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Certified Reference Materials (certified + reference_material)
Selected AbstractsTheoretical framework for the distribution of trace metals among the operationally defined speciation phases of a sedimentENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 4 2001René A. Nome Abstract The use of a model based on Langmuir's isotherm to evaluate the metal associated with separate geochemical phases of a sediment is proposed and its validity tested with sediments of certified composition. The model takes into account a standard procedure for a certified reference material (CRM601), which defines, experimentally, a set of sequential extractions that divide the sediment into four operational fractions. The derived equations allow the treatment of data from sediment of Flumendosa Lake, Italy, and certified material CRM601 and also allow the computation of corrected concentrations, i.e., the metal affinities for each fraction. Experimental values for Ni show its low sensitivity and an equal distribution among different phases, which suggests a similar adsorption mechanism in all cases. In the case of Cd, the corrected concentration in the Fe/Mn oxide phase is nine times higher than for the residual fraction. For sediment of the Bèsos River, Spain, results show the percentage distribution of Ni over different fractions. Affinity values for Ni on a Flumendosa Lake sediment have also been calculated. The present model is simple to apply and shows satisfactory agreement with experimental data. [source] Comparison of gas chromatography and liquid chromatography mass spectrometric measurements for high accuracy analysis of cholesterol in human serum by isotope dilution mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 9 2002Céline S. J. Wolff Briche Cholesterol measurements are of vital clinical importance and reliable reference materials are essential for method validation. Gas chromatography with mass spectrometry (GC/MS) is usually used for the high accuracy analysis of cholesterol by isotope dilution. A certified reference material for cholesterol content in human serum was analysed by isotope dilution utilising GC/MS and liquid chromatography mass spectrometry (LC/MS). The use of LC/MS avoided the need for a derivatisation step. Both LC/MS and GC/MS produced results on the measurement of cholesterol that agreed within 0.5% of the certified value. Moreover, the precision obtained for ratio measurement using both techniques are comparable and lead to relative expanded standard uncertainties (with a coverage factor of 2) varying between 0.2 and 0.5%. Copyright © 2002 John Wiley & Sons, Ltd. [source] Analytical sensitivity of arsenobetaine on atomic spectrometric analysis and the purity of synthetic arsenobetaine,APPLIED ORGANOMETALLIC CHEMISTRY, Issue 9 2006T. Narukawa Abstract Arsenobetaine is one of the main organoarsenic compounds that exist in living organisms. Determination errors in total arsenic analyses for organoarsenic compounds occur because analytical sensitivities depend upon the chemical forms of the compounds. However, information on the analytical sensitivity of arsenobetaine by ICP-MS and ICP-AES and the purity of commercially available arsenobetaine standards is lacking. BCR CRM 626 (arsenobetaine solution) is a certified reference material from IRMM with a certified concentration of arsenobetaine. The sensitivity and behavior of arsenobetaine on ICP-MS and ICP-AES were investigated using the BCR arsenobetaine. The analytical sensitivity and behavior of arsenobetaine using ICP-MS and ICP-AES were also investigated using a commercially available synthetic arsenobetaine, and were compared with results for BCR-AB based on a Japan calibration service system (JCSS) arsenic standard solution. In the results, arsenic determined directly in arsenobetaine showed about 15% greater sensitivity in analysis by ICP-MS and ICP-AES than did inorganic (JCSS) arsenic. Copyright © 2006 John Wiley & Sons, Ltd. [source] Renewable Ceramic (TiN) Ring Electrode in Stripping Voltammetry.ELECTROANALYSIS, Issue 16 2009Determination of Pb(II) Without Removal of Oxygen Abstract Characteristic features of the process of Pb(II) reduction and oxidation at a renewable ceramic ring electrode (RCRE) were studied by stripping voltammetry. The main constituents of the RCRE are: a specially constructed TiN ring electrode, a silver sheet used as silver counter/quasi-reference electrode and a silicon O-ring are fastened together in a polypropylene body. The renovation of this electrode is carried out through mechanical removal of solid contaminants and electrochemical activation in the electrolyte which fills the RCRE body. The optimal measurement conditions, composition of supporting electrolyte and procedures of the electrode activation were selected. The measurements were carried out from nondeaerated