Simplified method for the Re-Os dating of molybdenite using acid digestion and isotope dilution ICP-MS

An analytical method was developed for Os-Re dating of molybdenite. The method is based on determination of Os and Re concentrations in molybdenite by isotope dilution inductively-coupled plasma mass spectrometry (ID-ICP-MS). Sample digestion and sample/spike equilibration were achieved by a two-stage autoclave-based procedure using a mixture of nitric and sulphuric acids. Os was separated from the sample digest by modified single-stage distillation of osmium tetraoxide (OsO₄) using elevated temperature and on-line addition of hydrogen peroxide. OsO₄(g) was trapped in a mixture of 0.05% thiourea in 0.05 M sodium hydroxide. An anion-exchange column was used to separate Re from excess Mo in the solution remaining after distillation. Os and Re isotope ratio measurements were performed by single-collector, double focusing inductively-coupled plasma mass spectrometry (ICP-MS) with on-line mass-bias correction. Typical instrumental precision was in the range 0.02-0.2% relative standard deviation (R.S.D.) depending on the analyte concentrations. Notorious Os memory effects in the ICP-MS introduction system were eliminated using 5% ammonia solution, both as matrix for final dilution of the trap mixture as well as for washing between the samples. The reproducibility of the entire analytical procedure was accessed by replicate dating of two molybdenite standards and three molybdenite separates, and was found to be in the range 0.87-1.52% R.S.D. Though accuracy of the method is limited by difficulties in evaluating exact concentration of Os in spike solution, ages obtained in the course of these work agrees well with previously published data.     

不同粒级辉钼矿的XRD和SEM及其可浮性差异研究

在浮选过程中,微细粒级的辉钼矿回收难度较大,易损失在尾矿中。为了分析不同粒级辉钼矿可浮性差异,揭示细粒级辉钼矿可浮性恶化的原因,以-150+74,-74+45,-45+38和-38 μm四个粒级辉钼矿为研究对象,通过辉钼矿纯矿物浮选试验,首次利用X射线衍射分析(XRD)、扫描电镜(SEM)及能谱(EDS)分析,对四个粒级辉钼矿的可浮性及其晶型特征和外在形貌的变化规律进行系统研究和对比。研究表明：随着粒级的减小,辉钼矿的可浮性降低,浮选效果恶化,且辉钼矿的可浮性由非极性、低能、疏水的“面”和活泼、亲水的“棱”的面积比决定。辉钼矿在受外力作用下由粗粒级变成细粒级过程中,首先主要是沿解理面破裂,然后沿断裂面的破裂增多,导致面棱比减小,辉钼矿的可浮性下降;同时辉钼矿晶型结构由3R亚稳定状态转变为2H型稳定状态。此外,与3R型的粗粒级辉钼矿相比,微细粒级辉钼矿以2H型为主,且其（002）晶面的面间距逐渐增大,导致水分子容易进入晶体结构内部,并在矿物表面形成水化膜,辉钼矿亲水性增强。晶型的不同使不同粒级辉钼矿的物理性质发生变化,面间距的增大则使辉钼矿断裂面暴露的亲水性钼-硫键数目增多,两者是细粒级辉钼矿亲水性增强及可浮性下降的本质原因。     

Determination of rhenium content in molybdenite by ICP-MS after separation of the major matrix by solvent extraction with N-benzoyl-N-phenylhydroxalamine

A simple and rapid analytical method for determining the concentration of rhenium in molybdenite for Re-Os dating was developed. The method used isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS) after the removal of major matrix elements (e.g., Mo, Fe, and W) from Re by solvent extraction with N-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform solution. The effect on extraction efficiency of parameters such as pH (HCl concentration), BPHA concentration, and extraction time were also assessed. Under the optimal experimental conditions, the validity of the separation method was accessed by measuring ¹⁸⁷Re/¹⁸⁵Re values for a molybdenite reference material (JDC). The obtained values were in good agreement with previously measured values of the Re standard. The proposed method was applied to replicate Re-Os dating of JDC and seven samples of molybdenite from the Yuanzhuding large Cu-Mo porphyry deposit. The results demonstrate good precision and accuracy for the proposed method. The advantages of the method (i.e., simplicity, efficiency, short analysis time, and low cost) make it suitable for routine analysis.     

A Study on Molybdenite Electronic Structure

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粤西坡仔营钼矿花岗质岩石光谱学特征及意义

选取粤西坡仔营钼矿的花岗质岩石,研究其XRD,FT-NIR和Raman光谱特征。与花岗斑岩及远带样品相比,近带花岗岩样品XRD衍射信号弱,FT-NIR吸收信号强,石英Raman光谱信号弱。分析表明,其石英(101)晶面的XRD衍射峰、绢云母铝羟基(Al—OH)的FT-NIR特征峰(4 529 cm-1)及石英本征位移峰(464 cm-1)的半高宽均大于前二者。与其他样品不同,近带样品造岩矿物含量低,低温蚀变矿物含量高;且该带内矿物结晶度、有序度及结晶温度均较低。研究认为,坡仔营钼矿发育着一个以花岗斑岩为中心的面型低温蚀变带,而控制钼成矿的石英斑岩实为该蚀变带靠近官山嶂岩体的一部分。     

湖北蕲春花岗岩钾长石的结构状态研究

为探究湖北蕲春花岗岩岩体的岩浆作用演化与辉钼矿化作用关系,采用X射线粉晶衍射（XRD）、傅里叶红外吸收光谱（FTIR）、以及电感耦合等离子体质谱（ICP-MS）等方法,对岩体不同岩性单元中钾长石的结构状态特征开展深入研究。结果显示,蚀变钾化脉体中钾长石有序度、三斜度均较高,为具有三斜对称的微斜长石。白垩纪早世钾长石有序度相对较低,T1(o)位置中Al占位率也较低,[131]峰发生明显的宽化现象,结构由无序逐渐过渡到局部三斜有序。白垩纪晚世钾长石有序度最低,T1(o)位置中Al占位率最小,[131]峰形敏锐,为均匀、单一的单斜钾长石。640 cm-1吸收谱带显示出随钾长石有序度增大而向高波数方向移动的趋势,而540 cm-1吸收谱带则向低波数方向移动。1 010 cm-1吸收谱带随钾长石有序度的增大分裂成1 010和1 046 cm-1两个,形状也从宽缓变为尖锐。白垩纪早世钾长石含较高的成矿元素和稀土元素,有较好的成矿物质背景,蚀变脉体中的钾长石Sr和Ba含量明显偏低,证实蚀变热液流体为岩浆期后的产物,钾化蚀变是辉钼矿的重要找矿标志。     

Tracks in MoS2 irradiated with 20 MeV fullerene and 1 GeV lead ions

The first results of a Transmission Electron Microscopy study of Molybdenite (MoS₂) irradiated with 20 MeV fullerene and 1 GeV lead ions are presented. It is shown that the energy deposited by electronic excitation by both types of projectiles leads to track formation. Although the value of the linear rate of energy deposition is comparable for 20 MeV C₆₀ clusters and 1 GeV Pb ions, the diameters of the tracks created by the clusters is two times greater than the diameter of the tracks induced by 1 GeV Pb ions. Furthermore, the tracks in the sample irradiated with fullerene ions present specific contrast features.