GGR Critical Review of Analytical Developments in 2008–2009: An Introduction

This collection of articles represents the fourth in a series of reviews in which authors have aimed at capturing the key advances in a range of analytical fields ( Hergt et al. 2005, 2006, 2008 ). The publication period under review is 2008–2009 and the intention here is to provide readers with a summary of the most influential developments published during this period, across a broad range of topics appropriate to the Earth and environmental sciences. Most authors comment on the ways in which the emphases of research in their specific fields of examination have changed over time. All note an increase in rigour and focus on data quality. Whether advances have taken place in instrumentation, sample manipulation or data deconvolution, there are a large number of dedicated scientists out there contributing to the high quality of geochemical data employed in geological and environmental research.     

电感耦合等离子体原子发射全谱直读光谱仪测定地质样品中的钽

采用电感耦合等离子体原子发射全谱直读光谱仪,以HF-HNO3-HClO4-HCl溶样,不经分离富集,直接测定地质样品(岩石、水系沉积物、土壤)中Ta。方法检出限可达0. 8μg/g。通过国家一级标准物质测试和其他样品以不同方法测定相比较,测定结果基本一致;GBW 07309标准物质6次测定的相对标准偏差(RSD)为12. 0%。     

高频熔样等离子体发射光谱标准加入法测定刚玉中硅钛

以Li2B4O7 为熔剂高频电感熔样,等离子体发射光谱标准加入法测定了刚玉中的硅和钛。方法的检出限Si为0. 05mg/L,Ti为0. 02mg/L;线性浓度上限Si为40mg/L,Ti为80mg/L;回收率为95. 2% ~104. 3%;RSD(n=6)为0. 88% ~1. 36%。     

Comparison of Recoveries by Lead Fire Assay and Nickel Sulfide Fire Assay in the Determination of Gold/ Platinum/ Palladium and Rhenium in Sulfide Ore Samples

We compared the recovery of gold, palladium and platinum by two fire assaying procedures, using nickel sulfide and lead as collectors. The presence of appreciable amounts of sulfide minerals in the sample caused interferences in both procedures. An in-house reference sample, a reference sample of high-grade sulfide ore and samples of high sulfide content from the Recsk porphyry copper ore in Hungary were analysed by both methods. The elements were determined by inductively coupled plasma-atomic emission (ICP-AES) and/or inductively coupled plasma-mass spectrometry (ICP-MS). It was found that for the sulfide ore samples, the recoveries of Au and Pd are sometimes lower by nickel sulfide fire assay than by lead fire assay. Recovery of Re by nickel sulfide fire assay was found to be low: the average recovery of five repeated analyses of the reference sample NIST SRM 330 was 9% with a relative standard deviation of 48%. Increasing the amount of S in the fusion flux gave better recovery.     

Use of Chelating Resin YPA4 Micro-Columns for the On-Line Preconcentration and Separation of Gold(III), Silver(I), Palladium(II) and Platinum(IV) in Geological and Environmental Samples and Their Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

A simple and selective method of flow injection (FI) using a micro-column packed with chelating resin YPA₄ as solid phase extractant was developed for the preconcentration and separation of trace amount of noble metals, Au(III), Ag(I), Pd(II) and Pt(IV), followed by ICP-AES determination. In HNO₃ media, the chelating resin was selective towards Au(III), Ag(I), Pd(II) and Pt(IV), and the analysed ions were readily desorbed quantitatively with 5 ml of 2.5% m/v thiourea. Effects of acidity, sample flow rate and concentration, elution solution and interfering ions on the recovery of the analytes were systematically investigated. Under optimum conditions, the adsorption capacities of YPA₄ for Au(III), Ag(I), Pd(II) and Pt(IV) were 67.2, 43.1, 64.8 and 27.6 mg per gram of resin in HNO₃ media, respectively. It was found that YPA₄ could be used for more than eight runs in HNO₃ media without loss of capacity. The proposed method was used for the determination of trace noble metals in geological and environmental samples, and the analytical results obtained were in good agreement with the recommended values.     

Trace Determination of Strontium and Barium in River Waters by Inductively Coupled Plasma-Atomic Emission Spectrometry Using an Ultrasonic Nebulizer

Inductively coupled plasma-atomic emission spectrometry in conjunction with an ultrasonic nebulizer was employed for the determination of Sr and Ba in river waters at parts per billion (μg l⁻¹) levels without pre-concentration. The ultrasonic nebulizer, equipped with a desolvation system, enhanced the analytical sensitivity by ten to twenty fold compared to conventional pneumatic nebulizers. The detection limits for Sr and Ba, ascertained from blanks and reference samples made in 0.05% NaCl solution, were 0.045 μg l⁻¹ and 0.16 μg l⁻¹ respectively. The accuracy of measurements, based on analyses of solutions of reference materials (G-2 and W-1) and multielement commercial standards (Merck®), was ± 10%. Replicate analyses of samples and reference samples showed measurement precision to be to be better than ± 5%, which is adequate considering that the concentration of Sr and Ba in river waters varies by one to two orders of magnitude.     

难熔元素铌钽铀锆在电热蒸发—等离子体发射光谱中氟化蒸发行为研究

提出了以聚四氟乙烯(PTFE)为氟化剂,氟化辅助ETV-ICP-AES测定难熔元素Nb、Ta、Zr和U的新方法。对待测元素的氟化蒸发行为进行了研究,并探讨了其相应的氟化蒸发机理。该法测定Nb、Ta、Zr和U的线性范围达4个数量级,检出限分别为50、90、16和120pg。     

感耦等离子体发射光谱法测定锆英石中主次痕量元素

研究了感耦等离子体发射光谱测定锆英石中３１种元素的方法，样品碱熔后不经分离富集直接测定；对共存元素间的谱线干扰及其消除进行了试验；设置了４个测定程序，标准加入回收率为９１％－１１４％，样品测定的ＲＳＤ（ｎ＝７）在０．７％－１８％范围。     

ICP—AES仪器装置的新进展

本综述回顾了近年来ICP-AES仪器装置的新进展,介绍了电荷转移成象器件和中阶梯光栅光谱仪联用、傅里叶变换光谱的应用、样品处理和进样装置的研制及TCP-AES仪器智能化等方面的近期成就。     

ICP—AES法测定硅石样品中多种杂质元素

用电感耦合等离子体原子发射光谱法(ICP-AES)对地质样品硅石中多种杂质元素进行测定。方法确定了各元素的检出限,回收率在92%至105%之间,RSD小于1.93%,实验表明,该方法简便快速,具有很低的检出限和良好的精密度、准确度。