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本工作主要研究硅钼蓝法对测定高纯钠中微量硅的可行性,包括钠的取样、处理及分析条件的选择。结果表明,按制定方法,操作简便,分析时间短,精确度也符合工业钠、试剂级钠及核级钠的要求。 (一)主要仪器、实验装置和试剂 1.751-G型分光光度计。 2. 附有循环净化系统的惰气-真空手套箱及高纯钠净化回路。其作用及结构见文献。 3.溶钠装置:包括氩气钢瓶、氩气水洗瓶及50毫升的塑料溶样瓶及冷却杯等。 4.主要试剂:①碳酸钠中和液:称基准碳酸钠23g于塑料杯内,加100ml水溶解,加2滴0.1％溴酚蓝指示剂,用1:1硫酸中和至黄色,过量1滴硫酸,冷后稀至150ml,存于塑料
This work mainly studies the feasibility of silicon molybdenum blue method for the determination of trace silicon in high-purity sodium, including sodium sampling, processing and analysis of the choice of conditions. The results show that, according to the formulation method, the operation is simple, the analysis time is short, the accuracy also meets the requirements of industrial sodium, reagent grade sodium and nuclear grade sodium. (A) of the main equipment, laboratory equipment and reagents 1.751-G spectrophotometer. 2. With the cycle of purification system inert gas - vacuum glove box and high purity sodium purification circuit. Its role and structure of the literature. 3. Sodium dissolving device: Including argon cylinder, argon water bottle and 50ml plastic sample bottle and cooling cup. 4. The main reagents: ① sodium carbonate and neutralizing solution: said the reference sodium carbonate 23g in plastic cups, add 100ml of water dissolved, add 2 drops of 0.1% bromophenol blue indicator, neutralized with 1: 1 sulfuric acid to yellow, excess 1 Drops of sulfuric acid, diluted to 150ml after cold, stored in plastic