燃烧-电导法测定电解镍粉中的硫量

本文提出了铝箔-磷酸·硼酸混合液组成的除氯、除氟体系,有效地消除氟、氯等元素对硫的电导法测定的干扰;系统地研究了铝箔的用量、燃烧温度、燃烧时间、氧气流速对除氯、除氟和二氧化硫的析出及测定的影响。提出了采用燃烧-电导法测定电解镍粉中硫含量的最佳条件。本法测定含硫量为0.0020%的镍粉试样时,相对标准偏差为0.0002%,硫的回收率为98.38%,检测下限为0.0002%,该法操作简便,测量下限低,结果准确可靠,经济实用。

Determination of Sulphur in Electrolytic Nickel Powder by Combustion-Conduction Method

A chlorine and fluorine removal system consisting of the mixture of aluminium foil,phosphate and borate is presented. The system effectively eliminates the F & Cl interference of the determination of S by the conduction method. This paper systematically discusses the amount of aluminium foil,combustion temperature,combustion time,the effect of oxygen flowrate on the segregation and determination of Cl,F and SO2. The best condition for the determination of S in electrolytic nickel powder by the combustion-conduction method is given. When the nickel powder sample with the S content of 0.0020% is tested through the method,the relative standard deviation is 0.0002%,the S recovery rate 98.38%,the lower limit of determination 0.0002%. The method is characterized by easy operation,lower limit of determination,accurate and reliable results and economic and practical effect.