Acute and chronic exposure to arsenic is a growing problem in the industrialized world. Arsenic is a potent carcinogen and
toxin in humans. In the body, arsenic is metabolized to produce several species, including inorganic forms, such as trivalent
(AsIII) and pentavalent (AsV), and the methylated metabolites such as monomethylarsonic acid, (MMAV), and dimethylarsinic acid (DMAV), in addition to arsenobetaine (AsB) which is ingested and excreted from the body in the same form. Each of these species
has been reported to possess a specific but different degree of toxicity. Thus, not only is the measurement of total As required,
but also quantification of the individual metabolites is necessary to evaluate the toxicity and risk assessment of this element.
There are a large number of reference materials that are used to validate methodology for the analysis of As in blood and
urine, but they are limited to total As concentrations. In this study, the speciation of five arsenic metabolites is reported
in blood and urine from commercial available control materials certified for total arsenic levels. The separation was performed
with an anion exchange column using inductively coupled plasma mass spectrometry as a detector. Baseline separation was achieved
for AsIII, AsV, MMAV, DMAV, and AsB, allowing us to quantify all five species. Excellent agreement between the total arsenic levels and the sum of the
speciated As levels was obtained. 相似文献
An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium pyrrolidinedithiocarbamate (APDC) in citrate buffer and the chelate is extracted into isobutyl methyl ketone (IBMK), which is separated from the aqueous phase by means of a newly designed dual-conical gravitational phase separator. A metered amount of the organic eluate is aspirated and stored in the PTFE holding coil (HC) of the SI-system. Afterwards, it is dispensed and mixed with an aqueous back extractant of dilute nitric acid containing Hg(II) ions as stripping agent, thereby facilitating a rapid metal-exchange reaction with the APDC ligand and transfer of the Cd into the aqueous phase. The aqueous phase is separated in a second dual-conical gravitational phase separator, and 30 μl of it is entrapped and metered in a sample loop (SL) and subsequently introduced via air segmentation into the graphite tube for analyte quantification. The ETAAS determination is performed in parallel with the separation/preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng l−1, along with a sampling frequency of 13 h−1 were obtained at a sample flow rate of 6.0 ml min−1. The precision (R.S.D.) at the 0.4 μg l−1 level was 1.8% as compared to 3.2% when quantifying the organic extractant directly. The applicability of the procedure is demonstrated for the determination of trace levels of cadmium in three certified reference materials. 相似文献
A chitosan resin functionalized with 3-nitro-4-amino benzoic acid moiety (CCTS-NABA resin) was newly synthesized for the collection/concentration of trace molybdenum by using cross-linked chitosan (CCTS) as base material. The carboxyl group of the moiety was chemically attached to amino group of cross-linked chitosan through amide bond formation. The adsorption behavior of molybdenum as well as other 60 elements on the resin was examined by passing the sample solutions through a mini-column packed with the resin. After the elution of the elements collected on the resin with 1 M HNO3, the eluates were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic emission spectrometry (ICP-AES).
The CCTS-NABA resin can adsorb several metal ions, such as vanadium, gallium, arsenic, selenium, silver, bismuth, thorium, tungsten, tin, tellurium, copper, and molybdenum at appropriate pHs. Among these metal ions, only molybdenum could be adsorbed almost completely on the resin at acidic regions. An excellent selectivity toward molybdenum could be obtained at pH 3–4. The adsorption capacity of CCTS-NABA resin for Mo(VI) was 380 mg g−1 resin. Through the column pretreatment, alkali and alkaline earth metals in river water and seawater samples were successfully removed.
