石墨炉原子吸收光谱法测定土壤样品中镉   总被引：5，自引：0，他引：5  

卞莉  曹萍 《吉林地质》2005,24(2):115-117

采用磷酸氢二铵作基体改进剂塞曼扣背景石墨炉原子吸收光谱法测定土壤样品中镉，方法检出限DL=0．012μg／g，精密度RSD在3．55％～7．33％，满足了土壤样品中镉测定的镉质量要求。  相似文献   

Laser Ablation ICP-MS Developments and Trends for 2003     

Paul J. Sylvester 《Geostandards and Geoanalytical Research》2005,29(1):41-52

This annual review of laser-ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) covers the year 2003. Significant advances were made in understanding laser-sample interactions. In particular, research defined the distribution of particle sizes produced by the interplay of laser wavelength, laser pulse width and the gas environment of ablation. A link between particle sizes and elemental and isotopic fractionation at both the ablation site and in the ICP was established. Experimental 15 7 nm and femtosecond laser systems were tested with promising results. The number of applications of LA-ICP-MS in geology and environmental Earth science continued to grow with particular interest in element concentration and isotope ratio profiling of materials, linking composition to time scales. In situ isotopic ratio measurements were increasingly made using multicollector magnetic sector ICP-MS instruments. Other applications of wide interest included bulk sampling of rocks and ores prepared as lithium borate glasses; low level analysis of platinum-group elements, rhenium and gold in sulfides, metal and silicates; in situ uranium-lead zircon geochronology; and melt and fluid inclusion analysis.  相似文献   

GGR Critical Review of Analytical Developments in 2003     

Janet M. Hergt  L. Paul Bédard  Etienne Deloule  Kathryn L. Linge  Paul J. Sylvester  Michael Wiedenbeck  Jon D. Woodhead 《Geostandards and Geoanalytical Research》2005,29(1):5-52

The articles that comprise this critical review serve to draw attention to research papers published in specific fields of interest during 2003, provide critical comment on the relevance and importance of individual publications in these fields, and offer an overview of the comparative importance of advances in particular areas. In this way, these articles aim to assist experts in the field by keeping them informed of relevant recent publications, as well as providing an important resource for students or early career researchers who are embarking on studies in an area new to them. This year, five papers provide summaries of developments in bulk sample determinations employing (1) ICP-AES and ICP-MS (trace elements), (2) XRF and atomic absorption spectrometry and INAA, (3) isotope ratio measurements (TIMS, MC-ICP-MS, ICP-MS, ToF), as well as in situ measurements conducted using (4) secondary ion mass spectrometry and (5) laser ablation ICP-MS (trace element and isotope ratio determinations).  相似文献   

Determination of Lithium, Beryllium and Boron at Trace Levels by Laser Ablation-Inductively Coupled Plasma-Sector Field Mass Spectrometry   总被引：1，自引：2，他引：1  

Massimo Tiepolo  Alberto Zanetti  Riccardo Vannucci 《Geostandards and Geoanalytical Research》2005,29(2):211-224

The analytical capabilities of laser ablation (LA)-ICP-MS in determining Li, Be and B at trace levels in geological samples have been tested on a series of glass reference materials and natural samples. The LA-ICP-MS instrument used consisted of a sector-field ICP-MS coupled with a laser ablation microprobe operating at either 266 or 213 nm wavelength. Reference glasses from NIST (SRM 612, 614 and 616) and MPI-DING (KL2-G, ML3B-G, StHs6/80-G, GOR128-G, GOR132-G, T1-G and ATHO-G) were selected to develop the analytical method and to assess the best instrumental configuration. A series of calcic amphiboles with different Li, Be and B concentrations were also analysed using both LA-ICP-MS and SIMS to test the applicability of the method to natural minerals. Results indicated that with a spot size of 40 μm the agreement between measured and reference values of Li, Be and B is generally better than 10% for NIST SRM 612 and 20% for NIST SRM 614. Average reproducibility at the 2s level was 10% for Li, 20% for Be and 15% for B. Limits of detection were approximately 100 ng g^-1 for Be and B and 200 ng g^-1 for Li. These results were confirmed by analyses carried out on natural amphiboles and compared well in terms of precision and accuracy with those commonly achieved by SIMS.  相似文献   

Preliminary Characterisation of New Glass Reference Materials (GSA-1G, GSC-1G, GSD-1G and GSE-1G) by Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry Using 193 nm, 213 nm and 266 nm Wavelengths   总被引：5，自引：1，他引：5  

Marcel Guillong  Kathrin Hametner  Eric Reusser  Stephen A. Wilson  Detlef Günther 《Geostandards and Geoanalytical Research》2005,29(3):315-331

