Abstract:The noble lead sample was scanned and analyzed by energy dispersion X-ray spectrometer (EDX) and X-ray diffractometer (XRD). The results showed that the noble lead was mainly composed of lead, silver, bismuth, iron, antimony, copper, arsenic and tellurium. Moreover, the phases of silver mainly included silver-antimony alloy, silver-bismuth alloy, elemental silver and silver-arsenic alloy. The noble lead sample was treated and dissolved with nitric acid. It was found that gray white precipitate could be formed due to the hydrolysis of antimony. Based on the complex reaction between tartaric acid and antimony, the hydrolysis of antimony compounds could be effectively prevented by adding tartaric acid. Consequently, a determination method of silver in noble lead by potentiometric titration was established after dissolving the sample with mixed nitric acid and tartaric acid. The experimental conditions were optimized. The interference test of coexisting impurity elements in noble lead sample was conducted. The results showed that the interference of coexisting elements could be ignored. The proposed method was applied for determination of silver in three noble lead samples. The relative standard deviations (RSD, n=6) of determination results were between 0.18% and 0.21%. The recoveries were between 99% and 101%. The noble lead actual sample was analyzed according to the experimental method. The results were in good agreement with those obtained by fire assaying-gravimetric method.
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