solutions. As shown on selected examples, RCRE exhibits good performance in underpotential deposition stripping voltammetry (UPD-SV) applied for the determination of lead(II) in synthetic solutions with and without surfactants and in certified reference materials. The peak current is proportional to the concentration of lead(II) over the range 2×10,9,1×10,7,mol L,1, with a 3, detection limit of 1×10,9,mol L,1 with an accumulation time of 30,s. The obtained results showed good reproducibility, (RSD=2,5%; n=5) and reliability. [source] Fast Simultaneous Adsorptive Stripping Voltammetric Determination of Ni(II) and Co(II) at Lead Film Electrode Plated on Gold SubstrateELECTROANALYSIS, Issue 14 2007Katarzyna Tyszczuk Abstract A fast adsorptive stripping voltammetric procedure for simultaneous determination of Ni(II) and Co(II) in the presence of nioxime as a complexing agent at an in situ plated lead film electrode was described. The time of determination of these ions was shortened due to the application of gold as a substrate for lead film. At gold substrate lead film formation and accumulation of Ni(II) and Co(II) complexes with nioxime proceeds simultaneously. To obtain a stable signals for both ions a simple procedure of activation of the electrode was proposed. Calibration graphs for an accumulation time of 20,s were linear from 5×10,9 to 1×10,7 mol L,1 and from 5×10,10 to 1×10,8 mol L,1 for Ni(II) and Co(II), respectively. The procedure with the application of a lead film electrode on a gold substrate was validated in the course of Ni(II) and Co(II) determination in certified reference materials. [source] Catalytic Adsorptive Stripping Voltammetric Procedure for Determination of Total Chromium in Environmental MaterialsELECTROANALYSIS, Issue 12 2006gorzata Grabarczyk Abstract A sensitive catalytic adsorptive stripping voltammetric procedure for determination of traces of total chromium in environmental samples is reported. The method is based on the preconcentration of a Cr(III)H2DTPA complex by adsorption at the HMDE from an acetate buffer solution at the potential ,1.0,V vs. Ag/AgCl. Total chromium was determined as Cr(III) after reduction of Cr(VI) to Cr(III) by NaHSO3. In order to stabilize the signal of Cr(III) the measurements were performed at 5,°C. The calibration graph for chromium for an accumulation time of 60,s was linear in the range from 5×10,10 to 5×10,8,mol L,1. The relative standard deviation for a chromium concentration of 1×10,8,mol L,1 was 3.9% (n=5). The detection limit for accumulation time of 60,s was about 8×10,11,mol L,1. The validation of the procedure was performed by the analysis of the certified reference materials. [source] Development of Cu and Zn Isotope MC-ICP-MS Measurements: Application to Suspended Particulate Matter and Sediments from the Scheldt EstuaryGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 2 2008Jérôme C.J. Petit isotopes de Cu et Zn; interférences spectrales et non spectrales; fractionnement de masse instrumental; MC-ICP-MS; sédiments The present study evaluates several critical issues related to precision and accuracy of Cu and Zn isotopic measurements with application to estuarine particulate materials. Calibration of reference materials (such as the IRMM 3702 Zn) against the JMC Zn and NIST Cu reference materials were performed in wet and/or dry plasma modes (Aridus I and DSN-100) on a Nu Plasma MC-ICP-MS. Different mass bias correction methods were compared. More than 100 analyses of certified reference materials suggested that the sample-calibrator bracketing correction and the empirical external normalisation methods provide the most reliable corrections, with long term external precisions of 0.06 and 0.07, (2SD), respectively. Investigation of the effect of variable analyte to spike concentration ratios on Zn and Cu isotopic determinations indicated that the accuracy of Cu measurements in dry plasma is very sensitive to the relative Cu and Zn concentrations, with deviations of ,65Cu from ,0.4, (Cu/Zn = 4) to +0.4, (Cu/Zn = 0.2). A quantitative assessment (with instrumental mass bias corrections) of spectral and non-spectral interferences (Ti, Cr, Co, Fe, Ca, Mg, Na) was performed. Titanium and Cr were the most severe interfering constituents, contributing to inaccuracies of ,5.1, and +0.60, on ,68/64Zn, respectively (for 500 ,g l,1 Cu and Zn standard solutions spiked with 1000 ,g l,1 of Ti or Cr). Preliminary isotopic results were obtained on contrasting sediment matrices from the Scheldt estuary. Significant isotopic fractionation of zinc (from 0.21, to 1.13, for ,66Zn) and copper (from ,0.38, to 0.23, for ,65Cu), suggest a control by physical mixing of continental and marine water masses, characterized by distinct Cu and Zn isotopic signatures. These results provide a stepping-stone to further evaluate the use of Cu and Zn isotopes as biogeochemical tracers