New glass reference materials GSA-1G, GSC-1G, GSD-1G and GSE-1G have been characterised using a prototype solid state laser ablation system capable of producing wavelengths of 193 nm, 213 nm and 266 nm. This system allowed comparison of the effects of different laser wavelengths under nearly identical ablation and ICP operating conditions. The wavelengths 213 nm and 266 nm were also used at higher energy densities to evaluate the influence of energy density on quantitative analysis. In addition, the glass reference materials were analysed using commercially available 266 nm Nd:YAG and 193 nm ArF excimer lasers. Laser ablation analysis was carried out using both single spot and scanning mode ablation. Using laser ablation ICP-MS, concentrations of fifty-eight elements were determined with external calibration to the NIST SRM 610 glass reference material. Instead of applying the more common internal standardisation procedure, the total concentration of all element oxide concentrations was normalised to 100%. Major element concentrations were compared with those determined by electron microprobe. In addition to NIST SRM 610 for external calibration, USGS BCR-2G was used as a more closely matrix-matched reference material in order to compare the effect of matrix-matched and non matrix-matched calibration on quantitative analysis. The results show that the various laser wavelengths and energy densities applied produced similar results, with the exception of scanning mode ablation at 266 nm without matrix-matched calibration where deviations up to 60% from the average were found. However, results acquired using a scanning mode with a matrix-matched calibration agreed with results obtained by spot analysis. The increased abundance of large particles produced when using a scanning ablation mode with NIST SRM 610, is responsible for elemental fractionation effects caused by incomplete vaporisation of large particles in the ICP.  相似文献   

Microcrack networks in granite affected by a fault zone: Visualization by confocal laser scanning microscopy     

Celia T. Onishi  Ichiko Shimizu   《Journal of Structural Geology》2005,27(12):170

Microcracks in the Cretaceous Ryoke-type granite in Japan were investigated by using deep drilling core samples collected in the Mizunami Underground Research Project of the Japan Nuclear Cycle Development Institute (JNC). The granite body suffered brittle deformation associated with Tertiary thrust movement. Based on core-scale and microscopic deformation features, the drill core from a depth of 300 to 700 m is divided into four domains, i.e. (A) undeformed granite, (B) granite intruded by cataclastic seams, (C) fractured granite in the fault damage zone, and (D) foliated cataclasite at the fault center. To characterize microcrack geometries in each domain, we employed the impregnation method using a low-viscous acrylic resin doped with fluorescent agents and captured the microcrack images by confocal laser scanning microscopy (CLSM). The CLSM image in the fault damage zone revealed anisotropic development of microcrack networks related to the fault movement. Both CLSM observation and porosity measurements reveal a drastic increase of micro-pores in the foliated cataclasite, possibly caused by fragmentation, and granulation and crack sealing in the fault zone.  相似文献   

Structural properties of (Mn1-x Fe x )Nb2O6 columbites from X-ray diffraction and IR spectroscopy     

S. C. Tarantino  M. Zema  F. Maglia  M. C. Domeneghetti  M. A. Carpenter 《Physics and Chemistry of Minerals》2005,32(8-9):568-577

A suite of (Mn_1-x Fe _x )Nb₂O₆ (x=0, 0.05, 0.25, 0.50, 0.75, 1) columbite samples has been prepared by solid-state reaction from oxides. X-ray diffraction and spectroscopic investigations have been carried out in order to gain different perspectives on how the solid solution adapts at different length scales to cation mixing. X-ray powder diffraction and powder absorption IR spectroscopy data are presented. The powder diffraction data show that there is no significant excess volume of mixing on the Fe–Mn columbite join. All the unit-cell parameters decrease linearly as a function of increasing Fe content. Substitution of Fe²⁺ for the larger Mn²⁺ cation causes a decrease in the volume of the A polyhedron, which also becomes more regular with respect to both bond-length and edge-length distortion parameters. No significant variation of the B site has been observed. Wavenumber shifts of the IR peaks nearly all vary linearly with composition, consistent with linear variations of the lattice parameters. Line broadening has been quantified by autocorrelation analysis of the IR spectra. This is interpreted as suggesting that there is some element of local strain or positional disorder at the length scale of second or third nearest neighbours around sites occupied by Fe.  相似文献   

High-T phase transition of synthetic ANaB(LiMg)CMg5Si8O22(OH)2 amphibole: an X-ray synchrotron powder diffraction and FTIR spectroscopic study     

Gianluca Iezzi  Mario Tribaudino  Giancarlo Della Ventura  Fabrizio Nestola  Fabio Bellatreccia 《Physics and Chemistry of Minerals》2005,32(7):515-523

