A Rapid Acid Digestion Technique for the Simultaneous Determination of Bromine and Iodine in Fifty‐Three Chinese Soils and Sediments by ICP‐MS

Bromine and iodine are important tracers for geochemical and environmental studies. In this study, a rapid acid digestion (HNO₃ + HF) with ammonia dilution for the simultaneous determination of bromine and iodine in soils and sediments using ICP‐MS was developed. The recoveries of Br and I were controlled by the synergic effect of temperature and time. It took only 15 min at 140 °C for the complete recovery of Br and I in sediment (GSD‐2) and soil (GSS‐24) reference materials, which is a process that needs 2–6 h at 90 °C. A serious loss of Br and I was found at a higher digestion temperature of 190 °C. A 5% v/v NH₄OH dilution effectively eliminated the memory effects and stabilised the signals of Br and I. Moreover, ammonia dilution also avoided the corrosiveness of HF on the sample introduction system and torch of ICP‐MS. Tellurium is a more suitable internal standard element than In in the ammonia medium. To avoid the adsorption of residues of dissolution on Te, addition of Te should be carried out after centrifuging the solution. The developed method was successfully applied to determine Br and I in fifty‐three Chinese soil and sediment reference materials. This simple method shows great potential for the rapid determination of Br and I in large batches of geological and environmental samples commonly analysed for mineral exploration and environmental geochemistry studies.     

异烷基磷酸（1甲基庚基）酯萃淋树脂分离感耦等离子体光谱法测定氧化铕中微量稀土元素

用５７０９萃淋树脂还原色层法分离富集高纯氧化铕中微量稀土杂质，随后用顺序扫描等离子体光电光谱法测定。色层分离的条件：上柱稀土基体的质量浓度为２０ｇ／Ｌ，ｐＨ２～３，流速为２５ｍＬ／ｍｉｎ，洗脱液为６ｍｏｌ／Ｌ的ＨＣｌ溶液。共测定铈、镨、钕、钐、钆和镝６种稀土杂质。回收率为８９％～１０５％，相对标准偏差≤４％。方法可用于荧光级氧化铕中杂质稀土的测定     

Determination of Trace Element Mass Fractions in Ultramafic Rocks by HR‐ICP‐MS: A Combined Approach Using a Direct Digestion/Dilution Method and Preconcentration by Coprecipitation

A procedure is described for the determination of thirty‐seven minor and trace elements (LILE, REE, HFSE, U, Th, Pb, transition elements and Ga) in ultramafic rocks. After Tm addition and acid sample digestion, compositions were determined both following a direct digestion/dilution method (without element separation) and after a preconcentration procedure using a double coprecipitation process. Four ultramafic reference materials were investigated to test and validate our procedure (UB‐N, MGL‐GAS [GeoPT12], JP‐1 and DTS‐2B). Results obtained following the preconcentration procedure are in good agreement with previously published work on REE, HFSE, U, Th, Pb and some of the transition elements (Sc, Ti, V). This procedure has two major advantages: (a) it avoids any matrix effect resulting from the high Mg content of peridotite, and (b) it allows the preconcentration of a larger trace element set than with previous methods. Other elements (LILE, other transition elements Cr, Mn, Co, Ni, Cu, Zn, as well as Ga) were not fully coprecipitated with the preconcentration method and could only be accurately determined through the direct digestion/dilution method.     

Determination of the Tin Stable Isotopic Composition in Tin‐bearing Metals and Minerals by MC‐ICP‐MS

This study uses MC‐ICP‐MS for the precise analysis of the stable tin isotopic composition in ore minerals of tin (cassiterite, stannite), tin metal and tin bronze. The ultimate goal is to determine the provenance of tin in ancient metal objects. We document the isotope compositions of reference materials and compare the precision of different isotope ratios and the accuracy of different procedures of mass fractionation correction. These data represent a base with which isotopic data of future studies can be directly compared. The isotopic composition of cassiterite and stannite can be determined after reduction to tin metal and bronze, respectively. Both metals readily dissolve in HCl, but while the solutions of tin metal can be directly measured, the bronze solutions must be purified with an anion exchanger. The correction of the mass bias is best performed with an internal Sb standard and an empirical regression method. A series of Sn isotope determinations on commercially available mono‐element Sn solutions as well as reference bronze materials and tin minerals show fractionations ranging from about ?0.09‰ to 0.05‰/amu. The combined analytical uncertainty (2s) was determined by replicate dissolutions of reference materials of bronze (BAM 211, IARM‐91D) and averages at about 0.005‰/amu.     

