摘要
利用自动电位滴定仪和DP5光度电极研究了原位自动光度滴定法在全铁测量中的应用。以HNO3、HCl和HF溶液为溶剂,采用密封微波消解系统分解试样。用NaOH溶液调节溶液酸度至pH 1.5,在原消解罐中以乙二胺四乙酸二钠盐(磺基水杨酸为指示剂)滴定铁。主要对滴定温度、试样的分解条件以及杂质对测定的干扰情况进行了研究。研究结果表明,称样量为0.05 g,溶剂为60%王水10 mL加1 mL HF(1+99),温度为210℃,消解时间为20 min时溶样效果最好,50～60℃条件下,pH 1.5时进行滴定,结果准确可靠,能有效消除干扰。
The in situ determination of iron content in iron ores is presented with the automatic photometric titration method using an automatic potentiometric titrator and a DP5 photometric electrode.The samples are digested in closed vessels in a microwave oven with a mixture of nitric acid,hydrochloric acid and hydrofluoric acid solution.The resulting solution is diluted with water and adjusted to pH1.5 with sodium hydroxide solution.Iron is determined in situ by automatic photometric titration with EDTA（Sulfosalicylic acid as indicator）.The conditions of titration temperature,sample decomposition and interferences are studied.The results show that optimal conditions are as follows,0.05 g of samples,10 mL of 60% aqua regia and 1 mL of（1＋99） HF,digestion temperature of 210 ℃,digestion time of 20 minutes,the titration solution at 50~60 ℃ and pH 1.5.The obtained results are accurate and reliable,and the interferences can be eliminated.
出处
《分析试验室》
CAS
CSCD
北大核心
2012年第12期53-56,共4页
Chinese Journal of Analysis Laboratory
基金
国家质量监督检验检疫总局科研项目(2011IK031)资助
关键词
铁矿石
全铁
微波消解
原位测定
微型光度滴定
Iron ores
Total iron content
Microwave assisted digestion
In situ determination
Microscale photometric titration
