摘要
石墨化学性质稳定,需采用高温碱熔（1000℃）才可使样品分解完全,已有分析方法在样品前处理不同的阶段使用不同材质的坩埚。基于石墨性质和坩埚熔样情况,本文采用预先已均匀铺垫0.50 g碳酸钾的高熔点铂坩埚灼烧石墨样品,样品灼烧后直接在原坩埚中加入0.80 g碳酸钠碱熔,熔融物用稀盐酸提取后用电感耦合等离子光谱法（ICP-OES）实现了石墨中8种常量元素（硅铝钙镁铁钛锰磷）的同时测定。方法检出限为13~228μg/g,方法精密度（RSD,n=12）为0.7%~7.2%;全流程加标回收率为90.5%~105.0%;实际土状和鳞片石墨样品的测定结果与化学分析法无显著差异。本方法避免了铂坩埚的损毁和样品在前处理过程中的损失,分析过程简单、分析速度快。
Graphite is a stable nonmetal and must be decomposed completely by alkali fusion at high temperature（ 1000℃）. In previous methods,different crucibles were used in different phases in order to shorten the utility time of the platinum crucible and avoid damage to the platinum crucible and sample loss. Based on the nature of graphite ore and the character of the crucible,a new method has been developed. The sample was firstly ignited at high temperature in a platinum crucible,which was prepared with 0. 50 g potassium carbonate at the bottom. The sample was then directly digested by 0. 80 g sodium carbonate in the former platinum crucible. Lastly the melt was dissolved by diluting hydrochloric acid. Eight major elements（ Si, Al, Ca, Mg, Fe, Ti, Mn, P） were simultaneously determined by Inductively Coupled Plasma-Optical Emission Spectrometry（ ICP-OES）. The proposed method has a detection limit of 13- 228 μg / g,precision（ RSD,n = 12） of 0. 7%- 7. 2%,and wholeprocess recoveries of 90. 5%- 105. 0%. The analytical results of flake graphite and amorphous graphite by this method are in agreement with those by chemical method. This method avoids sample loss and platinum crucible damage. The whole process of treatment is simple and rapid.
出处
《岩矿测试》
CAS
CSCD
北大核心
2015年第3期308-313,共6页
Rock and Mineral Analysis
基金
河北省保定地质工程勘查院技术创新项目(20130810)
关键词
石墨
常量元素
铂坩埚
碳酸钾-碳酸钠碱熔
电感耦合等离子体发射光谱法
graphite
major elements
platinum crucible
potassium carbonate-sodium carbonate fusion
Inductively Coupled Plasma-Optical Emission Spectrometry
