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1.
Iron (Fe) and copper (Cu) are essential metals in physiological cell metabolism. While Fe is easy to determine biochemically in histological slices, Cu and zinc (Zn) distribution is frequently critical in confirming the presence of an overload in disturbed Fe/Cu metabolism. To analyze Fe, Cu and Zn in a near histological resolution, energy dispersive microscopic synchrotron radiation X-ray fluorescence was applied.In normal liver tissue, after fixation and imbedding in paraffin, mean Fe, Cu and Zn concentrations were 152 ± 54, 20.1 ± 4.3 and 88.919.5 μg/g sample weight, respectively. No substantial, characteristic differences in their distribution were found in the two-dimensional scans. In slices from patients with hemochromatosis mean Fe, Cu and Zn concentrations were 1102 ± 539, 35.9 ± 14.6 and 27.2 ± 6.7 μg/g sample weight, respectively. Additionally, a significant decrease in phosphorus and sulphur concentrations existed. An increased Cu around cirrhotic regenerations nodules is mostly associated with a lymphocytic infiltration in this region. Analyzing concentrations of Fe in different regions of the samples show a clear negative dependency between Fe and Cu, Cu and Zn, but a positive one between Fe and Zn.Conclusion: With a focal beam size of 15 μm in diameter a resolution of the elemental distribution was achieved which is widely comparable with stained histological slices (20× light microscope). The analysis of simultaneous determined elements reveals metabolic differences between Fe, Cu and Zn in liver tissue from patients with hemochromatosis.  相似文献   

2.
A versatile route has been explored for the synthesis of nanorods of transition metal (Cu, Ni, Mn, Zn, Co and Fe) oxalates using reverse micelles. Transmission electron microscopy shows that the as-prepared nanorods of nickel and copper oxalates have diameter of 250 nm and 130 nm while the length is of the order of 2.5 μm and 480 nm, respectively. The aspect ratio of the nanorods of copper oxalate could be modified by changing the solvent. The average dimensions of manganese, zinc and cobalt oxalate nanorods were 100 μm, 120 μm and 300 nm, respectively, in diameter and 2.5 μm, 600 nm and 6.5 μm, respectively, in length. The aspect ratio of the cobalt oxalate nanorods could be modified by controlling the temperature.The nanorods of metal (Cu, Ni, Mn, Zn, Co and Fe) oxalates were found to be suitable precursors to obtain a variety of transition metal oxide nanoparticles. Our studies show that the grain size of CuO nanoparticles is highly dependent on the nature of non-polar solvent used to initially synthesize the oxalate rods. All the commonly known manganese oxides could be obtained as pure phases from the single manganese oxalate precursor by decomposing in different atmospheres (air, vacuum or nitrogen). The ZnO nanoparticles obtained from zinc oxalate rods are ~55 nm in diameter. Oxides with different morphology, Fe3O4 nanoparticles faceted (cuboidal) and Fe2O3 nanoparticles (spherical) could be obtained.  相似文献   

3.
An electrothermal vaporization (ETV) system useful for the analysis of solutions and slurries has been coupled with a sector-field inductively coupled plasma mass spectrometer (ICP–MS) equipped with an array detector. The ability of this instrument to record the transient signals produced for a number of analytes in ETV–ICP–MS is demonstrated. Detection limits for Mn, Fe, Co, Ni, Cu, Zn and Ga are in the range of 4–60 pg μL 1 for aqueous solutions and in the low μg g 1 range for the analysis of 10 mg mL 1 slurries of Al2O3 powders. The dynamic ranges measured for Fe, Cu and Ga spanned 3–5 orders of magnitude when the detector was operated in the low-gain mode and appear to be limited by the ETV system. Trace amounts of Fe, Cu and Ga could be directly determined in Al2O3 powders at the 2–270 μg g 1 level without the use of thermochemical reagents. The results well agree with literature values for Fe and Cu, whereas deviations of 50% at the 90 μg g 1 level for Ga were found.  相似文献   

4.
HCOOH, CH3COOH, and CH3CH2OH were used as chemical modifiers in a solution-cathode glow discharge. Emission was measured directly from the discharge, without a gas–liquid separator or a secondary excitation source. Emission from Ag, Se, Pb, and Hg was strongly enhanced, and the detection limits (DL) for these elements were improved by up to an order of magnitude using a combination of HCOOH and HNO3 compared to using HNO3 alone. The DL was measured for Mg (1 μg/L), Fe (10 μg/L), Ni (6 μg/L), Cu (6 μg/L), Pb (1 μg/L), Ag (0.1 μg/L), Se (300 μg/L), and Hg (2 μg/L). Coefficients of determination (R2) were between 0.9986 and 0.9999. A voltage of 1 kV was used, which produced a current of approximately 70 mA.  相似文献   