The synthetic amphibole Na_0.95(Li_0.95Mg_1.05)Mg₅Si₈O₂₂(OH)₂ was studied in situ at high-T, using IR OH-stretching spectroscopy and synchrotron X-ray powder diffraction. At room-T the sample has P2₁ /m symmetry, as shown by the FTIR spectrum. It shows in the OH region two well-defined and intense absorptions at 3,748 and 3,712 cm⁻¹, respectively, and two minor bands at 3,667 and 3,687 cm⁻¹. The main bands are assigned to the two independent O–H groups in the primitive structure. The two minor bands evidencing the presence of small amount of vacant A-site (^A□_0.05). With increasing T, these bands shift continuously and merge into a unique absorption at high temperature. A change as a function of increasing T is revealed by the evolution of the refined unit-cell parameters, whose trend shows a transition to C2/m at about 320–330°C. The spontaneous scalar strain, fitted with a tricritical 2–6 Landau potential, gives a T _c of 325(10)°C (β parameter = 0.27). Comparison with the second-order P2₁ /m ⇔ C2/m phase transition at 255°C for synthetic amphibole ^ANa_0.8^B(Na_0.8Mg_1.2)^CMg₅Si₈O₂₂(OH)₂ indicates that the substitution of Na with Li at the B-sites strongly affects the thermodynamic character and the T _c of the phase transition. The comparison of LNMSH amphiboles with cummingtonitic ones shows that the high-T thermodynamic behaviour is affected by A-site occupancy.  相似文献   

Diamond in metasedimentary crustal rocks from Pohorje,Eastern Alps: a window to deep continental subduction          下载免费PDF全文

M. Janák  N. Froitzheim  K. Yoshida  V. Sasinková  M. Nosko  T. Kobayashi  T. Hirajima  M. Vrabec 《Journal of Metamorphic Geology》2015,33(5):495-512

We report the first finding of diamond and moissanite in metasedimentary crustal rocks of Pohorje Mountains (Slovenia) in the Austroalpine ultrahigh‐pressure (UHP) metamorphic terrane of the Eastern Alps. Microscopic observations and Raman spectroscopy show that diamond occurs in situ as inclusions in garnet, being heterogeneously distributed. Under the optical microscope, diamond‐bearing inclusions are of cuboidal to rounded shape and of pinkish, yellow to brownish colour. The Raman spectra of the investigated diamond show a sharp, first order peak of sp³‐bonded carbon, in most cases centred between 1332 and 1330 cm^?1, with a full width at half maximum between 3 and 5 cm^?1. Several spectra show Raman bands typical for disordered graphitic (sp²‐bonded) carbon. Detailed observations show that diamond occurs either as a monomineralic, single‐crystal inclusion or it is associated with SiC (moissanite), CO₂ and CH₄ in polyphase inclusions_. This rare record of diamond occurring with moissanite as fluid‐inclusion daughter minerals implies the crystallization of diamond and moissanite from a supercritical fluid at reducing conditions. Thermodynamic modelling suggests that diamond‐bearing gneisses attained P–T conditions of ≥3.5 GPa and 800–850 °C, similar to eclogites and garnet peridotites. We argue that diamond formed when carbonaceous sediment underwent UHP metamorphism at mantle depth exceeding 100 km during continental subduction in the Late Cretaceous (c. 95–92 Ma). The finding of diamond confirms UHP metamorphism in the Pohorje Mountains, the most deeply subducted part of Austroalpine units.  相似文献   

Combining two filter paper‐based analytical methods to monitor temporal variations in the geochemical properties of fluvial suspended particulate matter          下载免费PDF全文

R. J. Cooper  B. G. Rawlins  B. Lézé  T. Krueger  K. M. Hiscock 《水文研究》2014,28(13):4042-4056

Many of the commonly used analytical techniques for assessing the properties of fluvial suspended particulate matter (SPM) are neither cost effective nor time efficient, making them prohibitive to long‐term high‐resolution monitoring. We present an in‐depth methodology utilizing two types of spectroscopy which, when combined with automatic water samplers, can generate accurate, high‐temporal resolution SPM geochemistry data, inexpensively and semi‐destructively, directly from sediment covered filter papers. A combined X‐ray fluorescence spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy approach is developed to estimate concentrations for a range of elements (Al, Ca, Ce, Fe, K, Mg, Mn, Na, P, Si, Ti) and compounds (organic carbon, Al_dithionate, Al_oxalate, Fe_dithionate, and Fe_oxalate) within SPM trapped on quartz fibre filters at masses as low as 3 mg. Calibration models with small prediction errors are derived, along with mass correction factor models to account for variations in retained SPM mass. Spectral pre‐processing methods are shown to enhance the reproducibility of results for some compounds, and the importance of filter paper selection and homogeneous sample preparation in minimizing spectral interference is emphasized. The geochemical signal from sediment covered filter papers is demonstrated to be time stable enabling samples to be stored for several weeks prior to analysis. Example results obtained during a heavy precipitation event in October 2012 demonstrate the methodology presented here has considerable potential to be utilized for high‐resolution monitoring of SPM geochemistry under a range of in‐stream hydrological conditions. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献