火花源原子发射光谱法测定银中铜铋铁铅锑钯硒碲

Spark source atomic emission spectrometric determination of copper,bismuth,iron,lead,antimony,palladium,selenium and tellurium in silver

探讨了火花源原子发射光谱法分析银中杂质元素铜、铋、铁、铅、锑、钯、硒和碲的分析条件、样品处理方法,确定了各杂质元素测定范围.采用对测定结果无明显影响的车床或压样机加工样品表面,用盐酸（1＋9）去除试样表面的沾污,校准曲线采用仪器内置的纯银标准曲线,并通过内部质量控制样品和校正样品监控.实验方法用于纯银标准样品中8种元素的分析,测定值与认定值一致;对银锭样品进行分析,各元素11次测定结果的相对标准偏差在1.0％～4.0％之间.方法可用于纯银和银锭中包括钯的杂质元素分析.

This research focused on illustrating the analysis conditions and sample processing method for the determination of the impurity elements, such as copper, bismuth, iron, lead, antimony, palladium, selenium and tellurium, in silver by spark source atomic emission spectrometry. The detection ranges of impurity elements were determined, as well. The sample surface was processed by presser or lathe without significant effect on the measurement results. Hydrochloric acid （1＋9） was used to remove the contaminations which attached to the sample surface. The built-in sterling silver standard curve was used as calibration curve. The samples for internal quality control and calibration were used monitored. The method was applied to analyze eight elements in sterling silver samples. The results were consistent with the reference values. The relative standard deviation （RSD） of eleven test results was 1.0%-4. 0%. The method can be applied to the analysis of impurity elements including palladium in silver and silver ingot.