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1.
Hélène Balcone‐Boissard Agnès Michel Benoît Villemant 《Geostandards and Geoanalytical Research》2009,33(4):477-485
Concentrations of halogens (fluorine, chlorine, bromine and iodine) were determined in six geochemical reference materials (BHVO‐2, GS‐N, JG‐1, JR‐1, JB‐1b, JB‐2). Halogens were first extracted from powdered samples using a pyrohydrolysis technique, then hydrolysis solutions were analysed by ion chromatography for F and Cl and inductively coupled plasma‐mass spectrometry for Br and I. The detection limits in solutions were 100 μg l?1 for both F and Cl and 10 ng l?1 for Br and I. Considering the extraction procedure, performed on a maximum of 500 mg of sample and producing 100 ml of pyrohydrolysis solution, detection limits in rock samples were 20 mg kg?1 for F and Cl and 2 μg kg?1 for Br and I. The mean analytical errors on the studied composition ranges were estimated at 10 mg kg?1 for F and Cl, 100 μg kg?1 for Br and 25 μg kg?1 for I. The concentration values, based on repeated (generally > 10) sample analysis, were in good agreement generally with published values and narrowed the mean dispersion around mean values. Large dispersions are discussed in terms of samples heterogeneity and contaminations during sample preparation. Basaltic RMs were found to be more suitable for studies of halogen compositions than differentiated rock material, especially granites – the powders of which were heterogeneous in halogens at the 500 mg level. 相似文献
2.
Andrew J. Mason Gideon M. Henderson Anton Vaks 《Geostandards and Geoanalytical Research》2013,37(3):261-275
A new method for the simultaneous recovery of U, Th and Pb from ca. 0.5 g calcium carbonate samples for the purpose of U‐(Th)‐Pb geochronometry is presented. The protocol employs ion‐exchange chromatography. Standard anion exchange resin (AG 1‐X8 100–200 mesh) was used as the static phase, and 90% acetic acid was used as the mobile phase to elute the unwanted matrix components; dilute nitric acid was used to elute the U, Th and Pb. Blanks of 1.8 pg Th, 6.4 pg Pb and 8.4 pg U were obtained. The protocol was evaluated by determining the isotopic composition of U‐Th‐Pb separates obtained from an in‐house reference material (prepared from a natural speleothem) by MC‐ICP‐MS. An independently dated speleothem was also reanalysed. Based on these tests, the extraction protocol had an acceptable blank and produced a Pb separate sufficiently free of matrix‐induced instrumental biases to be appropriate for U‐Th‐Pb chronology. 相似文献
3.
New Thorium Isotope Ratio Measurements in Silicate Reference Materials: A‐THO,AGV‐2, BCR‐2, BE‐N,BHVO‐2 and BIR‐1 
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下载免费PDF全文 Marion Carpentier Abdelmouhcine Gannoun Christian Pin Olgeir Sigmarsson 《Geostandards and Geoanalytical Research》2016,40(2):239-256
A two‐step Th isolation protocol, involving micro‐columns of TRU‐Spec extraction chromatography material and AG1 resin, was evaluated. The MC‐ICP‐MS procedure included 232Th tailing characterisation and correction, and calibrator bracketing using an in‐house standard solution (ThS1) to correct for instrumental mass bias and Faraday cup to secondary electron multiplier relative gain. Repeated analyses of reference solutions (UCSC Th ‘A’, WUN, OU Th ‘U’, IRMM‐36) were consistent with published data. Six reference materials (A‐THO, BCR‐2, AGV‐2, BHVO‐2, BE‐N and BIR‐1) were processed. The average 230Th/232Th values obtained for these samples are in excellent agreement with published data. In addition, we report the first 230Th/232Th values for BE‐N and BIR‐1. The intermediate precisions for rock samples ranged from ± 0.24 to ± 0.49% (2 RSD) and were similar to those achieved for synthetic solutions, thereby supporting the overall validity of the chemical separation, data acquisition and reduction procedures. Counting statistics on the 230Th isotope was the most significant source of uncertainty. The intermediate precision of the mean 230Th/232Th for the Th‐depleted BIR‐1 (5.64 × 10?6 ± 0.27%, 2 RSD) is in the range of the analyses of other reference materials analysed in this study. 相似文献
4.
Qiaoyun Wang Akio Makishima Eizo Nakamura 《Geostandards and Geoanalytical Research》2010,34(2):175-183
A method to determine F and Cl in silicate materials by employing pyrohydrolysis and ion chromatography (IC) is described. Pyrohydrolysis involved mixing a pulverised sample (∼ 40 mg) with V2O5 (∼ 160 mg) and heating to 1100 °C under a wet oxygen flow in a quartz tube. Recovery yields of F and Cl were ∼ 97% using a NaF + NaCl standard solution. Detection limits of the pyrohydrolysis-IC method for silicate samples were 0.36 and 0.69 μg g-1 for F and Cl, respectively. Fluorine and Cl concentrations were determined in the reference materials JB-2, JB-3 and JA-1 from the GSJ; BCR-2, BHVO-1, BHVO-2, AGV-1 and AGV-2 from the USGS; and NIST SRM 610, 612 and 614 glasses. Precisions (RSD) for determinations of F were 1–13% (except NIST SRM 614) and 2–19% for Cl, and were dependent on the concentration and blank correction. Most results obtained in this study were in good agreement with those of previous studies. In comparison, the Na2CO3 + ZnO fusion method at 900 °C showed that the yields of F and Cl by alkaline fusion systematically decreased with fusion duration time. The yields were 84% and 83% for JB-3, inferring that F and Cl were lost in this alkaline fusion. 相似文献
5.
