可溶性钾盐主要成分分析前处理技术与分析方法研究  

Research on Pre-Treatment Technology and Analysis Methods for Main Components in Soluble Potassium Salt

作　　者：孙红宾[1] 于汀汀 臧慧媛 郭琳[1] 王蕾[1] SUN Hongbin;YU Tingting;ZANG Huiyuan;GUO Lin;WANG Lei(National Research Center for Geoanalysis,Beijing 100037,China;Shougang Institute of Technology,Beijing 100041,China)

机构地区：[1]国家地质实验测试中心,北京100037 [2]首钢工学院,北京100041

出　　处：《岩矿测试》2024年第3期449-458,共10页Rock and Mineral Analysis

基　　金：国家重点研发计划项目(2021YFC2903000)课题“战略性矿产多元素同时分析技术和标准化”;中国地质科学院基本科研业务费项目(CSJ-2022-09)。

摘　　要：钾盐是中国最紧缺的矿产资源之一,为农业三大肥料中钾肥的主要原料,当前具有开发利用价值的主要是可溶性钾盐资源。而目前可溶性钾盐尚无国家标准物质和标准分析方法,本文对称样量、固液比、溶解温度、溶解时间、搅拌条件、超声时间和功率等条件进行实验研究,利用电热板和超声振荡两种溶解方式,建立了可溶性钾盐中主要成分钾、钠、钙、镁、氯和硫酸根离子的分析方法。采用电感耦合等离子体发射光谱仪测定样品中的Ca^(2+)、Mg^(2+)、K^(+)和Na^(+)的含量,离子色谱仪测定样品中Cl^(-)和SO_(4)^(2-)的含量,两种溶解方法分析可溶性钾盐样品中上述离子的实验结果基本吻合。电热板溶解方法精密度为0.52%~3.19%(RSD,n=11),超声振荡溶解方法精密度为0.55%~3.07%(RSD,n=11),两种方法检出限为0.01~0.05μg/g。利用主要成分百分含量加和、加标回收率、阴阳离子平衡验证方法准确性,两种溶解方法的主要成分加和在99.0%~101.0%之间,加标回收率在95.3%~103.8%,阴阳离子平衡在-3%~3%之间,均满足DZ/T 0130.3—2006质量管理规范中的分析要求。两种可溶性钾盐的溶解方法均可在日常检测中应用,对于较大批的钾盐样品分析,电热板溶解法整体工作效率较高,更适用于实验室内批量样品分析;超声振荡器溶解方法与电热板溶解方法相比,更为简单快速,对于少量样品的分析,效率更高,且超声波振荡器方便野外携带,使用在钾盐的野外现场勘探工作中,可较大地提高工作效率,实时指导找矿行动顺利开展。Potassium salt is one of the scarcest mineral resources in China,and it is the main raw material for potassium fertilizer in the three major fertilizers of agriculture.Currently,soluble potassium salt resources are the main ones with development and utilization value.At present,there is no national standard material or standard analysis method for soluble potassium salts.In the experiments,soluble potassium salt samples were dissolved by electric heating plate and ultrasonic oscillation.According to the main components of soluble potassium salts,a method for the determination of K^(+),Na^(+),Ca^(2+)and Mg^(2+)by ICP-OES and a method for the determination of Cl^(−) and SO_(4)^(2−) by ion chromatography(IC)in soluble potassium salts were established.Through experimental conditions,the dissolution temperature of the electric heating plate was determined to be 160℃and slightly boiled for 20min;the ultrasonic oscillation dissolution power was 60Hz and the time was 20min.The precision of the two methods was between 0.55%−3.19%(RSD,n=11),and the detection limit was between 0.01μg/g to 0.05μg/g.Both dissolution methods of soluble potassium salts can be widely used in daily detection.The electric heating plate dissolution method is more suitable for batch sample analysis in the laboratory.The ultrasonic oscillator dissolution method is simple and fast,and can be widely used in the field exploration of potassium salts,which can greatly improve the work efficiency and guide the smooth development of prospecting operations in real time.

关 键 词：可溶性钾盐 钾 电感耦合等离子体发射光谱法 离子色谱法 超声振荡 电热板 

分 类 号：P575[天文地球—矿物学] P619.211[天文地球—地质学]