摘要
针对冰铜中硫含量高不易被完全氧化的特点，采用氧化锌-碳酸钠-高锰酸钾为熔剂，建立了重量法测定冰铜中总硫含量的方法。确定了碳酸钠、氧化锌、高锰酸钾混合熔剂的最佳质量比为10：10：1；最佳熔融温度为750~800℃。试验表明，干扰离子中的Pb计、Si㈣和高价锰在熔融浸取后，即被沉淀过滤分离；在微酸性条件下以氯化钡作为沉淀剂，沉淀溶液中硫酸根离子时，通过加入柠檬酸和三氯化铝溶液可掩蔽F-、Bi3＋、Sb3＋、Fe3＋，将沉淀物过滤，灼烧，称重可得知硫酸钡的含量，从而计算出冰铜中总硫的含量。方法用于冰铜样品中总硫的测定，结果与电感耦合等离子体原子发射光谱法一致，相对标准偏差（RSD，n=7）为0．39／6～0．5％，回收率在98％～103％之间。
As copper matte has a high content of sulfur, which is difficult to be completely oxidized, a method was established to determine total sulfur in copper matte by gravimetry with zinc oxide-sodium carbonate-potassium permanganate as flux. The optimum mass ratio of the mixed flux was 10 ： 10 ： 1 for sodium carbonate, zinc oxide and potassium permanganate. The optimum melting temperature was 750-800 ℃. Experiments showed that, after molten leaching, the interfering ion of Pb2＋ , Si（IV） and manganese with high valence were separated by precipitation and filtration. Under the slightly acidic condition, when sulfate ions in the solution was precipitated with barium chloride as precipitate, F- , Bi3＋ , Sb3＋ and Fe3＋ could be masked with the addition of citric acid and aluminum chloride solution. After the precipitate was filtered, burned to weigh the content of barium sulfate, the content of total sulfur in copper matte was calculated. The method was applied to the determination of total sulfur in copper matte samples, and the results were consistent with those obtained by inductively coupled plas- ma atomic emission spectrometry. The relative standard deviations （RSD, n=7） were in the range of 0.3 %-0.5 % and the recoveries were in the range of 98%-103%.
出处
《冶金分析》
CAS
CSCD
北大核心
2014年第3期73-76,共4页
Metallurgical Analysis
关键词
重量法
冰铜
总硫
gravimetry
copper matte
total sulfur
