Determination of Ge, As, Se and Te in Silicate Samples Using Isotope Dilution-Internal Standardisation Octopole Reaction Cell ICP-QMS by Normal Sample Nebulisation

A method for the determination of Ge, As, Se and Te in silicate samples using isotope dilution-internal standardisation (ID-IS) octopole reaction cell (ORC) ICP-QMS by normal sample nebulisation was developed. The method does not involve either hydride generation or ion exchange. Germanium, Se and Te were determined by isotope dilution (ID), and As was determined by ID-IS. A silicate sample with an added Ge-Se-Te spike was digested with an HF-HNO₃-HBr mixture, dried, re-dissolved with HF and the supernatant liquid was directly aspirated into an ORC-ICP-QMS instrument with He or H₂ gas. No matrix effects were observed down to a dilution factor (DF) of ∼ 70 for Ge, Se and Te and DF of ∼ 1000 for As, which resulted in 3s detection limits in silicates of 2, 1, 0.1 and 4 ng g⁻¹, respectively. Advantages of the method are the simple sample introduction as well as a capability of determining S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by ID-IS-ICP-QMS/SFMS from the same solution. Furthermore, the total sample solution consumption was only 0.253 ml with DF = 2000. Therefore, only a 0.13 mg test portion was required. To demonstrate the applicability of this technique, Ge, As, Se and Te in eight silicate reference materials were determined, as well as S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta in four carbonaceous chondrites.     

硅酸盐聚乙稀醇冲洗液在新疆砂岩性铀矿钻探中的应用

分析并研究了硅酸盐聚合物冲洗液体系的作用机理,配制了一套专门针对砂岩性铀矿岩心钻探中复杂地层孔段长、极易引发多种孔内事故的冲洗液体系。生产实践证明,该冲洗液体系完全能够满足绳索取心钻进工艺各项性能要求,并在对付砂岩性复杂地层方面具有良好的效果。     

金在花岗质熔体中溶解度的初步实验研究

以合成花岗岩、水、不同浓度的盐酸溶液、氢氟酸溶液作为反应初始物,在850℃,100 MPa,接近于NNO的条件下开展了金在不同花岗质熔体中溶解度的实验研究,实验固液相产物中的金含量使用石墨炉原子吸收法测定。实验结果显示,金在花岗质熔体中的溶解度变化范围为1.87～156.62μg/g,流体相中金的溶解度为0.31～6.92μg/g;金在熔体相中的溶解度较其在共存液相中的高。花岗质熔体相中金的溶解度明显受熔体化学组成的影响,过碱性富钠花岗质熔体中金的溶解度明显高些;金在花岗质熔体中的溶解度随着熔体中Na2O/K2O摩尔比增大而增大;在氟氯共存岩浆体系中,氟含量变化对金在熔体相中的溶解度影响不明显,而液相中氯含量增大有利于提高金在流体相中的含量。     

胶质芽孢杆菌－蒙脱石相互作用实验研究

利用硅酸盐细菌研究了微生物对硅酸盐矿物的分解作用。选取层状硅酸盐矿物蒙脱石在30℃与一株编号为3025的硅酸盐细菌B.mucilaginosus进行交互作用,并利用电感耦合等离子体发射光谱仪(ICP-AES)分析溶液中Si、Al、Mg离子的出溶量,利用X射线衍射(XRD)和显微红外光谱(Micro-FTIR)分析微生物作用后矿物物相和微结构变化。发现经硅酸盐细菌作用后,蒙脱石化学成分及晶体结构发生了细微变化,为微生物活动促进粘土矿物分解作用研究提供了实验和理论依据。     

珠江三角洲滨海小流域离子化学特征及来源分析

在分析中山大学滨海小流域水循环综合试验基地内雨水、河水和地下水离子组分的基础上,讨论了该小流域内水体离子化学组分的特征及来源。结果显示:①河水中TDS变化范围为28.97～44.64 mg/l,平均值为33.90 mg/l;在离子化学组成中,阳离子以Na++K+为主,阴离子以Cl-和HCO3-为主;雨水中TDS的变化范围为0.88～26.07 mg/l,平均值为8.42 mg/l,离子含量变化幅度较大;地下水TDS变化范围为39.49～113.16 mg/l,均值为58.11 mg/l,约为流域河水的2倍,雨水的7倍;②海盐沉降中Ca2+、Mg2+、Na+、K+、SO42-的贡献率:雨季分别为6%、60%、47%、2%和15%,旱季分别为3%、41%、54%、2%、9%;③硅酸盐风化中,雨季:(Ca/Na)sil=0.31,(Mg/K)sil=0.21;旱季:(Ca/Na)sil=0.36,(Mg/K)sil=0.27;CO2消耗率为12.4 t/(km2.a);④河水中的NO3-和(SO42-)res主要来源于大气酸沉降,且具有旱季含量低、雨季含量高的特点;⑤R1潜水井受到一定程度的NO3-污染,NO3-的...     

