Search results for "reference material"
showing 10 items of 51 documents
Development of a non-chromatographic method for the speciation analysis of inorganic antimony in mushroom samples by hydride generation atomic fluore…
2009
Abstract A simple and sensitive method has been developed for the direct determination of toxic species of antimony in mushroom samples by hydride generation atomic fluorescence spectrometry (HG AFS). The determination of Sb(III) and Sb(V) was based on the efficiency of hydride generation employing NaBH 4 , with and without a previous KI reduction, using proportional equations corresponding to the two different measurement conditions. The extraction efficiency of total antimony and the stability of Sb(III) and Sb(V) in different extraction media (nitric, sulfuric, hydrochloric, acetic acid, methanol and ethanol) were evaluated. Results demonstrated that, based on the extraction yield and th…
Determination of mercury in rice by cold vapor atomic fluorescence spectrometry after microwave-assisted digestion.
2010
Abstract A cold vapor atomic fluorescence spectrometry method (CV-AFS) has been developed for the determination of Hg in rice samples at a few ng g−1 concentration level. The method is based on the previous digestion of samples in a microwave oven with HNO3 and H2O2 followed by dilution with water containing KBr/KBrO3 and hydroxylamine and reduction with SnCl2 in HCl using external calibration. The matrix interferences and the effect of nitrogen oxide vapors have been evaluated and the method validated using a certified reference material. The limit of detection of the method was 0.9 ng g−1 with a recovery percentage of 95 ± 4% at an added concentration of 5 ng g−1. The concentration level …
Determination of total mercury in nuts at ultratrace level
2014
Abstract Total mercury, at μg kg−1 level, was determined in different types of nuts (cashew nut, Brazil nuts, almond, pistachio, peanut, walnut) using a direct mercury analyser after previous sample defatting and by cold vapour atomic fluorescence spectrometry. There is not enough sensitivity in the second approach to determine Hg in previously digested samples due to the strong matrix effect. Mercury levels in 25 edible nut samples from Brazil and Spain were found in the range from 0.6 to 2.7 μg kg−1 by using the pyrolysis of sample after the extraction of the nut fat. The accuracy of the proposed method was confirmed by analysing certified reference materials of Coal Fly Ash-NIST SRM 1633…
Simultaneous determinations of zirconium, hafnium, yttrium and lanthanides in seawater according to a co-precipitation technique onto iron-hydroxide.
2013
Very low concentrations (pg mL(-1) or sub-pg mL(-1) level) along with the high salinity are the main problems in determining trace metal contents in seawater. This problem is mainly considered for investigations of naturally occurring YLOID (Y and Lanthanides) and Zr and Hf in order to provide precise and accurate results. The inductively coupled plasma mass spectrometry (ICP-MS), both in high and low resolution, offers many advantages including simultaneous analyses of all elements and their quantitative determination with detection limits of the order of pg mL(-1). However in the analysis of YLOID in seawater, a better determination needs an efficient combination of ICP-MS measurement wit…
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…
Non-chromatographic speciation of toxic arsenic in fish
2004
Abstract A rapid, sensitive and economic method has been developed for the direct determination of toxic species of arsenic present in fish and mussel samples. As(III), As(V), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were determined by hydride generation–atomic fluorescence spectrometry using a series of proportional equations without the need of a chromatographic previous separation. The method is based on the extraction of arsenic species from fish through sonication with HNO3 3 mol l−1 and 0.1% (m/v) Triton and washing of the solid phase with 0.1% (m/v) EDTA, followed by direct measurement of the corresponding hydrides in four different experimental conditions. The li…
Determination of arsenic compounds in beverages by high-performance liquid chromatography-inductively coupled plasma mass spectrometry.
2005
Arsenic compounds including arsenous acid (As(III)), arsenic acid (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) were separated by high-performance liquid chromatography (HPLC) and detected by inductively coupled plasma mass spectrometry (ICP-MS). A Hamilton PRX-100 anionic-exchange column and a pH 8.5 K(2)HPO(4)/KH(2)PO(4) 5.0x10(-3)molL(-1) mobile phase were used to achieve arsenic speciation. The separation of arsenic species provided peaks of As(III) at 2.75min, DMA at 3.33min, MMA at 5.17min and As(V) at 12.5min. The detection limits, defined as three times the standard deviation of the lowest standard measurements, were found to be 0.2, 0.2, 0.3 and 0.5ngmL(-1) f…
Assessing the particle size of a broadly dispersed powder by complementary techniques
1998
The experimental determination of reliable particle size distribution curves and statistical parameters of broad distributions is known to be a difficult task. This problem is addressed here in an attempt to characterize the granularity of three distinct batches of a pharmaceutical powder (fenofibrate from Fournier Laboratories). The methodology consists in comparing the results, expressed in terms of surface based mean diameter, as obtained by three complementary techniques, namely optical microscopy image analysis, laser light low angle diffraction and surface area measurement by krypton physisorption. These techniques are applied in parallel to the material of interest and to a certified…
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 …
Direct and fast determination of polychlorinated biphenyls in contaminated soils and sediments by thermal desorption-gas chromatography-tandem mass s…
2019
Abstract A direct procedure based on thermal desorption-gas chromatography-tandem mass spectrometry (TD–GC–MS–MS) was developed for the fast extraction of seven polychlorinated biphenyls (PCBs) from sediments and soils. PCBs were directly extracted, from 20 to 75 mg of sample, without any chemical pre-treatment or use of organic solvents, after the addition of 10 µL internal standard (PCB 195) in acetone. Sample treatment was totally automated. PCBs were extracted at 250 °C for 20 min, using a helium flow and the PCBs were trapped in a cryogenic Tenax trap at −10 °C. After that, analytes were directly desorbed at 270 °C and introduced to the GC–MS–MS system. Recoveries were established usin…