in estuarine environments. L'étude présentée ici porte sur l'évaluation critique d'un certain nombre de paramètres contrôlant la précision et la justesse des mesures des isotopes de Cu et Zn, dans le cadre d'une application à du matériel particulaire estuarien. Une calibration de matériaux de référence (tels que le Zn IRMM 3702) par rapport aux matériaux de référence JMC Zn et NIST Cu a été effectuée avec des plasmas humides et secs (avec Aridus I et DSN-100) sur un MC-ICP-MS Nu. Différentes méthodes de correction de biais de masse ont été comparées. Plus de 100 analyses de matériaux de référence certifiés ont montré que la correction par l'intercalation d'un calibrateur entre chaque échantillon et la calibration externe empirique fournissaient les corrections les plus fiables, avec des précisions externes sur le long terme de 0.06 et 0.07, (2SD) respectivement. Les effets de la variation des rapports de concentrations entre analyte et spike sur les mesures des rapports isotopiques de Cu et Zn ont montré que la justesse des mesures pour Cu en plasma sec est très tributaire des concentrations relatives de Cu et Zn, avec des déviations de ,65Cu allant de ,0.4, (Cu/Zn = 4) à+0.4, (Cu/Zn = 0.2). Une estimation quantitative des interférences spectrales et non spectrales (Ti, Cr, Co, Fe, Ca, Mg, Na) a été faite. Ti et Cr se sont révélés être les constituants interférents les plus importants pouvant entraîner des erreurs de ,5.1, et +0.60, sur ,68/64Zn respectivement (pour des solutions standards à 500 ,g l,1 de Cu et Zn dopées avec 1000 ,g l,1 de Ti ou Cr). Des données isotopiques préliminaires ont été obtenues sur des matrices sédimentaires très différentes provenant de l'estuaire de Scheldt. Les fractionnements significatifs du zinc (de 0.21,à 1.13, pour ,66Zn) et du cuivre (de ,0.38,à 0.23, pour ,65Cu) suggèrent un contrôle par un processus physique de mélange entre des masses d'eaux continentales et marines ayant des signatures isotopiques de Cu et Zn distinctes. Ces résultats constituent un tremplin vers une utilisation future des isotopes de Cu et Zn comme traceurs biogéochimiques des environnements estuariens. [source] The Use of Reference Materials: A TutorialGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 1 2001Jean S. Kane reference materials; certified reference materials; method validation; traceability of measurement; geochemical analysis Any review of the analytical literature shows that, while reference materials are routinely used in laboratories world-wide, not all uses follow ISO Guide 33 (1989), which outlines best practices. Analytical data quality can suffer as a result. This paper reviews the various uses that the geoanalytical community has made of reference materials from a historical perspective, and suggests improvements in practice that would more closely follow ISO Guide 33 recommendations. Un examen de la littérature dans le domaine analytique montre que, si les matériaux de référence sont utilisés en routine dans les laboratoires du monde entier, ces derniers ne suivent pas toujours les recommandations du guide ISO 33 (1989a), qui souligne les bonnes pratiques de laboratoire. La qualité des données analytiques peut alors en souffrir. Cet article passe en revue les différentes utilisations des matériaux de référence par la communauté de géoanalyse, ceci d'un point de vue historique, et suggère des améliorations de pratiques pour suivre au mieux les recommandations du guide ISO 33. [source] Simultaneous determination of mono-, di- and tributyltin in environmental samples using isotope dilution gas chromatography mass spectrometryJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 5 2004Giuseppe Centineo Abstract The development of a rapid, precise and accurate speciation method for the simultaneous determination of mono-, di- and tributyltin in environmental samples is described. The method is based on using isotope dilution gas chromatography/mass spectrometry (GC/MS) with electron ionization, a widely used technique in routine testing laboratories. A mixed spike containing 119Sn-enriched monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) was used for the isotope dilution of the samples. Five molecular ions were monitored for each analyte, corresponding to the 116Sn, 117Sn, 118Sn, 119Sn and 120Sn isotopes. The detection at masses corresponding to 116Sn and 117Sn were used to correct for m + 1 and m + 2 contributions of 13C from the organic groups attached to the tin atom on the 118Sn, 119Sn and 120Sn masses with simple mathematical equations and the concentrations of the butyltin compounds were calculated based on the corrected 118Sn/119Sn and 120Sn/119Sn isotope ratios. The 119Sn-enriched multispecies spike was applied with satisfactory results to the simultaneous determination of MBT, DBT and TBT in three certified reference materials: two sediments, PACS-2 and BCR 646, and the mussel