摘要
为了准确快捷有效地对青海某地区铌矿物进行化学物相分析研究,采用电感耦合等离子体质谱法测定各相态中的铌,建立了一套准确快速测定铌矿物化学物相的分析方法。通过对溶剂的选择,实现对易解石、黄绿石、铌钙矿、铌铁矿、钛铁金红石和分散相的分离与测定。物相分析试样以两份完成,一份在550~600℃的高温炉中焙烧,氟化铵溶解易解石中铌。另一份试样不经高温焙烧,用含氯化亚锡的盐酸溶解分散相中的铌;用含氢溴酸的氟化铵溶解易解石和黄绿石中的铌;用含氢氟酸的硫酸溶解铌钙矿中的铌;用含氢氟酸的盐酸溶解铌铁矿中的铌;用焦硫酸钾熔融提取钛铁金红石中的铌,最后用电感耦合等离子体质谱法(ICP-MS)测定以上各相态中铌的质量分数。在ICP-MS工作条件下连续7次测定样品空白,计算各铌相态的方法检出限(3S/N)分别为0.023、0.021、0.018、0.025、0.016、0.007μg·g^(-1)。对7个铌矿物样品进行铌物相分析,做精密度和准确度试验,符合《地质矿产实验室测试质量管理规范》(DZ/T 0130.3—2006)的要求。
For accurate,rapid and effective chemical phase analysis of niobium minerals in a certain area of Qinghai, a analytical method for the accurate and rapid determination of niobium mineral chemical phase of niobium mineral was established by ICP-MS determination of niobium in each phase state. The separation and determination of pyroxene,chlorite,niobite,niobiumperovskite,ilmenite rutile and other dispersed phases were realized by the choice of solvent. The phase analysis samples included two copies, one sample was roasted in 550~600 ℃ high temperature furnace, and ammonia fluoride dissolved niobium in calcite. Another sample was dissolved in the dispersed phase with stannous chloride hydrochloric acid without high temperature roasting. Niobium in calcite and chlorite was dissolved with ammonium fluoride containing hydrobromate. The niobium in the niobium calcium ore was dissolved by sulfuric acid containing hydrofluoric acid. The niobium in the niobium iron ore was dissolved with hydrofluoric acid containing hydrofluoric acid.The niobium in ilmenorutite was extracted by melting potassium pyrosulfate.Finally,the mass fraction of niobium in the above phase states was determined by inductively coupled plasma mass spectrometry. Under the ICP-MS working conditions, the blank of the sample was determined 7 times continuously, and the detection limit(3 S/N) of each niobium phase state was 0.023,0.021,0.018,0.025,0.016,0.007 μg·g^(-1). The niobium phase analysis was carried out on 7 niobium mineral samples,and the precision and accuracy were tested,which met the requirements of(DZ/T 0130.3—2006) Standard for Quality Management of Geological and Mineral Laboratory Testing.
作者
胡兰基
朱琳
王洪桂
赵玉卿
马龙
霍成玉
张建民
HU Lan-ji;ZHU Lin;WANG Hong-gui;ZHAO Yu-qin;MA Long;HUO Cheng-yu;ZHANG Jian-min(Qinghai Research Institute of Geological and Mineral,Xining 810021,China)
出处
《当代化工》
CAS
2021年第6期1504-1508,共5页
Contemporary Chemical Industry
基金
青海省重点研发和转化计划项目(项目编号:2019-SF-139)
青海学者资助,青人社厅函[2019]48号
青海学者专项,柴达木盆地及周缘战略性矿产成矿作用及找矿突破项目(项目编号:QHS201802)。
关键词
铌钙矿
物相分析
电感耦合等离子质谱法
易解石
黄绿石
钛铁金红石
Niobium-calcium ore
Phase analysis
Inductively coupled plasma mass spectrometry(ICP-MS)
Aeschynite
Pyrochlore
Ilmenorutite
