铜阳极泥是一种重要的冶金工业副产品, 因其中含有多种贵金属和有价金属元素, 铜阳极泥的综合回收利用日益受到关注。 铜阳极泥预处理富集渣中富含的Sb难以用常规方法溶解, 有必要建立一种准确、 简便的测试方法实现Sb的定量分析。 采用X射线荧光光谱、 X射线衍射光谱和场发射扫描电镜能谱分析等多种光谱学分析手段对富集渣的化学成分、 物相和微观结构做了全面分析, 结果表明, 富集渣的化学组成和物理结构复杂, 组分化学性质稳定且共生紧密。 Sb以高锑酸金属化合物的形式存在, 结构稳定化学惰性强。 采用Na2O2熔融法消解试样, 合成标准样品做标准系列, 用火焰原子吸收光谱法测定了富集渣中Sb的含量值为8.23%, 相对标准偏差为0.97%。 该方法的检出限为0.072%, 加标回收率为94.9%~99.2%。 本方法溶样彻底, 不需贵重试剂和仪器, 方法简单易行。 采用与样品基体相近的合成标准样品, 消除了样品化学成分复杂所造成的共存物质干扰。 通过标准样品测试验证和其他仪器方法比对, 证明本方法灵敏度高, 准确性好, 可用于铜阳极泥预处理渣料中Sb的定量测定。

Copper anode smile is an important by-product of metallurgical industry which contains a variety of precious metals and valuable metals, so that its comprehensive recycling and utilization is increasingly concerned. It is difficult to use conventional method to dissolve the Sb in pretreated residue of copper anode slime (enriched slag). Therefore, it is necessary to develop an accurate and simple method to realize the quantitative analysis of Sb. Here, a comprehensive analysis method was developed for the chemical composition, phase and microstructure of the enriched slag by means of X-ray fluorescence spectroscopy, X-ray diffraction and field emission scanning electron microscopy by using alkali fusion procedure. The analysis results showed that the chemical composition and physical structure of the enriched slag are complex, and its components are chemical stable and intergrowth closely. Sb exists in the form of high state antimony acid salt with a stable structure. The samples were digested by Na2O2 fusion method, and the standard series of synthetic standard samples were synthesized. The content of Sb in the enriched slag by flame AAS was 8.23% with the relative standard deviation of 0.97%, the detection limit of 0.072% and the recoveries of 94.9%～99.2%. Here, the enriched slag can be completely dissolved by this simple method, which does not require the use of special reagents and instruments. Because the synthetic standard sample is similar to the actual sample, the interference of coexisting substances caused by the complicated chemical composition can be eliminated. This method with high sensitivity and good accuracy in comparison experiment, can be used for the quantitative determination of Sb in pretreated copper anode slime.