The CCTS-NABA resin was applied to the adsorption/collection of molybdenum in river water and seawater samples. The concentrations of molybdenum in river water samples were found in the range of 0.84 and 0.95 ppb (ng g−1), whereas molybdenum in seawater was about 9 ppb. The validation of the proposed method was carried out by determining molybdenum in the certified reference materials of SLRS-4, CASS-4, and NASS-5 after passing through the CCTS-NABA resin; the results showed good agreement with the certified values. 相似文献
About Perrhenates. 3 On the Structure of the Mesoperrhenate Na3[ReO5] By tempering powder samples (prepared from mixtures of binary oxides: Na2O2/ReO2 and Na2O/ReO3 respectively, Na : Re = 3 : 1, Ar and O2 atmosphere respectively, 400–450°C, corundum boat) in a closed Ag cylinder (500–550°C, 10 d) yellow single crystals of Na3ReO5, sensitive to moisture, were grown. The compound crystallizes trigonal, space group P31, P32 respectively, with a = 5.544(1), c = 13.580(7) Å, Z = 3, drö. = 4.62 g/cm3. The crystal structure [4-circle diffractometer data, 1091 I0(hkl), AgKα, R = 6.14, Rw = 6.08%] is characterized by “isolated” bipyramids ReO5. Na+ ions are occupying all the tetrahedral (Na2, Na3) and octahedral (Na1) holes of the pseudocubic face centred (c/a = 2.441) Re part of the lattice; resulting in a Na3Re kation framework corresponding to the Li3Bi type of structure. Effective Coordination Numbers (ECoN), the Madelung Part of Lattice energy (MAPLE) and the charge distribution (CHARDI) are computed and discussed. 相似文献
Precise conductances for tetrabutylammonium tetrabutylboride (Bu4NBBu4) at 25°C have been measured in a number of nonaqueous solvents, and the data have been analyzed by the 1957 Fuoss-Onsager conductance equation. Limiting ion conductances for the Bu4N+ ion at infinite dilution 0(Bu4N+) in various solvents have been evaluated by dividing 0 values of the salt into two equal parts. The 0(Bu4N+) values so obtained are in fairly good agreement (within±0.1–3.5%) with the corresponding values determined from direct transference number measurements in these solvents. 相似文献
The most sensitive emission lines for the elements B, Be, Co and Mo are strongly influenced by disturbing emission lines of Fe using normal optical resolution. The advantages of high resolution, applying the new ICP-spectrometer JY 38 Plus (Jobin-Yvon, France) with the 2400 lines/mm grating measuring in the 1st and 2nd order will be discussed. Beside the concentrations in soils, sediments and sludges, applying aqua regia and HF decomposition methods, the detection limits in these matrices will be given. The possibilities of ICP-spectrometry for the determination of the above-mentioned elements are shown at the examples of SRMs (standard reference materials). The materials used here were three soils and three sludges from the BCR (Community Bureau of Reference, European Communities) and one sediment from NBS (National Bureau of Standards, USA). For example, the most sensitive and normally used line for the determination of boron at 249.7733 nm cannot be used in case of this type of matrix due to normally high Fe-concentrations and due to a strong Fe-interference. Therefore, it is necessary to use the line at 249.6778 nm, where an interference-free measurement can be achieved in case of high optical resolution. The measured B-contents in these samples are in the range of 20 to 60 g/g, for Co in the 10 g/g region, for Be well below 1 g/g, for Sn between 3 and 400 g/g. Mo was only detectable in the sludge samples (limit of determination 0.5 g/g).Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria 相似文献
The determination of extractable trace metal contents in soil using single extraction procedures is currently performed in many laboratories to assess the bioavailable metal fraction (and related phytotoxic effects) and the accessability to the environment (e.g. contamination of ground waters). Owing to the need for validation of the extraction schemes used and of the analytical techniques, the EC Measurements and Testing Programme (formerly BCR) has organized a project for improving the quality of determination of extractable trace metal contents in soil, the first step being an interlaboratory study to adopt common extraction procedures and the second being a certification campaign to certify two soils for their extractable trace element contents following these procedures. This paper gives a brief overview of the project organisation and describes the preparation, homogeneity and stability studies of two soil candidate reference materials (sewage sludge-amended and terra rossa soils). 相似文献
Taylor-Couette flow subject to a Coriolis force is studied experimentally and numerically. In the experiment, the Couette apparatus is mounted on a turntable with the axis of the cylinders orthogonal to the rotation vector of the turntable. The Coriolis force stabilizes the fluid against the onset of Taylor vortices and alters the velocity fields, both above and below the transition from the initial flow. At small dimensionless turntable frequencies, the transition yields time-independent Taylor vortices which are tilted with respect to the cylinder axis. At larger there is a direct transition to turbulence. We determine the first-order correction to the classical Couette initial flow, to account for the effects of the Coriolis force, by expanding in powers of. We present numerical results for the axial velocity (the only nonvanishing correction term to order) in the infinite-cylinder approximation. 相似文献