摘要
炭质板岩地质结构及其性质特点决定了按照常规分析方法对伴生金属元素铬、钒检测时存在操作繁琐、干扰因素多或溶解不完全等难点。为了快速准确测定炭质板岩中伴生元素铬、钒,根据炭质板岩样品的成分特征,对测定铬、钒的常规方法进行了改进,增加了高温焙烧,通过实验选择了合适的焙烧温度。确定采用700℃马弗炉高温焙烧,经硝酸-氢氟酸-高氯酸混酸处理,王水(1+1)提取定容后,选择Cr 267.716 nm、V 292.402 nm为分析谱线,用电感耦合等离子体原子发射光谱(ICP-AES)法对炭质板岩中的铬、钒进行测定。在仪器工作条件最佳化条件下,各元素校准曲线的线性回归方程相关系数均大于0.9996;方法检出限为铬1.38μg/g,钒1.76μg/g;铬、钒回收率分别为96.8%~105%、96.8%~104%;相对标准偏差(RSD)分别为铬2.3%~3.6%,钒0.47%~1.3%;检测范围铬4.41~4000μg/g,钒5.28~6000μg/g,能够满足炭质板岩中伴生金属元素铬、钒的测定要求。
The geological structure and properties of carboniferous slate determine that there are some problems in the detection of associated metal elements chromium and vanadium by conventional analytical methods,such as complicated operation,many interference factors or incomplete dissolution.In order to quickly and accurately determine the associated elements chromium and vanadium in carboniferous slate,according to the composition characteristics of carboniferous slate samples,the conventional method for determination of chromium and vanadium was improved by adding high temperature roasting,and the appropriate roasting temperature was selected through experiments.The determination of chromium and vanadium in carbonite slate was carried out by ICP-AES after roasting in muff furnace at 700℃,mixed acid treatment of nitric acid-hydrofluoric acid and perchloric acid.After extraction from aqua regia(1+1),Cr 267.716 nm and V 292.402 nm were selected as analytical spectral lines.Under the optimal working conditions of the instrument,the correlation coefficients of the linear regression equations of each element calibration curve are greater than 0.9996.The detection limits of chromium and vanadium were 1.38μg/g and 1.76μg/g,respectively.Recoveries of chromium and vanadium were 96.8%—105%and 96.8%—104%.The relative standard deviations(RSDS)were 2.3%—3.6%for chromium and 0.47%—1.3%for vanadium.The detection range of chromium(4.41—4000μg/g)and vanadium(5.28—6000μg/g)can meet the requirements of determination of the associated metal elements chromium and vanadium in the carbonaceous slate.
作者
黄登丽
刘彤彤
程帆
HUANG Dengli;LIU Tongtong;CHENG Fan(Lanzhou Geo-mine Survey Institute of Non-ferrous Metal Geological Exploration Bureau of Gansu Province,Lanzhou,Gansu 730030,China;Zhangye Geo-mine Survey Institute of Non-ferrous Metal Geological Exploration Bureau of Gansu Province,Zhangye,Gansu 734000,China;Gansu Huatest and Verification Co.,Ltd.,Lanzhou,Gansu 730000,China)
出处
《中国无机分析化学》
CAS
北大核心
2023年第1期105-110,共6页
Chinese Journal of Inorganic Analytical Chemistry
