摘要
通过对铜冶炼渣化学组成和性质的研究,确定了测定镍的实验方法.铜冶炼渣中二氧化硅含量在20％～40％,硫含量10％～20％,样品的分解具有一定的难度,必然影响镍的测定结果,因此需在样品分解过程中加入一定量的氟化氢铵、溴使二氧化硅生成四氟化硅、硫生成硫化氢挥发除去,溶液中其余共存元素主要有铜、银、铁、锌等元素不干扰测定结果,在硝酸（5％）介质中,用火焰原子吸收光谱法测定镍的含量,测定范围为0.01％～1％,加标回收率在99.5％～100.4％,测定结果的相对标准偏差（n=7）在0.61％～1.18％,检出限为0.004 μg/mL,方法快速,简捷,能够满足日常生产检测需要.
Through the study on chemical composition and properties of copper smelting slag, the experimental method for the determination of nickel was established. In copper smelting slag, silica content is about 20%-40% and the sulfur content is about 10% - 20%. Such high silica and sulfur contents bring some difficulties to the sample decomposition, which inevitably influence the determination of nickel. To overcome this problem, a certain amount of ammonium hydrogen fluoride and bromide are added to the sample during sample decomposition process. Due to the reaction between silica and ammonium hydrogen fluoride, which generates silicon tetrafluoride, and the reaction between sulfur and bromide, which generates hydrogen sulfide, the influence of silica and sulfur was eliminated. Afterwards, the rest of coexisting elements in the solution mainly are copper, silver, iron, and zinc etc. , which do not interfere with the determination results. In 5% （V/V） nitric acid medium, the content of nickel was determined by flame atomic absorption spectrometry. The concentration ranges were from 0.01% to 1 %. The recovery rates were 99. 5%-100. 4%. The relative standard deviations （n=7） were 0. 61%-1. 18% and the detection limit was 0. 004μg/mL. The method is rapid, simple, and can meet the need of daily production inspection.
出处
《中国无机分析化学》
CAS
2014年第1期63-65,共3页
Chinese Journal of Inorganic Analytical Chemistry
关键词
火焰原子吸收光谱法
铜冶炼渣
镍
flame atomic absorption spectrometry
copper smelting slag
nickel
