Search results for "reference material"
showing 10 items of 51 documents
Validation of Powder X-Ray Diffraction Following EN ISO/IEC 17025
2012
: Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase iden…
Systematic procedure for the preparation of sets of calibration standards for x-ray fluorescence analysis of ceramic materials
1998
A systematic procedure for the preparation of optimized sets of calibration solid standards for the x-ray fluorescence analysis of ceramic materials is described. The matrix of the contents of the N analytes in the n standards (n ≥ N) is calculated from an n x N experimental design matrix, and from the upper and lower limits of the calibration range for each of the N analytes. Two procedures, which are useful for taking into account analyte interactions, are proposed for constructing the experimental design matrix, i.e. the scroll procedure and the procedure of the centers. A program developed to help the analyst in designing and preparing the set of standards following the proposed procedu…
Direct determination of total mercury in phosphate rock using alkaline fusion digestion
2014
The aim of this work was to develop a new method to determine the mercury (Hg) concentrations in phosphate rock using a dedicated analytical instrument (the DMA80 Tricell by Milestone) that employs an integrated sequence of thermal decomposition followed by catalyst conversion, amalgamation and atomic absorption spectrophotometry. However, this instrument underestimates Hg concentrations when phosphorite and apatite rocks are investigated with a classic thermal decomposition treatment that complies with US EPA method 7473. Therefore, to improve the recovery of total Hg, we performed alkaline fusion digestion (AFD) directly inside the furnace of the instrument, using BCR(32) as a certified r…
Comparative evaluation of liquid chromatography versus gas chromatography using a β-cyclodextrin stationary phase for the determination of BTEX in oc…
2009
An HPLC method for the determination of benzene, toluene, ethylbenzene and o-xylene, m-xylene and p-xylene in occupational environments was developed and compared with a GC-MS method. Chromatographic analysis using a beta-cyclodextrin stationary phase was performed after active and passive air sampling by adsorption on activated charcoal and pressurized fluid extraction. The analytes were completely separated and quantified using both methods, although GC-MS provided better resolutions and lower detection limits than HPLC. The HPLC method was unsuccessfully applied to the determination of benzene in real samples because its sensitivity was too low. Both methods were applied to the analysis …
Species-Specific GC/ICP-IDMS for Trimethyllead Determinations in Biological and Environmental Samples
2005
An accurate and sensitive species-specific isotope dilution GC/ICPMS method was developed for the determination of trimethyllead (Me3Pb+) in biological and environmental samples. A trimethyllead spike was synthesized from 206Pb-enriched metallic lead by reaction of lead halide with methyllithium and subsequent formation of trimethyllead iodide. The isotopic composition of the spike solution was determined by GC/ICPMS after derivatization with tetraethylborate, and its concentration was determined by reverse isotope dilution analysis. The species-specific GC/ICP-IDMS method was validated by reference material CRM 605 (urban dust) certified for Me3Pb+. The method was also applied to determine…
Isotope dilution mass spectrometry as a calibration method for the analysis of trace elements in powder samples by LA-ICP-MS
2003
The applicability of the isotope dilution (ID) technique for trace element determinations in powdered solid samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is demonstrated. LA-ICP-IDMS combines the advantage of the isotope dilution technique as a definitive method with the powerful capability of LA-ICP-MS for a fast and direct multi-element analysis of solid samples. LA-ICP-IDMS therefore allows matrix-matched quantification of element concentrations without any external standard, which is not possible by other calibration strategies used in LA-ICP-MS, up to now. The sample preparation effort is kept minimal and consists of an addition of the corresponding…
Assessment of Five Monazite Reference Materials for U-Th/Pb Dating Using Laser-Ablation ICP-MS
2019
Monazite is a common accessory phosphate mineral that occurs under a wide range of pressure and temperature conditions in sedimentary, metamorphic and igneous rocks. Monazite contains high amounts of Th and U, rendering single monazite grains suitable for in-situ U-Th/Pb dating using laser ablation inductively-coupled mass spectrometry (LA-ICP-MS). Two key aspects of monazite dating that are critical for accurate age data with maximum precision are (i) optimized instrumental conditions to minimize analytical scatter and (ii) a well characterized reference material to ensure the accuracy of the obtained aged. Here, we analyzed five monazite reference materials (USGS 44069, 94-222, MAdel, Moa…
Recovering bronze metallurgy from archaeological artefacts for the production of reference materials in conservation science
2007
The production of reference Cu-based alloys is the first step of an original experimental protocol to be used in the field of conservation and restoration of metal artefacts. The production of these synthetic alloys has a double value. They can be used both as suitable substitutes of unique archaeological pieces for testing new materials and methods for conservation, and as guidelines for contemporary metal production. We report on a research activity focused on the recovery of the ancient production techniques from the investigation of archaeological copper-based artefacts. The chemical, physical and metallurgical characterization of several Cu-based artefacts, found in different Italian a…
Fractionation of mercury in sediments during draining of Augusta (Italy) coastal area by modified Tessier method
2013
Abstract A modified Tessier method was applied to sediments dredged from Augusta (Italy) coastal area with the purpose of establishing the amount and the forms in which mercury is present in the different sediment fractions. The mercury fractionation was made by measuring the concentration of the metal ion on the solutions and directly on the sediment fractions obtained by sequential extraction. The measurements on the solutions as well as that on the solid fractions were carried out by using a Direct Mercury Analyser, DMA 80. This new instrument does not require sample preparation, and gives results comparable to those obtained with CV-AAS and ICP-MS and few minutes are necessary for each …
Speciation of methylmercury in market seafood by thermal degradation, amalgamation and atomic absorption spectroscopy
2014
Sample thermal decomposition followed by mercury amalgamation and atomic absorption has been employed for the determination of methylmercury (MeHg) in fish. The method involves HBr leaching of MeHg, extraction into toluene, and back-extraction into an aqueous l-cysteine solution. Preliminary studies were focused on the extraction efficiency, losses, contaminations, and species interconversion prevention. The limit of detection was 0.018µgg(-1) (dry weight). The intraday precision for three replicate analysis at a concentration of 4.2µgg(-1) (dry weight) was 3.5 percent, similar to the interday precision according to analysis of variance (ANOVA). The accuracy was guaranteed by the use of for…