5.
Zn was electrochemically deposited onto square TiN electrodes with edge dimensions of 490 μm and 40 μm. These were fabricated by standard microfabrication techniques, which provide an extremely reproducible electrode for experimentation. Reliable constant-potential electrodeposition of Zn on the TiN was performed at −1.2 V, just below the Zn/Zn2+ redox potential. At more negative potentials, the hydrogen evolution reaction on TiN interfered with bulk metal electrodeposition, resulting in poor quality Zn films. A two-step plating procedure was shown to be most efficient for electrochemical deposition of Zn, with Zn nucleation on the TiN substrate at high cathodic overpotential during the first step and a second step of bulk metal growth on the nucleated layer at low cathodic overpotential. These results were most consistent with 3D progressive nucleation of Zn on the TiN surface. Using this procedure, deposits of Zn on 490 μm TiN electrodes were uniform. In contrast, Zn deposits on 40 μm electrodes formed high-surface area and volume surface structures resulting from preferential growth at the electrode corners due to enhanced hemispherical diffusion at these sites. This should enable the formation of high surface area, high current density Zn anodes on biocompatible TiN microelectrodes, which could find application as improved microanodes for implantable miniature power supplies, e.g., implantable glucose sensors and internal cardioverter defibrillators.  相似文献   

6.
The present area of study is located in the Upper Course of the Lerma River (UCLR). The Lerma is one of the most important rivers of Mexico, where it drains highly populated and industrialized regions. The aim of the present study is to determine the heavy metal concentration of Cr, Mn, Fe, Cu and Pb in dissolved and total phases of the UCLR by means of Total Reflection X-ray Fluorescence Spectrometry (TXRF). The surface water samples were collected at 8 sites distributed following the stream flow direction of the river. Four sampling campaigns were carried out in each site in a 1-year period. A sample preparation method was applied in order to obtain the total and dissolved fraction and to destroy the organic matter. The total heavy metal average concentration decrease in the following order: Fe (2566 μg/L) > Mn (300 μg/L) > Cu (66 μg/L) > Cr (21 μg/L) > Pb (15 μg/L). In general, the heavy metal concentrations in water of the UCLR are below the maximum permissible limits.  相似文献   

7.
This work introduces the feasibility of using sugar cane bagasse (SCB) – a sugar cane industry waste – as a selective solid phase extractor for Fe(III). The order of metal uptake capacities in μmol g?1 for the extraction of six tested metal ions from aqueous solution using static technique is Fe(III) > Cu(II) > Pb(II) > Zn(II) > Cd(II) > Co(II). Since SCB exhibits remarkable binding characteristics for Fe(III), special interest was devoted for optimizing its uptake and studying its selectivity properties under static and dynamic conditions. In this respect, batch experiments were carried out at the pH range 1.0–4.0, initial concentration of metal ion (10–100 μmol), weight of phase (25, 50, 75, 100, 125 and 150 mg) and shaking time (10, 30, 45, 60, 90, 120 and 150 min). FT-IR spectra of SCB before and after uptake of Fe(III) were recorded to explore the nature of the functional groups responsible for binding of Fe(III) onto the studied natural biosorbent. The equilibrium data were better fitted with Langmuir model (r2 = 0.985) than Freundlich model (r2 = 0.934). Moreover, Fe(III) sorption was fast and completed within 60 min. The adsorption kinetics data were best fitted with the pseudo-second-order type. As a view to find a suitable application of SCB based on its unique property as a benign sorbent, it was found that, Fe(III) spiked natural water samples such as doubly distilled water (DDW), drinking tap water (DTW), natural drinking water (NDW), ground water (GW) and Nile River water (NRW) was quantitatively recovered (>95.0%) using batch and column experiments, with no matrix interferences.  相似文献   