tissue CRM 477. The method was compared with a previously published GC/inductively coupled plasma MS isotope dilution procedure, developed in our laboratory, by injecting the same samples into both instruments. Comparable analytical results in terms of precision and accuracy are demonstrated for both atomic and molecular mass spectrometric detectors. Thus, reliable quantitative organotin speciation analysis can be achieved using the more widespread and inexpensive GC/MS instrument. Copyright © 2004 John Wiley & Sons, Ltd. [source] Optimisation of the headspace-solid phase microextraction for organomercury and organotin compound determination in sediment and biotaJOURNAL OF SEPARATION SCIENCE, JSS, Issue 4 2008Alejandra Delgado Abstract Headspace solid-phase microextraction was optimised for the simultaneous preconcentration of methylmercury (MeHg+), monobutyltin, dibutyltin, tributyltin, monophenyltin (MPhT), diphenyltin (DPhT), and triphenyltin (TPhT) from sediments and biota. Extraction time (3,24 min), extraction temperature (20,90°C), desorption time (1,10.4 min), desorption temperature (152,260°C), and sample volume (5,22 mL) were simultaneously optimised, while variables such as fibre type (30 ,m polydimethylsiloxane, PDMS), pH (acetic acid/sodium acetate, HOAc/NaOAc, 2 mol/L, pH , 4.8), the concentration of the derivatisation agent (sodium tetraethylborate, NaBEt4, 0.1% m/v), and the ionic strength (fixed by the buffer solution) were kept constant. The variables were optimised according to the experiments proposed by the MultiSimplex program and the responses were considered in order to establish the optimum conditions. The repeatability (relative standard deviation, RSD, 5,20.6%) and limits of detection (LODs, 0.05,0.97 ng/g) of the overall method were also estimated. The lowest precisions were obtained for DPhT and TPhT. The optimised preconcentration method was applied to the determination of MeHg+, butyl- and phenyltins in certified reference materials (IAEA-405 MeHg+ in estuarine sediment, BCR-646 butyl- and phenyltins in marine sediment, BCR-463 MeHg+ in tuna fish, DOLT-2 MeHg+ in dogfish liver, and BCR-477 butyltins in mussel tissue) by GC with microwave-induced plasma/atomic-emission detection. [source] EU Forum: The CREATE Project: development of certified reference materials for allergenic products and validation of methods for their quantificationALLERGY, Issue 3 2008R. Van Ree Allergen extracts have been used for diagnosis and treatment of allergy for around 100 years. During the second half of 20th century, the notion increasingly gained foothold that accurate standardization of such extracts is of great importance for improvement of their quality. As a consequence, manufacturers have implemented extensive protocols for standardization and quality control. These protocols have overall IgE-binding potencies as their focus. Unfortunately, each company is using their own in-house reference materials and their own unique units to express potencies. This does not facilitate comparison of different products. During the last decades, most major allergens of relevant allergen sources have been identified and it has been established that effective immunotherapy requires certain minimum quantities of these allergens to be present in the administered maintenance dose. Therefore, the idea developed to introduce major allergens measurements into standardization protocols. Such protocols based on mass units of major allergen, quantify the active ingredients of the treatment and will at the same time allow comparison of competitor products. In 2001, an EU funded project, the CREATE project, was started to support introduction of major allergen based standardization. The aim of the project was to evaluate the use of recombinant allergens as reference materials and of ELISA assays for major allergen measurements. This paper gives an overview of the achievements of the CREATE project. [source] Sensitive determination of bromine and iodine in aqueous and biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry using tetramethylammonium hydroxide as a chemical modifierRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 12 2008Hiroko Kataoka A procedure for the simultaneous determination of bromine and iodine by inductively coupled plasma (ICP) mass spectrometry was investigated. In order to prevent the decrease in the ionization efficiencies of bromine and iodine atoms caused by the introduction of water mist, electrothermal vaporization was used for sample introduction into the ICP mass spectrometer. To prevent loss of analytes during the drying process, a small amount of tetramethylammonium hydroxide solution was placed as a chemical modifier into the tungsten boat furnace. After evaporation of the solvent, the analytes instantly vaporized and were then introduced into the ICP ion source to detect the 79Br+, 81Br+, and 