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1.
A new self-tuning single-mode-focused microwave technology has been evaluated in this work to perform the quantitative routine extraction of organometallic species from solid matrices of environmental interest. Species-specific isotope dilution analysis has been employed to better investigate the real influence of the microwave-assisted extractions on the final results. The advantages of such methodology in comparison with other established microwave units for the routine speciation analysis of organomercury and organotin compounds are discussed (such as the capability of using disposable glass vials, a self-tuning mode to provide an accurate control of the temperature and pressure inside of the vials, and the possibility of performing automated sequence of extractions with low sample size). The results obtained in this work demonstrated that such technology provides a fast and reliable quantitative extraction of the organometallic species in a wide range of extraction conditions even when the multi-elemental (Sn and Hg) species-specific determination is carried out.  相似文献   
2.
《Analytical letters》2012,45(9):1691-1699
Abstract

Four kinds of mercury species (inorganic mercury (Hginorg), methylmercury (MeHg), total organic mercury (ΣHgorg), and insoluble mercury, deemed to be mercuric selenide (HgSe), were determined in the livers of dolphins from the Brazilian coast. The MeHg was identified and quantified in the toluene layer on a Gas Chromatograph with an Electron Capture Detector (GC-ECD). The ΣHgorg was isolated by acid leaching (H2SO4-KBr-CuSO4) and then extracted into CH2Cl2. The ΣHgorg and Hginorg were determined by Cold-Vapor Atomic Absorption Spectroscopy (CV-AAS). The MeHg was the smallest fraction of Hgtot, with a median of 9%, whereas the highest fraction of the Hgtot was as HgSe, corresponding to 53%. The fractions of Hginorg and ΣHgorg corresponded to 30% and 39%, respectively. The lowest fraction of MeHg and the highest fraction of HgSe in the liver of all animals are related to different capacities or strategies of detoxification of methylmercury in this organ.  相似文献   
3.
A systematic study of Hg2+ and CH3Hg+ (MeHg+) speciation using hyphenated techniques, was performed for high-performance liquid chromatography coupled to on-line UV irradiation and cold-vapour atomic fluorescence spectroscopy (HPLC-UV-CV-AFS). First, a comparative study of the behaviour of three mobile phase compositions (using tetrabutylammonium bromide (TBAB), L-cysteine and ammonium pyrrolidinedithiocarbamate (APDC)) is presented. The separation and detection system was optimised by considering factors that modify fluorescence signal and the separation such as, the addition of different percentages of an organic modifier (methanol (MeOH) and acetonitrile (ACN)) to the mobile phase, the type of reducing agent used (SnCl2 and NaBH4) and the potential memory effects of the material of which the injection system is made (stainless steel, PEEK). The mobile phase selected for its sensitivity was a mixture 80?:?20 MeOH?:?0.0015?mol?l–1 APDC and 0.01?mol?l–1 NH4CH3COO (pH 5.5). The detection and quantification limits were close to 1.5 and 5?µg?l?1 for both species (as Hg), respectively. Recoveries obtained using fortified water samples of distinct origin (soft mineral, tap, river, seawater, and wastewater), ranged from 90 to 115% for concentrations about 2 and 20 times over quantification limits. Good repeatability was obtained (about 5%) independently of the concentrations, with reproducibility values about 20% at low concentrations and 5–10% at higher concentrations. Our proposed method proved to be straightforward for use by environmental laboratories for routine Hg2+ and MeHg+ determinations in polluted water samples.  相似文献   
4.
《Analytical letters》2012,45(14):1175-1188
Abstract

The development of a new technique for the measurement of organometallic species is presented. It combines the resolution of high performance liquid chromatography with sensitive electrochemical detection used in a reductive mode. Past difficulties with this detection system have been overcome including the choice of a suitable working electrode and purification of the solvent.

The redox behavior of the organometals in the chromatographic solvent was studied by cyclic voltammetry in order to optimize the detector cell potential.

