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131.
研究了由4,4'-癸二酰-双-(1-苯基-3-甲基-5-吡唑啉酮)(DBPMP,简作H2A),氧化三辛基膦(TOPO),吡啶(Py)组成的三元体系从硝酸溶液中对铀的协同萃取,斜率法确定萃合物组成为UO2A.TOPO.Py,制取了固体协萃配合物,并用元素分析、IR及HNMR等进行了表征。 相似文献
132.
Solid Phase Extraction and Flame Atomic Absorption Spectrometric Determination of Trace Amounts of Zinc and Cobalt Ions in Water Samples 总被引:1,自引:0,他引:1
A simple and rapid method for the preconcentration of Co2+ and Zn2+ as their 2-guanidino-benzimidazole chelates is proposed using an octadecyl silica cartridge. The retained analytes were recovered with a mixture of 5mL of 0.01M HNO3 and 5mL of methanol. The metal ions in the effluent were determined by flame atomic absorption spectrometry. The effect of different parameters, such as sample matrix, amount of ligand, type of eluent for elution of ions from cartridge, flow rates of sample solution and eluent, breakthrough volume, and limit of detection, were evaluated. The effects of various cationic and anionic interferences on the percent recovery of Co2+ and Zn2+ were also studied. Quantitative extraction efficiencies were obtained by elution of the cartridge with a minimal amount of solvent. Hence, with a typical preconcentration factor of 50, the limits of detections of the proposed method are 0.26 and 1.62ngmL–1 for Zn2+ and Co2+, respectively. The method was applied to the determination of zinc and cobalt ions in different water samples. 相似文献
133.
Summary In this study, a rapid and efficient semi-micro extraction procedure is presented for the extraction of some higher n-alkanes
from water and soil samples. In the case of water samples n-hexane was used as the organic phase in a phase volume ratio (volume
of aqueous phase/volume of organic phase) higher than 285, while in the case of soil samples, extraction with n-hexane was
carried out in the presence of an excess of 2 M NaCl solution. The extraction rate from soil samples is very high and is better
than Soxhlet extraction, comparable with supercritical fluid extraction. High preconcentration factor in water samples allows
the limits of detection to be in the ng.mL−1 level with the use of gas chromatographic analysis. Flame ionization detector was used for monitoring the analytes. The obtained
recoveries of all studied compounds from both water and soil samples are higher than 90%. This method was successfully used
to determine some n-alkanes in municipal wastewater and contaminated soil. 相似文献
134.
The performance of ultrasonic and Soxhlet extraction using hexane, dichloromethane, ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) for the analysis of seventeen insecticides in sediments was evaluated. The contents of the extracts differed severely. The extracts obtained with ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) were dark yellow to green, whereas the extracts obtained with dichloromethane and hexane were light yellow and clear respectively. This is due to higher solubility of matrix compounds in ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v). High loads of coextracted matrix compounds lead to matrix effects in the evaporation step of GC–MS measurements. This is known as matrix induced response enhancement effect. Matrix effects and recoveries were checked by analysis of spiked sediments. The suitable choice of extraction method in connection with an appropriate solvent separates the analytes from matrix compounds. Matrix effects are reduced and recoveries of spiked samples are improved.Revised: 6 January and 2 May 2005 相似文献
135.
Jun Ping Xiao Qing Xiang Zhou Hua Hua Bai Department of Chemistry University of Science Technology Beijing Beijing China School of Chemistry Environmental Sciences Henan Normal University Henan Key Laboratory for Environmental pollution Control Xinxiang China 《中国化学快报》2007,18(6):714-717
A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1-100 ng/mL (R2 = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment. 相似文献
136.