The characterization of refractory organic substances (ROS) is very complicated because of their heterogeneous structure. Size-exclusion chromatography with continuous detection of dissolved nitrogen (LC-DN), dissolved organic carbon (LC-DOC), and UV-absorbance (LC-UV) is a very useful analytical tool for the characterization of changes of ROS in natural aquatic systems and in technological treatment. The effect of natural, oxidative, and biochemical processes on formation and removal of ROS is described. Additionally the role of hydrolysable carbohydrates in the composition of ROS is presented. 相似文献
6.
Jie Li Xi‐Rong Liang Li‐Feng Zhong Xuan‐Ce Wang Zhong‐Yuan Ren Sheng‐Ling Sun Zhao‐Feng Zhang Ji‐Feng Xu 《Geostandards and Geoanalytical Research》2014,38(3):345-354
A novel preconcentration method is presented for the determination of Mo isotope ratios by multi‐collector inductively coupled plasma‐mass spectrometry (MC‐ICP‐MS) in geological samples. The method is based on the separation of Mo by extraction chromatography using N‐benzoyl‐N‐phenylhydroxylamine (BPHA) supported on a microporous acrylic ester polymeric resin (Amberlite CG‐71). By optimising the procedure, Mo could be simply and effectively separated from virtually all matrix elements with a single pass through a small volume of BPHA resin (0.5 ml). This technique for separation and enrichment of Mo is characterised by high selectivity, column efficiency and recovery (~ 100%), and low total procedural blank (~ 0.18 ng). A 100Mo‐97Mo double spike was mixed with samples before digestion and column separation, which enabled natural mass‐dependent isotopic fractionation to be determined with a measurement reproducibility of < 0.09‰ (δ98/95Mo, 2s) by MC‐ICP‐MS. The mean δ98/95MoSRM 3134 (NIST SRM 3134 Mo reference material; Lot No. 891307) composition of the IAPSO seawater reference material measured in this study was 2.00 ± 0.03‰ (2s, n = 3), which is consistent with previously published values. The described procedure facilitated efficient and rapid Mo isotopic determination in various types of geological samples. 相似文献
7.
Sune G. Nielsen Julie Prytulak Alex N. Halliday 《Geostandards and Geoanalytical Research》2011,35(3):293-306
We present the first technique to obtain precise and accurate vanadium (V) stable isotope compositions by chemical isolation and multi‐collector inductively coupled plasma‐mass spectrometry (MC‐ICP‐MS). Separation of V from matrix elements was achieved via five separate ion exchange columns. The procedure quantitatively removed Ti and Cr, which contain direct isobaric interferences on the minor isotope 50V. Isotope compositions were determined using a conventional standard solution‐sample bracketing technique. The V isotope composition for an in‐house secondary standard solution from BDH Chemicals was δ51V = ?1.19 ± 0.12‰ (2s, n = 600), measured as the per mil deviation relative to the composition of a widely available Specpure Alfa Aesar (AA) vanadium solution. This represents an improvement in measurement precision on previous techniques of almost two orders of magnitude. The effects of adding Cr, Ti and S to standard solutions were explored to determine the robustness of protocols. Only very low levels of these elements could be tolerated to obtain precise and accurate isotope compositions and was achieved with the chemical purification procedure. Standard solutions from AA and BDH processed as unknowns through the entire chemical separation and measurement protocols returned 100% yields and the same isotopic compositions as those of unprocessed standard solutions. 相似文献
8.
Humic substances (HS) were isolated from two contaminated groundwater samples (B22 and B53) from a site of a former gas facility. The isolation yielded almost only the fulvic acid fractions (FA). For characterization spectroscopic (UV, fluorescence) and chromatographic techniques (hydrophobic interaction chromatography – HIC as well as size-exclusion chromatography – SEC) were applied. The sample designated B22 FA was collected from the contamination plume whereas the sample B53 FA was collected downstream. Distinct differences were exhibited by these samples. The UV and fluorescence spectra as well as the HIC and SEC chromatograms of the B53 FA sample resemble those of the FA fraction obtained from natural water (groundwater, bog). The HIC and SEC chromatograms reveal the presence of organic compounds in B22 FA which can be derived from coal tar contaminants or their metabolites. Some of the compounds can be extracted from the FA fraction with non-polar organic solvents indicating adsorptive forces between the contaminants and the FA fraction. 相似文献
9.
A bulk aquatic natural organic material (NOM) was characterized by high-performance size exclusion chromatography (HPSEC) coupled with multi-angle laser light scattering (MALLS), UV-Vis, and refractive index detection. This technique was used to measure the molar mass and radius of the natural organic matter in solution. Results indicate that the NOM aggregates to a large extent at the concentrations used in this study (5... 15 mg mL–1). The solution conditions of pH and ionic strength were also shown to affect the measured size of NOM. The number and type of HPSEC columns also influenced these measurements. The importance of using multiple detectors was illustrated by peaks that were not detected by all the detectors. While these data are preliminary and have large errors associated with them, it is nevertheless an indication that HPSEC-MALLS can be used to investigate the effects of solution conditions and aggregation on the size of humic substances in solution. 相似文献
10.
An organic solvent‐free two‐step column procedure is presented that provided robust, high yield and super clean separation of Li from silicate rock sample matrices. The measured δ7Li value for BHVO‐2 of +4.29 ± 0.23‰ (1s) is comparable with the reported values. The δ7Li values for GSJ JP‐1 (+3.14 ± 0.41‰, 1s) and USGS DTS‐2 (+4.91 ± 0.34‰, 1s) presented here provide new reference values for ultramafic rock reference materials. 相似文献