127I+ ions. By using this system, detection limits of 0.77,pg and 0.086,pg were achieved for bromine and iodine, respectively. These values correspond to 8.1,pg,mL,1 and 0.91,pg,mL,1 of the aqueous bromide and iodide ion concentrations, respectively, for a sampling volume of 95,µL. The relative standard deviations for eight replicate measurements were 2.2% and 2.8% for 20,pg of bromine and 2,pg of iodine, respectively. Approximately 25 batches were vaporizable per hour. The method was successfully applied to the analysis of various certified reference materials and practical situations as biological and aqueous samples. There is further potential for the simultaneous determination of fluorine and chlorine. Copyright © 2008 John Wiley & Sons, Ltd. [source] Development and validation of a liquid chromatography/tandem mass spectrometric method for the determination of 39 mycotoxins in wheat and maizeRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 18 2006Michael Sulyok This paper describes the first validated method for the determination of 39 mycotoxins in wheat and maize using a single extraction step followed by liquid chromatography with electrospray ionization triple quadrupole mass spectrometry (LC/ESI-MS/MS) without the need for any clean-up. The 39 analytes included A- and B-trichothecenes (including deoxynivalenol-3-glucoside), zearalenone and related derivatives, fumonisins, enniatins, ergot alkaloids, ochratoxins, aflatoxins and moniliformin. The large number and the chemical diversity of the analytes required the application of the positive as well as the negative ion ESI mode in two consecutive chromatographic runs of 21,min each. The solvent mixture acetonitrile/water/acetic acid 79,+,20,+,1 (v/v/v) has been determined as the best compromise for the extraction of the analytes from wheat and maize. Raw extracts were diluted 1,+,1 and were injected without any clean-up. Ion-suppression effects due to co-eluting matrix components were negligible in the case of wheat, whereas significant signal suppression for 12 analytes was observed in maize, causing purely proportional systematic errors. Method performance characteristics were determined after spiking blank samples on multiple levels in triplicate. Coefficients of variation of the overall process of <5.1% and <3.0% were obtained for wheat and maize, respectively, from linear calibration data. Limits of detection ranged from 0.03 to 220,µg/kg. Apparent recoveries (including both the recoveries of the extraction step and matrix effects) were within the range of 100,±,10% for approximately half of the analytes. In extreme cases the apparent recoveries dropped to about 20%, but this could be compensated for to a large extent by the application of matrix-matched standards to correct for matrix-induced signal suppression, as only a few analytes such as nivalenol and the fumonisins exhibited incomplete extraction. For deoxynivalenol and zearalenone, the trueness of the method was confirmed through the analysis of certified reference materials. Copyright © 2006 John Wiley & Sons, Ltd. [source] Determination of total urinary mercury by on-line sample microwave digestion followed by flow injection cold vapour inductively coupled plasma mass spectrometry or atomic absorption spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 15 2002M. Bettinelli The total mercury content in urine was determined by inductively coupled plasma mass spectrometry with the so-called cold vapour method after on-line oxidative treatment of the sample in a microwave oven (FI-MW-CV-ICPMS). Use of a KBr/KBrO3 mixture, microwave digestion, and the final oxidation with KMnO4, assure the complete recovery of the organic forms of Hg which would be difficult to determine otherwise if using only the CV-ICPMS apparatus. Quantitative recoveries were obtained for phenyl Hg chloride (PMC), dimethyl Hg (DMM), Hg acetate (MA) and methyl Hg chloride (MMC). Use of automatic flow injection microwave systems (FI-MW) for sample treatment reduces environmental contamination and allows detection limits suitable for the determination of reference values. Since no certified reference materials were commercially available in the concentration ranges of interest, the accuracy of the proposed procedure has been assessed by analysing a series of urine samples with two independent techniques, ICP-MS and AAS. When using the FI-MW-CV-ICP-MS technique, the detection limit was assessed at 0.03µg/L Hg, while with FI-MW-CV-AAS it was 0.2µg/L Hg. The precision of the method was less than 2,3% for FI-MW-CV-ICP-MS and about 3,5% for FI-MV-CV-AAS at concentrations below 1µg/L Hg. These results show that ICP-MS can be considered as a "reference technique" for the determination of total urinary Hg at very low concentrations, such as are present in non-exposed subjects. Copyright © 2002 John Wiley & Sons, Ltd. [source] | ||||||||||