A fully automated flow-through microcolumn fractionation system with on-line post-extraction derivatization is proposed for monitoring of orthophosphate in solid samples of environmental relevance. The system integrates dynamic sequential extraction using 1.0 mol l−1 NH4Cl, 0.1 mol l−1 NaOH and 0.5 mol l−1 HCl as extractants according to the Hieltjes-Lijklema (HL) scheme for fractionation of phosphorus associated with different geological phases, and on-line processing of the extracts via the Molybdenum Blue (MB) reaction by exploiting multisyringe flow injection as the interface between the solid containing microcolumn and the flow-through detector. The proposed flow assembly, capitalizing on the features of the multicommutation concept, implies several advantages as compared to fractionation analysis in the batch mode in terms of saving of extractants and MB reagents, shortening of the operational times from days to hours, highly temporal resolution of the leaching process and the capability for immediate decision for stopping or proceeding with the ongoing extraction. Very importantly, accurate determination of the various orthophosphate pools is ensured by minimization of the hydrolysis of extracted organic phosphorus and condensed inorganic phosphates within the time frame of the assay. The potential of the novel system for accommodation of the harmonized protocol from the Standards, Measurement and Testing (SMT) Program of the Commission of the European Communities for inorganic phosphorus fractionation was also addressed. Under the optimized conditions, the lowest detectable concentration at the 3σ level was ≤0.02 mg P l−1 for both the HL and SMT schemes regardless of the extracting media. The repeatability of the MB assay was better than 2.5% and the dynamic linear range extended up to 7.0 mg P l−1 in NH4Cl and NaOH media and 15 mg P l−1 whenever HCl is utilized as extractant for both the HL and SMT protocols. 相似文献
137.
Rozhon W Petutschnig E Wrzaczek M Jonak C 《Analytical and bioanalytical chemistry》2005,382(7):1620-1627
Salicylic acid (SA) is an important signaling compound in plants and is involved in various defense responses. Here we report a new method for quantification of free and total soluble SA in Arabidopsis thaliana with 5-fluorosalicylic acid (5-FSA) as internal standard. The SA was isolated from leaf extracts by solid-phase extraction with phenyl-phase cartridges and selectively eluted as the cationic iron(III)-complex. Recoveries of SA and 5-FSA were equal and exceeded 90%. Free SA was subsequently released from the iron(III)-complex by addition of 2,2-bipyridyl and high-performance anion-exchange chromatography was performed on an NH2 column. The SA appeared as last peak with a retention time of 15 min, baseline-separated from other substances. On-line detection was performed fluorimetrically for both SA and 5-FSA at an excitation wavelength of 300 nm and an emission wavelength of 410 nm, because both substances give similar fluorescence spectra. The detection limit for SA was 5 ng g–1 FW for a sample size of 100 mg. Thus the main advantages of the method are highly selective sample preparation, increased sensitivity, reduced analysis time compared with reversed-phase HPLC, and use of a novel internal standard detectable under the same conditions as SA. The techniques described are applicable to other plant materials. 相似文献
138.
Quantitative analysis of docetaxel in human plasma using liquid chromatography coupled with tandem mass spectrometry 总被引:2,自引:0,他引:2
Kuppens IE van Maanen MJ Rosing H Schellens JH Beijnen JH 《Biomedical chromatography : BMC》2005,19(5):355-361
An assay for the quantitative determination of docetaxel in human plasma is described. Docetaxel was extracted from the matrix using liquid-liquid extraction with ter-butylmethylether, followed by high-performance liquid chromatographic analysis using an alkaline eluent. Paclitaxel was used as internal standard. Positive ionization electrospray tandem mass spectrometry was performed for selective and sensitive detection. The method was validated according to the FDA guidelines on bioanalytical method validation. The validated range for docetaxel was from 0.25--1000 ng/mL using 200 microL plasma aliquots. The method requires only a limited volume (200 microL) of human plasma and the method can be applied in studies requiring a low lower limit of quantitation of 0.25 ng/mL. The assay was applied successfully in several clinical and pharmacological studies with docetaxel. 相似文献
139.
A solution-phase synthesis of bicyclic prolines containing four points of diversity has been developed by a two-step synthesis involving 1,3-dipolar cycloaddition of perfluoroalkylsulfonyl-protected hydroxybenzaldehydes followed by Pd-catalyzed Suzuki coupling reaction of fluorous sulfonates with boronic acids. Both reactions are conducted under microwave irradiation and reaction mixtures are purified by solid-phase extractions without performing chromatography. 相似文献
140.
A new method for the determination of trace cadmium in water samples by flame atomic absorption spectrometry (FAAS) after
cloud point extraction (CPE) is proposed. The method is based on the complexation of Cd with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone
(PMBP) in the presence of non-ionic micelles of Triton X-100. The effect of experimental conditions such as pH, concentration
of chelating agent and surfactant, equilibration temperature and time on cloud point extraction was studied. Under the optimum
conditions, the detection limits are 0.64 ng mL±1 with relative standard deviations (RSDs) of 2.1% (n = 10). The proposed method was applied to the determination of trace
cadmium in water samples with satisfactory results. 相似文献