The X-ray fluorescence spectrometry method for the detection of 15 components containing Cu,Fe,SiO_(2),Al_(2)O_(3),S,Mn,CaO,MgO,K_(2)O,Zn,As,Ni,Co,Pb,Sb in copper smelting slag was established.The results showed that the detection limits of the method for various elements were 5.6-246.8 mg/kg,and the relative standard deviations were 0.4%-5.2%.The determination results of copper smelting slag samples were consistent with that of chemical method.

关 键 词：X射线荧光光谱法(XRF) 铜熔炼渣 熔片制样 成分 

分 类 号：O657.34[理学—分析化学]