8.
This paper describes a new type of glow discharge (GD) ion source coupled to a time-of-flight mass spectrometer (TOFMS). The GD is operated in the microsecond pulse (μs-pulse) mode. The operational parameters of the μs-pulse GD were optimized against the ion signals, giving 180 Pa for the discharge pressure, 3 A for the transient discharge current, 1.75 kHz for the discharge frequency and 2 μs for the discharge pulse duration. Experimental results show that the discharge current in the μs-pulse mode can be one order of magnitude higher than that obtained in the d.c. mode. The structure of the interface between the μs-pulse GD and the mass spectrometer was found to be critical, and a Macor disc must be applied in front of the sampling orifice in order to shield the sampling plate from the anode of the GD to achieve both a good vacuum and the best sputtering. A transient sputtering rate of 24.4 μs s−1 mm−2 was reached in the μs-pulse mode and was significantly higher than that for the d.c.-GD. Typical mass spectra of brass and nickel samples were studied and are discussed. © 1997 Elsevier Science B.V.  相似文献   

9.
The environmental pollution due to the industrial wastewater of four different areas in the Gulf of Suez, Red Sea, Egypt, was studied. Adsorption capacities toward the concerned heavy metal ions Cu(II), Zn(II), Fe(II), and Pb(II) by multiwalled carbon nanotubes (MWCNTs) and modified-MWCNTs with 5,7-dinitro-8-quinolinol were investigated. MWCNTs as well as the modified-MWCNTs were characterized using Fourier transform infrared (FTIR), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). Adsorption of the studied divalent metal ions was measured by atomic absorption spectrometry (AAS). The effects of solution conditions such as pH, shaking time, metal ion concentration, ionic strength and adsorbent dosage on the adsorption process were also examined. The obtained results showed that removals of the heavy metal ions under consideration by MWCNTs are obviously dependent on the experimental conditions. The maximum adsorption capacities as calculated applying Langmuir equation to single ion adsorption isotherms were found to be 142.8 mg/g for Cu(II), 250 mg/g for Zn(II), 111.1 mg/g for Fe(II), and 200 mg/g for Pb(II) using MWCNTs; meanwhile, the modified-MWCNTs exhibited higher values of the respective maximum adsorption capacities as 333.3 mg/g for Cu(II), 500 mg/g for Zn(II), 200 mg/g for Fe(II), and 333.3 mg/g for Pb(II). Kinetic studies were also performed and the experimental data followed a pseudo-second order model of the adsorption process. The obtained results suggest that the tested adsorption systems of MWCNTs and modified-MWCNTs have suitable affinity toward the metal ion under consideration. Both systems could act as potentially applicable tool in environmental protection.  相似文献   

10.
The present research was conducted to study heavy metal contamination in roadside soil viz. (i) at sites having more than two traffic signals (ii) roads having only one traffic signal and (iii) roads having no traffic signals. The samples were collected and analyzed for seven heavy metals i.e. cadmium (Cd), lead (Pb), copper (Cu), nickel (Ni), iron (Fe), manganese (Mn) and zinc (Zn) by Atomic Absorption Spectroscopy (AAS) following the acid digestion of the respective soil samples. The range of the metals observed in soil having more than two traffic signals were Cd (0.17–1.01), Pb (259.66–2784.45), Cu (15.51–65.90), Ni (13.31–98.13), Fe (325.64–5136.37), Mn (57.95–166.43), and Zn (91.34–166.43) mg kg?1 respectively. Similarly, the range of metals analyzed in samples collected from the roadside having only one traffic signal were Cd (nd–0.80), Pb (145.95–308.09), Cu (0.82–18.04), Ni (18.29–59.36), Fe (88.51–3649.42), Mn (25.88–147.34) and Zn (8.97–106.11 mg kg ?1) respectively. However, the range of metals at roads having no traffic signals were Cd (0.0–0.57), Pb (8.34–58.20), Cu (2.88–5.81), Ni (3.34–73.80), Fe (55.34–332.81), Mn (2.98–98.73) and Zn (1.23–46.6 mg kg?1) respectively. Cd, Cu, Ni, Fe, Mn and Zn in soil were present within the normal range of background levels, whereas lead was reported in high concentration. The level of lead had a correlation with the traffic density attributing its origin to vehicular exhaust. The values from three different sites of monitoring suggest that automobiles are a major source of the studied metals for the roadside environment.  相似文献   