X射线荧光光谱法测定高锶高钡的硅酸盐样品中主量元素

用百分总和检查硅酸盐岩石全分析数据的质量是分析工作者的传统做法,但对于微量元素含量较高的样品,采用X射线荧光光谱法(XRF)进行测定,如果不考虑微量元素的含量及其对主量元素基体效应的影响,往往会使主量元素含量更加偏离真实值。本文针对Sr、Ba含量较高的硅酸盐样品,通过人工配制标准样品,扩大了Sr、Ba校准曲线的定量范围,主量元素校准中加入Sr、Ba的基体校正系数,达到了主量元素定量更加准确可靠的实际效果。采用此方法分析国家标准物质,各主量元素的精密度(RSD)均小于2%;分析不参加回归的标准物质和人工配制的标准样品,主量元素的测量值与标准值(或参考值)基本一致。该方法可以满足硅酸盐的测定要求,主量元素各项结果的加和能够达到《地质矿产实验室测试质量管理规范》的一级标准(99.3%～100.7%)。     

An Optimised 1,10‐Phenanthroline Method for the Determination of Ferrous and Ferric Oxides in Silicate Rocks,Soils and Minerals

A precise, accurate and rapid method for the sequential determination of FeO and Fe₂O₃ in rocks, soils and some non‐refractory minerals by 1,10‐phenanthroline spectrophotometry is described. Fe(II) and Fe(III) were leached from the sample (?200 mesh) using a mixture of NH₄HF₂ and H₂SO₄ at 40–80 °C for 10 min on a hot plate. Both Fe(II) and Fe(III) could be conveniently estimated sequentially from the same reaction mixture at the μg g^?1 to percentage level. The method is better than the existing wet chemical methods, including the commonly used Pratt's titrimetric redox method, for Fe(II) and Fe(III) determinations in rock and soil samples in terms of precision, accuracy and rapidity. The throughput of the method was very high; at least forty to fifty samples could be estimated easily in a day. The results obtained compare favourably with those obtained by Pratt's method, as well as for certified/recommended values of a set of eleven certified reference materials having FeO and Fe₂O₃ contents in the range 0.21–14.63% and 0.58–8.48%, respectively. The optimised 1,10 phenanthroline method was found to be accurate to within 0.21% m/m FeO and 0.30% m/m Fe₂O₃ compared with the literature values of the certified reference materials studied.     

Effect of Mineral Dusts on the Growth of Silicate Bacteria S35

In order to compare the chemical compositions and physical properities of dusts on silicate bacteria S35, the chemical compositions of six kinds of mineral dusts have been analyzed and the changes of pH value, glucose （GLU）, electrolyte and Mn, Si, Fe before and after the dusts reacted with silicate bacteria S35 have been measured. The SEM analysis has been used to study the bacterial form and interface action status in the course of reaction between dusts and bacteria. The results show that these mineral dusts have different effects on experiment bacteria. Therefore, it is concluded that the effect of mineral dusts on silicate bacteria has correlation with the chemical compositions and physical properities of dusts.     

Precise and Accurate Doping of Nanoporous Silica Gel for the Synthesis of Trace Element Microanalytical Reference Materials

This study presents an experimental procedure to fabricate high‐purity silica glass containing a selected element at a specified mass fraction. The procedure was used to prepare glasses doped with trace‐level mass fractions of Ti with the goal of improving analytical confidence when measuring trace elements in quartz. Systematic tests were performed to determine the ideal conditions and procedures for doping nanoporous silica gel with the highest efficiency of dopant recovery. Silica gel was cleaned in concentrated HCl, immersed in a non‐polar doping medium at a controlled pH and doped with precise quantities of ICP‐MS standard solution. Using liquids composed of longer chain molecules as the doping medium diminishes recovery, suggesting that large molecules could obstruct nanopores to inhibit capillary uptake of the dopant. A control experiment using crystalline quartz reinforced the effectiveness of nanoporous silica gel for doping with trace‐level precision. Layered aggregates of silica gel doped with different Ti mass fractions were hot‐pressed to create multi‐layered reference materials that were analysed with multiple techniques at a variety of spatial scales. Analyses at the intra‐grain scale (cathodoluminescence scanning electron microscopy, electron probe microanalysis), at the single grain scale (SIMS), at the sample layer scale (EPMA, laser ablation‐ICP‐MS) and at the bulk scale (ICP‐OES) demonstrated acceptable homogeneity at sample volumes characteristic of most microanalysis techniques and show that nanoporous silica gel holds promise as a highly retentive doping substrate for preparing reference materials for laser‐, electron‐ and ion‐beam microanalysis.     

胶州湾沉积物-海水界面硅的交换速率及其影响因素探讨

采用实验室培养法在原位温度和溶氧条件下测定了胶州湾沉积物-海水界面硅的交换速率,并探讨了相关环境因子对界面交换速率的影响机制。结果表明,胶州湾沉积物-海水界面硅的交换表现为从沉积物向水体释放,其交换速率在947~4 889 μmol/（m2·d）范围内,平均速率为1 819 μmol/（m2·d）。表层沉积物中叶绿素a（Chl a）和总有机碳（TOC）是影响胶州湾沉积物-海水界面硅交换速率的主要环境因子,同时表层沉积物的含水率（φ）、生源硅（BSi）和粘土含量以及间隙水中溶解硅酸盐（DSi）对沉积物-海水界面硅的交换也有重要影响。由此可推知,胶州湾沉积物-海水界面硅的交换速率主要受生物活动和溶解-扩散双重过程调控,而表层沉积物粒度与底层水体中DSi对胶州湾硅的释放影响较小。