A separation of organomercurials and a multielement organometal mixture demonstrate the applicability of the system. Linear calibration curves can be obtained over a wide concentration range the detection limit for trimethyllead cation is about 0.1 ng.  相似文献   
5.
以甲基汞离子为模板,8-巯基喹啉为荧光单体,4-乙烯基吡啶为功能单体,乙二醇二甲基丙烯酸酯为交联剂,偶氮二异丁腈为引发剂,在二甲基亚砜溶剂中,以聚偏氟乙烯(PVDF)膜为支撑介质,65℃热引发聚合得到甲基汞离子荧光印迹膜。该荧光印迹膜对甲基汞离子表现出良好的选择性,最佳吸附pH值为7.0,检出限为3.5×10-7mol/L。将其作为吸附材料,应用于河水中甲基汞离子的分离和富集,结果表明,该传感器对甲基汞离子具有良好的选择性和特异性吸附,回收率达93%~104%。  相似文献   
6.
Uwe Harms 《Mikrochimica acta》1992,109(1-4):131-132
Determinations of methylmercury in biological tissues by gas chromatography with electron-capture detection are often disturbed by electron-capturing compounds simultaneously eluting with the organo-mercury compound.Identification and quantification of methylmercury is improved by interfacing the gas chromatograph to the gas cell of a flameless atomic absorption spectrometer. The construction of the transfer line used is described.  相似文献   
7.
本文报道了固相萃取预富集处理样品继以液相色谱分离测定不同形态痕量有机汞的方法.二乙基二硫代氨基甲酸钠(DDTC)作络合剂及甲醇作洗脱液的预富集系统能在线富集甲基汞(MeHg)、乙基汞(EtHg)和苯基汞(PhHg).用于测定加标海水中MeHg、EtHg和PhHg,回收率分别为96.9%、102.4%和98.0%;相对标准偏差分别为3.5%、5.0%和5.0%;检测下限分别为 1.0μg/L、1.2 μg/L和 1.2 μg/L.  相似文献   
8.
The usual presence of mercury(II) with monodi-, and tri-methyltin in water, sediments, and plants in estuarine environments suggests possible abiotic formation of methylmercury via methyl transfer from methyltin compounds. Kinetics studies of reactions between mercury(II) and methyltin compounds under pseudo-first-order conditions in seawater show that relative rate of methylmercury formation under the same conditions are: monomethyltin <trimethyltin> dimethyltin. This order is explainable mainly by the speciation and charge of methyltin compounds in seawater and by the existence of mercury(II) as a tetrachloro anion. A factorial experiment with the variables pH and salinity (seawater diluted with deionized water) showed that pH, but not salinity, is significant at the 95% confidence level; and that reaction rates increase as pH increases. These results suggest the possibility of abiotic methylation of mercury(II) in seawater. Additional experiments in seawater demonstrated an absence of methylation of mercury(II) (14 days) and mercury(0) (35 days) by methyl iodide.  相似文献   
9.
A simple procedure for the synthesis of an important standard, isotopically enriched methylmercury, which is not commercially available, has been established successfully. The isotopically enriched standard synthesized is utilized in conventional isotope dilution mass spectrometry (IDMS), as well as in speciated IDMS (SIDMS), for determination of the true concentration of methylmercury in environmental samples. The CH3201Hg+ standard has been synthesized from commercially available 201HgO and tetramethyltin. The synthesis time required is 1 h at 60°C. The product is highly pure, yielding more than 90% as 201Hg in CH3201Hg+. Hazardous dimethylmercury does not occur during this synthesis procedure. The product synthesized was analyzed using high‐performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (ICP‐MS) and ICP‐MS alone in order to determine its concentration, isotopic composition and purity. The stability of the product was also evaluated for over 6 months and found to be stable at 4°C in the dark. The isotopically enriched methylmercury synthesized can be used in SIDMS and IDMS analyses as a standard. Copyright © 2003 John Wiley & Sons, Ltd.  相似文献   
10.
Methyl-Hg is one of the most dangerous pollutants in the environment. It is highly toxic and accumulates through the food chain. Tuna fish especially tends to concentrate Hg in the form of methyl-Hg. Quality assurance is a well established routine in analytical laboratories to control the variability of analytical results and to maintain adequate stability, detection power and reproducibility. Capillary electrophoresis (CE) has shown in recent years powerful capabilities for the resolution and analysis of very complex samples. The high resolution and peak capacity characteristics of this technique could be used favourably in speciation studies of organo-Hg compounds. Since the time needed for separation is usually very short in this technique, it lends itself to routine analysis. The application of quality control approaches in the analysis of methyl-Hg in tuna freeze-dried materials using CE is reported.  相似文献   
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