摘要
采用X射线衍射仪对铜精矿及其预氧化效果进行考察,结果表明铜精矿中的铜、铁、硫元素主要以黄铜矿的形式存在;以硝酸钠作为氧化剂,在650℃下氧化30 min后,上述元素转变成氧化铜、三氧化二铁及硫酸盐的形式,从而可以避免熔融过程中坩埚腐蚀和元素的损失。同时,研究了熔剂与样品的比例、脱模剂加入量等关键熔融制样条件对熔片质量的影响。采用溴化锂作为脱模剂,在1050℃下以四硼酸锂和偏硼酸锂混合熔剂(质量比为12∶22)熔融12 min后得到均匀、完整的玻璃片;采用铜矿、铜精矿有证标准物质作为校准标样,并以上述标样的混合样及部分化学法定值实际样品作为补充,建立了具有一定含量梯度且涵盖日常分析所需的校准曲线。另外,还系统研究了仪器电压、电流、谱线重叠等测试条件的影响,建立了铜精矿中铜、铁、硫、氧化钙、氧化镁、二氧化硅、氧化铝、氧化钾、锌、砷、铅、铋、镍、锰、钴、钼等16种元素成分的波长色散X射线荧光光谱法。该方法对各元素成分测定的检测限为0.0010%~0.15%,定量限为0.0033%~0.50%,相对标准偏差为0.14%~10.12%,方法测定结果与有证标准物质标示值基本一致。
The pre-oxidation effect of copper concentrate was investigated using an X-ray diffractometer.The results showed that copper,iron and sulfur in copper concentrate were primarily present as chalcopyrite(CuFeS2).After oxidation at 650°C for 30 min with sodium nitrate as oxidant,the above elements were transformed into CuO,Fe2O3 and sulfate,so as to avoid crucible corrosion and element loss.The effects of key melting conditions,such as the flux-to-sample ratio and the release agent on the quality of the fused sheet were investigated.Lithium bromide was used as a release agent,and a mixture of lithium tetraborate and lithium metaborate(Li2B4O7-LiBO2) was used for melting in a mass ratio of 12:22.Uniform and complete glass sheets were obtained after melting at 1050°C for 12 min.A calibration curve,designed to meet daily analytical requirements,was established using certified reference materials from copper ore and copper concentrate as calibration standards,supplemented with a mixture of these standards and some actual samples.The effects of test conditions such as instrument voltage,current,and spectral overlap were systematically studied,and the wavelength dispersive X-ray fluorescence spectrometry method for the detection of 16 elements such as Cu,Fe,S,CaO,MgO,Si O2,Al2O3,K2O,Zn,As,Pb,Bi,Ni,Mn,Co,and Mo in copper concentrate was established.The detection limits of the method ranged from 0.0010% to 0.15%,with quantitative limits between 0.0033% and 0.50%,and the relative standard deviation(RSD) was 0.14%-10.12%.The results obtained using this method were consistent with the certified reference materials.
作者
肖彦亮
张艳燕
陈权
刘芳美
黄丽
钟坚海
冯均利
兰淑惠
XIAO Yan-Liang;ZHANG Yan-Yan;CHEN Quan;LIU Fang-Mei;HUANG Li;ZHONG Jian-Hai;FENG Jun-Li;LAN Shu-Hui(Technology Center,Xiamen Customs,Xiamen 361026;Xiamen Customs Cross Strait Agricultural Products Technology Center,Xiamen 361026;Zijin Copper Co.,Ltd.,Longyan 364100;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen 518067;China Certification&Inspection Group Guangxi Co.,Ltd.,Nanning 530000)
出处
《中国口岸科学技术》
2024年第11期60-66,共7页
China Port Science and Technology
基金
福建省科技计划项目(2021I0032)。
关键词
X射线荧光光谱法
铜精矿
预氧化
熔片制样
元素
s X-ray fluorescence spectrometry
copper concentrate
pre-oxidation
fusion sample preparation
elements
