Abstract:When the content of silver in noble bismuth sample was determined after enrichment by lead fire assaying, bismuth would interfere the enrichment of silver which lead to lower determination results of silver. The sample was dissolved with nitric acid, ammonium fluoride and perchloric acid. EDTA solution was added for the complexing of bismuth. Sodium chloride was added to react with silver to form silver chloride precipitation while the bismuth was remained in solution. The separation of bismuth and silver was achieved by filtration, thus eliminating the interference of bismuth with the enrichment of silver. Then, the silver in precipitation was enrichment into composite granule by lead fire assaying. The composite granule was dissolved with nitric acid for the determination of silver by sodium chloride potentiometric titration. Consequently, an analysis method of silver in noble bismuth was established by precipitation separation-lead fire assaying enrichment-sodium chloride potentiometric titration. The influence of coexisting components (bismuth, calcium, lead, iron, zinc, tin, antimony, arsenic, copper and gold) in noble bismuth on the determination of silver was discussed. The results showed that the coexisting components in samples did not interfere with determination of silver. The experimental method was applied for determination of silver in four actual samples of noble bismuth. The relative standard deviations (RSD, n=10) of determination results were between 0.26% and 0.68%. The spiked recoveries ranged from 99% to 101%. The determination results were consistent with those obtained by gravimetry.
夏兵伟.铋试金法测定高铋物料中的银[J].中国无机分析化学,2015,5(1):49-52.XIA Bing-wei.Determination of silver in high bismuth slag by bismuth fire assaying method[J].Chinese Journal of Inorganic Analytical Chemistry,2015,5(1):49-52.
[3]
刘秋波,肖一然,李文莉.硫氰酸钾电位滴定法测定铜冶炼分银渣中的银量[J].中国无机分析化学,2018,8(4):47-50.LIU Qiu-bo,XIAO Yi-ran,LI Wen-li.Determination of silver in copper smelting silver slag by automatic potentiometric titration method with potassium thiocyanate[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(4):47-50.
[4]
肖刘萍.灰吹富集-氯化钠电位滴定法测定贵铅中银[J].冶金分析,2018,38(3):56-60.XIAO Liu-ping.Determination of silver in noble lead by cupellation enrichment-sodium chloride potentiometric titration method[J].Metallurgical Analysis,2018,38(3):56-60.
[5]
吴敏.氯化铅共沉淀-硫氰酸钾容量法测定铅阳极泥中银[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2015,51(12):1750-1752.
盛建林.铅试金重量法结合数学校正法测定银[J].冶金分析,2016,36(9):9-18.SHENG Jian-lin.Determination of silver by lead fire assaying gravimetry combined with mathmetic correction[J].Metallurgical Analysis,2016,36(9):9-18.
[8]
魏巍.铅试金重量法结合原子吸收光谱法测定银钯精矿中银[J].冶金分析,2018,38(1): 64-69.WEI Wei.Determination of silver in silver-palladium concentrate by lead fire assaying gravimetry combined with atomic absorption spectrometry[J].Metallurgical Analysis,2018, 38(1): 64-69.