Method Development and Optimisation of Sodium Peroxide Sintering for Geological Samples

This work provides a measurement procedure for the complete digestion of rock samples containing refractory minerals such as zircon and chromite. Their dissolution by wet acid digestion is often incomplete but, although providing complete digestions, alkali fusion techniques can result in solutions with a high blank and total dissolved solid content. It was established by the systematic study with reference material trachyandesite MTA‐1 that a 1:6 sample to sodium peroxide (Na₂O₂) ratio is conservative for the complete digestion and recovery of all the analytes especially those contained in zircon. The sample decomposition time was 120 min for the zircon‐bearing rhyolite reference material MRH‐1. Complete digestion of chromite was obtained in the harzburgite RM MUH‐1. The sample solutions were stable for at least 1 year. Accurate measurements of SiO₂, Al₂O₃, TiO₂, P₂O₅ and K₂O could be made with ICP‐MS by not discarding the supernatant of the sinter solution and by using geological reference materials for external calibration. HF digestions are slow, not universal, and may form new mineral/phases that are insoluble under high temperature conditions. The validated sample decomposition procedure combined with ICP‐MS presents an alternative to the use of HF in routine analysis of difficult to digest geological materials.     

电感耦合等离子体质谱法测定生物样品中超痕量稀土时氧化物干扰的研究

试验了１００～７００ｕｇ／ＬＢａ的氧化物对Ｅｕ产生的干扰,干扰程度与Ｂａ量呈线性,其相关系数ｒ在０．９９８６～０．９９９５。用模拟样品溶液对不同含量的Ｂa对Ｅu的干扰采取了简单的数学方法校正,校正后的结果在误差允许范围之内。．对小麦和人发标准物质中Ｂa氧化物对Ｅu的干扰及校正效果进行了比较。结果表明,在所使用的仪器条件下,这两个标准物质中的Ｂa对Ｅu的干扰必须校正。研究了ｕｇ／Ｌ水平的轻稀土氧化物对重稀     

东昆仑洪水川地区科科鄂阿龙岩体锆石U Pb年代学、地球化学及其地质意义

东昆仑地区出露大量呈带状分布的中生代花岗岩,是我国一条巨型花岗质岩浆岩带,它的发育与该地区岩石圈动力学演化有着密切联系.对东昆仑造山带东段南缘洪水川地区的科科鄂阿龙石英闪长岩体的岩相学、岩石地球化学和LA-ICP-MS锆石U-Pb同位素年代学研究结果显示,岩石具有3组谐和锆石年龄:第一组年龄大于402Ma,为捕获围岩的锆石年龄;第二组年龄为243.9±3.0Ma(MSWD=0.94),代表该区玄武质岩浆底侵事件;第三组年龄为218.3±1.4Ma(MSWD=0.52),代表岩体的结晶年龄.地球化学分析表明该岩体具有高Sr,低Y、Yb,高Sr/Y比值,轻重稀土分异明显,Eu异常不明显,其微量元素显示出埃达克质岩石特征.其较低的Nb、Ta和较高的Mg=、Cr、Ni含量,高Nb/Ta比值,说明了在金红石稳定域内部分熔融形成的熔体交代了岩石圈地幔.岩体的年代学及地球化学特征表明,东昆仑地区在218Ma的晚三叠世时期发生了岩石圈地壳拆沉作用,它是早期俯冲形成的玄武质岩浆底侵而形成的加厚下地壳,在高压缺水的条件下相变为榴辉岩相并拆沉进入软流圈,部分熔融的熔体在上升过程中先与岩石圈地幔反应,然后与地壳围岩发生同化混染作用,最终形成了科科鄂阿龙石英闪长岩.     

