岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2015年
3期
308-313
,共6页
赵良成%郭秀平%胡艳巧%程文翠%王磊%马会春
趙良成%郭秀平%鬍豔巧%程文翠%王磊%馬會春
조량성%곽수평%호염교%정문취%왕뢰%마회춘
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
石墨%常量元素%鉑坩堝%碳痠鉀-碳痠鈉堿鎔%電感耦閤等離子體髮射光譜法
석묵%상량원소%박감과%탄산갑-탄산납감용%전감우합등리자체발사광보법
graphite%major elements%platinum crucible%potassium carbonate-sodium carbonate fusion%Inductively Coupled Plasma-Optical Emission Spectrometry
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。
石墨化學性質穩定,需採用高溫堿鎔(1000℃)纔可使樣品分解完全,已有分析方法在樣品前處理不同的階段使用不同材質的坩堝。基于石墨性質和坩堝鎔樣情況,本文採用預先已均勻鋪墊0.50 g 碳痠鉀的高鎔點鉑坩堝灼燒石墨樣品,樣品灼燒後直接在原坩堝中加入0.80 g 碳痠鈉堿鎔,鎔融物用稀鹽痠提取後用電感耦閤等離子光譜法(ICP -OES)實現瞭石墨中8種常量元素(硅鋁鈣鎂鐵鈦錳燐)的同時測定。方法檢齣限為13~228μg/g,方法精密度(RSD,n =12)為0.7%~7.2%;全流程加標迴收率為90.5%~105.0%;實際土狀和鱗片石墨樣品的測定結果與化學分析法無顯著差異。本方法避免瞭鉑坩堝的損燬和樣品在前處理過程中的損失,分析過程簡單、分析速度快。
석묵화학성질은정,수채용고온감용(1000℃)재가사양품분해완전,이유분석방법재양품전처리불동적계단사용불동재질적감과。기우석묵성질화감과용양정황,본문채용예선이균균포점0.50 g 탄산갑적고용점박감과작소석묵양품,양품작소후직접재원감과중가입0.80 g 탄산납감용,용융물용희염산제취후용전감우합등리자광보법(ICP -OES)실현료석묵중8충상량원소(규려개미철태맹린)적동시측정。방법검출한위13~228μg/g,방법정밀도(RSD,n =12)위0.7%~7.2%;전류정가표회수솔위90.5%~105.0%;실제토상화린편석묵양품적측정결과여화학분석법무현저차이。본방법피면료박감과적손훼화양품재전처리과정중적손실,분석과정간단、분석속도쾌。
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 whole-process 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.