CAJ | 학술논문

钨矿石和锡矿石成分复杂，具有丰富的共生或伴生元素。在国家标准方法中，对其中的微量共生或伴生元素含量多采用单元素测定，分析强度大，效率低。本文采用混合酸在敞开体系中消解样品，以50%盐酸提取盐类，电感耦合等离子体质谱仪（ ICP-MS）同时测定钨矿石和锡矿石中的锂钪铬钴镍铜铅锌铷钼铯锑铋钍等14种微量元素。通过比较碱熔法、盐酸+氢氟酸+硝酸+高氯酸四酸溶矿法、氢氟酸+硝酸+高氯酸三酸溶矿法这三种样品前处理方法，确定选择使用氢氟酸+硝酸+高氯酸三酸溶矿法溶解样品。ICP-MS测定过程中，选择铑和铼作为内标元素，有效监控分析信号的漂移。测定结果表明，各元素的检出限为0.003~1.64μg/g，相对标准偏差在0.1%~3.1%，方法回收率在93.1%~104.3%。方法应用于实际钨矿石和锡矿石分析，测定结果与各元素标准测定值吻合较好。相对于传统处理方法，本法一次溶样，多元素同时测定，使分析效率得到了有效提高，更适合大批量多元素钨矿石和锡矿石样品的分析。
오광석화석광석성분복잡，구유봉부적공생혹반생원소。재국가표준방법중，대기중적미량공생혹반생원소함량다채용단원소측정，분석강도대，효솔저。본문채용혼합산재창개체계중소해양품，이50%염산제취염류，전감우합등리자체질보의（ ICP-MS）동시측정오광석화석광석중적리항락고얼동연자여목색제필토등14충미량원소。통과비교감용법、염산+경불산+초산+고록산사산용광법、경불산+초산+고록산삼산용광법저삼충양품전처리방법，학정선택사용경불산+초산+고록산삼산용광법용해양품。ICP-MS측정과정중，선택로화래작위내표원소，유효감공분석신호적표이。측정결과표명，각원소적검출한위0.003~1.64μg/g，상대표준편차재0.1%~3.1%，방법회수솔재93.1%~104.3%。방법응용우실제오광석화석광석분석，측정결과여각원소표준측정치문합교호。상대우전통처리방법，본법일차용양，다원소동시측정，사분석효솔득도료유효제고，경괄합대비량다원소오광석화석광석양품적분석。
Tungsten and tin ores have abundant paragenesis or associated elements with complicated composition. At present,the contents of these trace elements are detected respectively by the national standard methods for tungsten ore and tin ore,which have a great labour intensity and low efficiency. The tungsten ore and tin ore samples were dissolved by mixed acid at normal pressure and extracted by hydrochloric acid(50% HCl),and 14 trace elements of Li,Sc,Cr,Co,Ni,Cu,Pb,Zn,Rb,Mo,Cs,Sb,Bi and Th were simultaneously measured by Inductively Coupled Plasma-Mass Spectrometry( ICP-MS ). Three sample pre-treatment methods were compared among alkali fusion method,HCl-HNO3-HF-HClO4 method and HNO3-HF-HClO4 method. It was found that the HNO3-HF-HClO4 method is a simple operation and requires fewer reagents than traditional methods,which was chosen to dissolve the tungsten ore and tin ore samples. In the measurement,Rh and Re were selected as the internal standards to compensate for analytical signal drift. The results indicate that the detection limits of this method are 0. 003-1. 64 μg/g with a relative standard deviation(RSD,n=11)in the range of 0. 1% -3. 1%. The recovery rates were between 93 . 1% -104 . 3%. This method has been verified using practical tungsten and tin ore samples,and the results are in good agreement with the certified values. Comparing with the traditional treatment,this method has improved analysis efficiency,and is more suitable for analysis and detection of tungsten ore and tin ore samples in large batches.