建立了高温氯盐法处理含铅锡物料时高铅氯盐溶液中锡的测定方法.研究发现,在草酸盐酸亚甲基蓝的底液中,Sn(Ⅳ)在 0.5V处有一灵敏的极谱波,Sn(Ⅳ)与pb2+、Cd2+峰电位相隔100mV,可以利用微分脉冲伏安极谱法测定锡.对于0.25 mg/L的锡,至少1 000倍的Cl、Na+、K+、F、SO42-、NO3-,200倍Cu2+、Fe3+、Zn2+、Al3+、Mn2+,100倍Ca2+、Mg2+、Cr3+、Sb3+、Bi3+,50倍Ni2+、Co2+,30倍As3+、Pb2+、Cd2+不干扰测定.在选定试验条件下,采用标准加入法对样品进行测定,测定值相对标准偏差小于2%,回收率在98.8%~104.2%之间.方法可应用于高铅氯盐溶液中锡的测定.
A method for the determination of tin was established in high-lead chloride salt solution. The solution was produced in precessing the lead-tin materials by high temperature chloride salt method. A sensitive polarographic wave of Sn(IV) was found at -0.5 V during the determination of tin in oxalic acid-hydrochloric acid-methylene blue solution by differential pulse voltammetry polarography. The overlapping of peak position of Pb2+ , Cd2+ with Sn4+ was solved. The results shown that the peak position of Sn4+ was separated from Pb2+ and Cd2+ and the gap was about 100 mV. For the determination of 0.25 mg/L Sn4+ in high-lead chloride salt solution,1 000 times of Cl-, Na+ , K+ , F-, SO4-, NO3- ; 200 times of Cu2+ , Fe3+ , Zn2+ , Al3+ , Mn2+ ; 100 times of Ca2+ , Mg2+ , Cr3+ , Sb3+ , Bi3+ ; 50 times of Ni2+ , Co2+ ; 30 times of As3+ , Pb2+ and Cd2+ did not interfere in the determination at least. Under the optimum experimental conditions, the sample was determined with standard addition method,with the relative standard deviation of 2% and the recovery of 98.8%-104.2%. The proposed method could be applied to determine tin in high-lead chloride salt solution.