辽宁四道沟热液金矿床中石英的稀土元素的特征及意义

本文用ＩＣＰ－ＭＳ测定了辽宁四道沟金矿矿脉中石英及其中流体包裹体中的稀土元素含量,发现石英的稀土元素配分模式类似于其中流体包裹体的稀土元素配分模式,推断石英中的稀土元素主要赋存于注流体包裹体中,流体包裹体中的稀土元素了石英的稀土元素配分模式,原生包裹中的流体是和石英同源的,其稀土元素指示的是石英形成过程中流体的信息。而次生包裹体中的流体是石英形成后的流体活动产物,其稀土元素指示的是后期流体活动的信     

内蒙苏尼特右旗吉布胡楞土岩体LA-ICP-MS锆石U-Pb定年、地球化学特征及地质意义

在华北板块北缘白乃庙岛弧岩浆活动带中发现了一套石榴石白云母花岗岩。锆石LA-ICP-MS U-Pb定年结果显示,该石榴石白云母花岗岩的结晶年龄为(500.8±2.4)Ma,为晚寒武世岩浆活动的产物。主量元素岩石地球化学特征方面:该岩体富硅、铝(w(SiO₂)=72.50%~74.11%;w(Al₂O₃)=14.73%~16.43%),贫铁、镁、钙(w(TFeO)=0.67%~1.14%;w(MgO)= 0.09%;w(CaO)=0.30%~0.61%),为高分异花岗岩(分异指数DI=91.99~93.20);铝饱和指数均大于1.1,发育富铝矿物石榴石和白云母,为过铝质花岗岩,但并非S型花岗岩;综合认为该石榴石白云母花岗岩是一套富铝、贫铁镁钙的高分异钙碱性I型花岗岩。微量元素特征方面:稀土总量较低,轻重稀土分馏不明显,具有强烈的负Eu异常;具明显的稀土元素四分组效应;并且部分岩石样品的Nb、Ta含量较高,暗示该岩体是分异岩浆与流体作用的产物。该岩体可为Nb、Ta等稀有金属成矿提供必要的物质基础。     

西昆仑慕士塔格-公格尔印支期侵入岩岩石与锆石地球化学特征及研究意义

西昆仑造山带南侧的麻扎-康西瓦缝合带,是古特提斯洋闭合的位置。慕士塔格-公格尔作为昆仑山的主峰,紧邻该缝合带的东北侧分布,主要岩性为花岗闪长岩和黑云母二长花岗岩。作者系统研究了两种岩性的地球化学及年代学特征,探讨了岩石成因,反演了古特提斯洋的构造演化历史。岩体岩浆锆石LA-ICP-MS U-Pb测年结果显示,花岗闪长岩和黑云母二长花岗岩的成岩年龄分别为(213.0±0.5)~(215.4±0.9)Ma和(220.6±0.5)~(222.1±0.4)Ma,是晚三叠世岩浆活动的产物。两种岩性均为高硅(w(SiO2)65%)、富碱(w(K2O+Na2O)6%)、钙碱性-高钾钙碱性、准铝质(A/CNK1),富集大离子亲石元素(LILE)和轻稀土元素(LREE),亏损高场强元素(HFSE)和重稀土(HREE)。微量元素组成特征、低锆石饱和温度及高分异指数显示慕士塔格-公格尔花岗岩体为高分异I型花岗岩。岩体锆石的εHf(t)值变化范围较小,为-4.46~-0.17,指示岩浆以壳源为主。综合研究表明,慕士塔格-公格尔花岗岩体可能是同碰撞造山环境下,老的下地壳受地幔热源影响部分熔融,形成的长英质壳源岩浆侵入地壳内部而冷却结晶形成。