第 47 卷第 1 期Vol. 47 No. 1
2017 年 2 月Feb 2017

所属栏目:分析与测试

湿法碱消解-淋洗液在线发生离子色谱法测定锂云母中氟量
杨 清,邹 娟,刘雨星,罗 稳,杨三妹,谢 超* (化工部长沙设计研究院 湖南省钾及伴生物工程技术研究中心,湖南 长沙 410116)
摘 要:建立了湿法碱消解-盐酸提取-淋洗液在线发生离子色谱法测定锂云母中氟量的方法。通过实验确定了盐酸用量、淋洗液浓度和淋洗液流速。方法检出限为0.011 mg/L,线性相关系数r大于0.999 9。对实际锂云母样品进行重复5次测定,并做了加标回收实验,相对标准偏差RSD为0.34 %,加标回收率为98.8%~103.1%。经国家标准品验证,测定值与标准值相符。该方法快速准确,能达到测定锂云母中氟量的分析要求。
关键词:锂云母;湿法碱消解;盐酸提取;离子色谱法;氟
中图分类号:O656  文献标识码:A  文章编号:1009-9212(2017)01-0070-03
Determination of Fluorine in Lepidolite Using Alkali Fusion-hydrochloric Acid Extract-ion Chromatography with On-line Eluent Generator
YANG Qing, ZOU Juan, LIU Yu-xing, LUO Wen, YANG San-mei, XIE Chao* (Changsha Design & Research Institute, the Ministry of Chemical Industry Changsha, Hunan Engineering Research Center of Potassium and its Co-existed Resources, Changsha 410116, China)
Abstract:A method of alkali fusion-hydrochloric acid extract-ion chromatography with on-line eluent generator was established, which was able to determine fluorine in lepidolite. The amount of hydrochloric acid, the eluent components and the flow rate of eluent were confirmed via experimental tests. The results showed that the limit of detection was of 0.011 mg/L and the correlation coefficient of calibration curve was over 0.999 9. The relative standard deviation was 0.34%, and the recovery was ranged from 98.8% to 103.1%. The result of national standard material agreed with the recommended value. This method was fast with good accuracy, which was able to meet the requirements for determination of fluorine in lepidolite samples.
Key words:lepidolite; alkali fusion; hydrochloric acid extract; ion chromatography; fluorine
作者简介:杨 清(1989-),女,湖南岳阳人,硕士研究生,研究方向:分析化学(E-mail: artemi@163.com)
联 系 人:谢 超,高级工程师,主要从事盐湖化工工艺研究。
收稿日期:2017-01-09