11.
Formation of the SEI layer on Si–Cu film electrode in the ionic liquid electrolyte of 1 M lithium bis(trifluoromethylsulfonyl)imide/1-methyl-1-propylpyrrolidinium bis(trifluoromethylsulfonyl)imide (LiTFSI/MPP-TFSI) was investigated using ex-situ ATR FTIR and X-ray photoelectron spectroscopy. The SEI layer is found to be composed of organic and inorganic compounds that are the decomposition products of MPP cation and TFSI anion, and effectively passivate the electrode surface during initial cycling. Formation of a stable SEI layer leads to an excellent capacity retention 98% of the maximum discharge capacity, delivering discharge capacities of > 1620 mAhg? 1 over 200 cycles. The data contribute to a basic understanding of SEI formation and composition responsible for the cycling performance of Si-based alloy anodes in ionic liquid electrolyte-based rechargeable lithium batteries.  相似文献   

12.
The present study is based on the measurement of selected metals (Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Pb, Sr and Zn) in the fruits of eight medicinal plants (Carrisa opeca, Phyllanthus emblica, Solanum nigrum, Zizyphus nummularia, Zizyphus mauritiana, Physalis minima, Opuntia dillenii and Phoenix dactylifera) and relevant soil samples by atomic absorption spectrometry. Highest average concentrations of Cu (14.4 mg/kg), Cr (19.0 mg/kg), and Zn (125 mg/kg) were found in the fruits of P. minima, C. opeca and Z. nummularia, respectively, while O. dillenii showed the elevated mean levels of Cd (3.49 mg/kg), Sr (61.4 mg/kg), Mg (0.21%), Ca (6.62%) and Mn (44.6 mg/kg). However, highest average levels of Pb (41.7 mg/kg) and Co (38.4 mg/kg) were found in Z. mauritiana. Overall, most of the fruit samples showed higher contributions of Ca and Mg, followed by Fe, Zn, Co and Pb. In the case of soil samples, highest concentration was observed for Ca, followed by Fe, Mg, Mn and Sr, while lowest concentration was shown by Cd. Bioaccumulation factors exhibited significantly higher accumulation of Co (0.813–1.829) and Pb (0.060–2.350) from the soil to the fruits. Principal component analysis revealed significant anthropogenic contributions of Pb, Fe and Co in the fruit samples. Contamination factors and enrichment factors of Cd and Pb in the soil indicated very high contamination and extreme enrichment of these metals.  相似文献   

13.
Cu-deposited TiO2 films were prepared by photoreduction of Cu(II) in the presence of sodium formate. With the initial Cu(II) concentrations more than 100 mg L?1, induction periods were observed before the transmittance decreased. Scanning electron microscopy indicated that Cu particles of 2.6 ± 0.5 μm were deposited isolatedly with much open space in the induction periods. The films prepared by changing the irradiation time within the induction periods showed a higher photocatalytic activity than a pure TiO2 for the degradation of methylene blue under the reaction condition without purging air.  相似文献   

14.
This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg 1 and 128 mg kg 1, respectively. The relative standard deviations were lower than 6% (n = 5). The accuracy of the entire procedure was checked with bovine liver from NIST (1577b) and determination of Cu and Zn using flame atomic absorption spectrometry after microwave-assisted sample digestion.  相似文献   

15.
A simple, rapid, sensitive and accurate spectrophotometric method for the determination of captopril in pure form and pharmaceutical formulations is developed. The procedure is based on the reaction of copper(II) with captopril in the presence of neocuproine (NC) (2,9-dimethyl-1,10-phenanthroline) reagent in acetate buffer at pH 5.0. Copper(II) is reduced easily by captopril to Cu(I)–neocuproine complex, which shows an absorption maximum at 448 nm. Beer’s law was obeyed in the concentration range 0.3–3.0 μg mL?1 with a minimum detection limit (LOD) of 0.039 μg mL?1 and a quantification limit (LOQ) of 0.129 μg mL?1. For more accurate results, Ringbom optimum concentration ranges was 0.5–2.7 μg mL?1. The apparent molar absorbtivity and Sandell sensitivity were calculated. The validity of the proposed method was tested by analyzing the pure and pharmaceutical formulations and compared well with those obtained by the official method and demonstrated good accuracy and precision.  相似文献   

16.
A slurry sampling electrothermal atomic absorption spectrometry method for the determination of Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn in powdered titanium dioxide is described. The behaviour of the titanium matrix in the atomizer and its interferences with the determination of Al, Fe, Co, Ni and Mn were studied. A tungsten carbide modified graphite tube was used to improve the signal shape and the repeatability for the determination of Fe. For all elements, except for Cd and Pb, quantification by a calibration curve established with aqueous standards was possible. No chemical modifier was used throughout in order to minimize contamination. For the contamination risk elements such as Ca, Fe, K, Mg, Na and Zn, the slurry sampling technique allows to achieve limits of detection (3σ of the blank) 5–20 times lower than the solution technique, resulting for these elements in values of 1, 3, 0.5, 0.5, 0.9 and 2 ng g−1, respectively, and, generally being in the range of 0.2 ng g−1 (Cd) to 10 ng g−1 (Al and Tl). The results obtained by the slurry sampling technique are compared with those of other independent methods including four solution methods and neutron activation analysis.  相似文献   

