铋试金-高分辨率连续光源火焰原子吸收光谱法测定矿石中的痕量金  

Determination of Trace Au in Minerals by Bismuth Fire Assay with Enrichment-high Resolution Continuum Source Flame Atomic Absorption Spectrometry

作　　者：王甜甜 郭晓瑞 樊蕾 毛香菊[1] 刘闫 倪文山[1] WANG Tiantian;GUO Xiaorui;FAN Lei;MAO Xiangju;LIU Yan;NI Wenshan(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,China National EngineeringResearch Center for Utilization of Industrial Minerals,Key Laboratory for Polymetallic Ores'Evaluation andUtilization,MNR,Zhengzhou 450006,Henan,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,国家非金属矿资源综合利用工程技术研究中心,自然资源部多金属矿评价与综合利用重点实验室,河南郑州450006

出　　处：《矿产综合利用》2024年第4期128-133,共6页Multipurpose Utilization of Mineral Resources

基　　金：国家自然科学基金项目[22106148]。

摘　　要：这是一篇分析测试领域的论文。铋试金作为一种高效分离富集矿石中痕量贵金属的绿色环保火试金方法,有效避免了铅试金有毒污染的问题。本篇采用低毒的Bi_(2)O_(3)作为Au元素的火试金捕集剂,在高温熔融过程中Bi_(2)O_(3)经试金配料中的还原剂面粉还原为Bi后,与样品中的Au形成Au_(2)Bi合金,并采用Ag保护灰吹法使Au与Ag形成约1 mg的Ag合粒;对Ag合粒采用酸溶法将其加热溶解,使Au完全进入溶液。本实验以国家标准物质GBW 07205中Au元素含量为参考,对连续光源火焰原子吸收光谱仪的CCD检测器有效像素点进行了优化选择,综合其灵敏度和稳定性,选择7作为CCD检测器的有效像素点。在质量浓度0~20μg/mL范围内与其对应吸光度运用二次方程最小二乘法拟合校准曲线,校准曲线拟合系数为0.9998;特征浓度为0.06997μg/mL,方法检出限为0.0127μg/mL。按照选定实验方法及优化仪器参数下对国家标准物质中Au进行测定,测定值与标准值吻合良好,相对标准偏差(RSD,n=6)为2.23%~4.54%。将所建立的方法应用于实际矿石样品中Au的测试,加标回收率为92.6%~106%;相对标准偏差(n=6)为2.53%~4.70%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。This is an article in the field of analytical testing.As a green and environmentally friendly fire gold test method for efficient separation and enrichment of trace precious metals in ore,bismuth gold test effectively avoids the problem of toxic pollution of lead test gold.In this article,Bi2O3 with low toxicity is used as the fire test gold trap of Au element,and Bi2O3 is reduced to Bi by the reducing agent flour in the test ingredient during the high-temperature melting process,and Au2Bi alloy is formed with Au in the samples,and the Ag protective ash blowing method is used to make Au and Ag form about 1mg of Ag zygote.The Ag zygoteum is heated and dissolved by acid solution method to completely enter the solution of Au.In this test,the Au element content in the national standard material GBW 07205 was used as a reference,and the effective pixels of the CCD detector of the continuous light source flame atomic absorption spectrometer were optimized,and 7 were selected as the effective pixels of the CCD detector based on their sensitivity and stability.In the mass concentration range of 0~20μg/mL,the corresponding absorbance was fitted by the quadratic equation least squares method,the fitting coefficient of the calibration curve was 0.9998,the characteristic concentration was 0.06997μg/mL,and the detection limit of the method was 0.0127 g/mL.According to the selected experimental method and optimized instrument parameters,Au in the national standard material was determined,and the measured value was in good agreement with the standard value,and the relative standard deviation(RSD,n=6)was 2.23%~4.54%.The established method was applied to the test of Au in actual ore samples,and the recovery rate of spiked was 92.6%~106%.The relative standard deviation(n=6)was 2.53%~4.70%,which met the requirements of the National Geological and Mineral Resources Industry Standard DZ/T 0130-2006.

关 键 词：分析测试 铋试金 Ag保护灰吹法 Au 连续光源火焰原子吸收光谱法 

分 类 号：P575.3[天文地球—矿物学]