火焰原子吸收光谱法测定锑矿石中锑  

Determination of antimony in antimony ore by flame atomic absorption spectrometry

作　　者：王小强 梁倩 赵亚男 张会 张丽曼 颜蕙园 WANG Xiaoqiang;LIANG Qian;ZHAO Yanan;ZHANG Hui;ZHANG Liman;YAN Huiyuan(Henan Academy of Geology,Zhengzhou 450016,China;General Institute for Non-ferrous Metals and Geological Exploration of Henan Province,Zhengzhou 450016,China;Henan Nonferrous Metals Deep Prospecting Engineering Technology Research Center,Zhengzhou 450016,China)

机构地区：[1]河南省地质研究院,河南郑州450016 [2]河南省有色金属地质勘查总院,河南郑州450016 [3]河南省有色金属深部找矿工程技术研究中心,河南郑州450016

出　　处：《冶金分析》2023年第3期57-63,共7页Metallurgical Analysis

基　　金：河南鑫利源地矿有限公司2021年度科技创新项目(YS202104)。

摘　　要：锑矿石中锑含量是进行矿床评价和工业选冶试验的重要指标,准确测定锑矿石中锑含量具有重要的指导意义。分别加入硫酸、硝酸冒硫酸烟溶解样品,利用柠檬酸可与锑形成络合物的特性,用柠檬酸-盐酸混合酸加热煮沸提取锑,解决了锑易在盐酸中水解从而导致测定结果偏低的难题,使用空气-乙炔火焰,以231.147 nm为测定波长,建立了火焰原子吸收光谱法(FAAS)测定锑矿石中锑的方法。锑矿中往往伴生砷和硫,砷的干扰试验表明,其对测定的干扰可忽略不计,而硫因与提取液中的盐酸反应生成硫化氢气体逸出也不干扰测定。按照实验方法对锑矿石成分分析标准物质进行处理,分别采用电感耦合等离子体原子发射光谱法(ICP-AES)和火焰原子吸收光谱法对试液中锑进行测定,结果表明,FAAS测定值与认定值基本一致,ICP-AES测定值比认定值偏低,这可能与ICP-AES雾化器进样毛细管管径比FAAS小,试液中残存的少量硫酸粘附在雾化器进样毛细管内侧,导致试液的提升量变小有关。在优化的实验条件下,锑质量浓度为2~10μg/mL范围内与其对应的吸光度呈良好的线性关系,其相关系数为0.999 6,方法检出限为0.1μg/g,定量限为0.3μg/g。应用实验方法测定锑矿石成分分析标准物质和锑矿石实际样品中锑的含量。结果表明,对于实际样品,测定结果的变异系数(CV)为0.75%~2.2%,对于标准物质,测定结果的相对误差(RE)为-0.76%~1.10%,分别满足标准GB/T 27417—2017和标准DZ/T 0130.3—2006对测定结果变异系数及相对误差的要求。The content of antimony in antimony ore is an important index for ore deposit evaluation and industrial beneficiation test.Therefore,the accurate determination of antimony content in antimony ore has an important guiding significance.The sample was dissolved by sulfuric acid smoking in sulfuric acid and nitric acid.Based on the characteristic that citric acid could react with antimony to form a complex,antimony was extracted by heating and boiling with citric acid-hydrochloric acid mixed acid.It solved the problem that antimony was easily hydrolyzed in hydrochloric acid,which caused low determination results.Thus,a method for determination of antimony in antimony ore was established by flame atomic absorption spectrometry(FAAS) with air-acetylene flame at wavelength of 231.147 nm.Arsenic and sulfur are often associated in antimony ores.The interference test of arsenic showed that its interference could be ignored.Since sulfur could react with hydrochloric acid in extracting solution to form hydrogen sulfide,which would be released and had no interference with the determination.The certified reference materials of antimony ore for composition analysis were treated according to the proposed method,and the contents of antimony in the test solution were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES) and flame atomic absorption spectrometry,respectively.The results showed that the measured values of FAAS were basically consistent with the certified values,while the measured values of ICP-AES were lower than the certified values.This might be related to the fact that the tube diameter of nebulizer injection capillary of ICP-AES was smaller than that of FAAS,and a small amount of sulfuric acid remained in test solution adhered to the inside of the nebulizer injection capillary,resulting in a smaller lifting volume of the test solution.Under the optimized experimental conditions,the mass concentration of antimony in range of 2-10 μg/mL showed a good linear relationship with its correspond

关 键 词：锑矿石 柠檬酸 锑 火焰原子吸收光谱法(FAAS) 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]