17.
Ti films sputtered on transparent fluorine-doped tin oxide glass substrates were anodized in fluoride-containing organic electrolyte in the presence of H2O. In this work, anodic TiO2 nanotubes (ATNs) as long as 9.2 ± 0.3 μm were obtained with high growth rate of 0.64 ± 0.3 μm min?1. We demonstrated the optimum anodization conditions for ATN growth on foreign substrates, were within the range of 0.3–0.5% (wt) NH4F, with 3–5% (vol) H2O at 60 V. XPS and ICP-MS were utilized to elucidate the increase of thickness and volume expansion obtained from the sputtered Ti film to their ATN forms. The ATN films exhibited excellent uniformity and adhesion to the substrates.  相似文献   

18.
LiFePO4/mesocarbon microbead (MCMB) cells of which the carbon electrodes were, respectively, coated with different metal layers were characterized for their charge/discharge cycle performance at 55 °C. The examined metals included Au, Cu, Fe, Ni, Co, and Ti, and the superficial layers were 30–50 nm in thickness and deposited by vacuum sputtering. It was found that the presence of a either Au or Cu layer remarkably reduces capacity fading, while the rest metals only accelerate fading. There was observed a consistent trend between the capacity fading rate and the amount of the soild-electrolyte-interphase (SEI) deposition; the faster the capacity fading, the greater amount of SEI materials appearing on the surface of cycled carbon electrode. Microscopic and composition analyses indicates that the superficial Au and Cu layers act as a sieve to collect the Fe ions that result form erosion of LiFePO4 before they diffuse into the interior of the carbon electrode, and that the so-deposited Fe particles do not show the tendency to catalyze the SEI formation, as in contrast to those directly deposited on the carbon surfaces.  相似文献   

19.
The present paper deals with the synthesis and characterization of Schiff base complexes of pyrazinamide an antitubercular drug. Metals selected for complexation are copper, silver, gold, zinc, mercury, iron and cobalt. The complexes have been suitably synthesized and isolated in pure powdered form. Analytical data agrees with the compositions M(L), M′(L)2 and M″(L)2·2H2O, respectively where M = Ag, M′ = Cu, Au, Zn and Hg and M″ = Fe and Co, ligand metal ratios were also confirmed by monovariation method and Job’s method of continuous variation. Molar conductance values suggest the non ionic nature of the complexes. The tentative structure assigned to the complexes on the basis of stoichiometry and analytical data were further supported by spectral studies viz; IR, NMR, magnetic susceptibility and electronic spectra. A preliminary attempt has also been made to compare the potencies of metal complexes with parent drug. The Cu and Ag complexes are giving encouraging results. Particle size studies further suggest that the drug molecule undergoes reduction in size on complexation.  相似文献   

20.
The Freundlich and Langmuir isotherms were used to describe the biosorption of Cu(II), Pb(II), and Zn(II) onto the saltbush leaves biomass at 297 K and pH 5.0. The correlation coefficients (R2) obtained from the Freundlich model were 0.9798, 0.9575, and 0.9963 for Cu, Pb, and Zn, respectively, while for the Langmuir model the R2 values for the same metals were 0.0001, 0.1380, and 0.0088, respectively. This suggests that saltbush leaves biomass sorbed the three metals following the Freundlich model (R2 > 0.9575). The KF values obtained from the Freundlich model (175.5 · 10−2, 10.5 · 10−2, and 6.32 · 10−2 mol · g−1 for Pb, Zn, and Cu, respectively), suggest that the metal binding affinity was in the order Pb > Zn > Cu. The experimental values of the maximal adsorption capacities of saltbush leaves biomass were 0.13 · 10−2, 0.05 · 10−2, and 0.107 · 10−2 mol · g−1 for Pb, Zn, and Cu, respectively. The negative ΔG values for Pb and the positive values for Cu and Zn indicate that the Pb biosorption by saltbush biomass was a spontaneous process.  相似文献   

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