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991.
Zaijun Li Yinjun Fang Peipei Chen Zhongyun Wang Liping Wang Guoxiao Ren 《International journal of environmental analytical chemistry》2013,93(11):856-868
In the current paper we describe a novel sample preparation technique termed dispersive liquid-phase microextraction for the preconcentration and determination of 2,2,2-trichloro-1,1-bis(4-chlorophenyl)ethanol (dicofol) and its degradation products in water samples that includes 2-(2-chlorophenyl)-2-(4-chlorophenyl)-1,1-dichloroethene(2,4′-DDE), 1,1-dichloro-2,2-bis(4-chlorophenyl)ethane(4,4′-DDE) and 1,1,1-trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethane (2,4′-DDT) coupled with gas chromatography mass spectrometry (GC-MS), in which a new ionic liquid 1,3-diisooctylimidazolium hexafluorophosphate abbreviated as [D(i-C8)IM][PF6] was used as extraction solvent. For each one extraction, 1.00 mL of the methanol solution containing 40 µL of the ionic liquid was sprayed into 25.00 mL of water sample. In the meantime the ionic liquid was finely dispersed into the aqueous phase and analytes were rapidly migrated into the ionic liquid. After the solution was centrifuged for 2 min at 5000 rpm, the droplets of the ionic liquid are subsided in the bottom of the conical test tube (30.0 ± 0.2 µL). Moreover, the factors relevant to extraction efficiencies were investigated and optimised including the volume of the ionic liquid, disperser solvent, extraction time, sample pH and ionic strength. Under optimal conditions, the enrichment factors of the extraction were between 550 and 725 with an extraction efficiency ranging from 66% to 87% for each different analyte. Finally, 1.0 µL of the ionic liquid collected from above extraction was injected into the injector block of GC-MS instrument for analysis. The detection limit (S/N = 3), the relative standard deviations for 2.0 µg L?1 of the standard analyte (n = 5) and linearity in a calibration range were found to be 3–8 ng L?1, 1.0–2.7% and 10–3000 ng L?1, respectively. Good spiked recoveries over the range of 92.0–13.5% were obtained. The proposed method offers the advantages of simplicity of operation, rapidity, good extraction efficiency and enrichment factor; it has been successfully applied to determination of dicofol and its degradation products in environmental water samples. 相似文献
992.
Gabriel G.A. de Carvalho Mário A. Feres Jr José R. Ferreira Valerie H. Kennedy 《International journal of environmental analytical chemistry》2013,93(9):686-696
A simple and reliable method for Hg determination in fish samples has been developed. Lyophilised fish tissue samples were extracted in a 25% (w/v) tetramethylammonium hydroxide (TMAH) solution; the extracts were then analysed by FI-CVAFS. This method can be used to determine total and inorganic Hg, using the same FI manifold. For total Hg determination, a 0.1% (w/v) KMnO4 solution was added to the FI manifold at the sample zone, followed by the addition of a 0.5% (w/v) SnCl2 solution, whereas inorganic Hg was determined by adding a 0.1% (w/v) L-cysteine solution followed by a 1.0% (w/v) SnCl2 solution to the FI system. The organic fraction was determined as the difference between total and inorganic Hg. Sample preparation, reagent consumption and parameters that can influence the FI-CVAFS performance were also evaluated. The limit of detection for this method is 3.7 ng g?1 for total Hg and 4.3 ng g?1 for inorganic Hg. The relative standard deviation for a 1.0 µg L?1 CH3Hg standard solution (n = 20) was 1.1%, and 1.3% for a 1.0 µg L–1 Hg2+ standard solution (n = 20). Accuracy was assessed by the analysis of Certified Reference Material (dogfish: DORM-2, NRCC). Recoveries of 99.1% for total Hg and 93.9% inorganic Hg were obtained. Mercury losses were not observed when sample solutions were re-analysed after a seven day period of storage at 4°C. 相似文献
993.
Sofia Batista Emília Silva Sara Galhardo Paula Viana Maria José Cerejeira 《International journal of environmental analytical chemistry》2013,93(8-9):601-609
In two Portuguese agricultural areas, "Beira Litoral" and "Ribatejo e Oeste", several pesticides regularly applied in vineyards, maize, potato, tomato for industry, apple, pear and rice were detected in ground water. Atrazine was the most frequently detected, being found in 70% of the total of 79 sites selected in the year 2000, followed by its metabolites desethylatrazine and desisopropylatrazine with frequencies of detection, respectively, of 56% and 48% and by simazine (37%), alachlor (25%), metolachlor (24%) and metribuzin (15%). Other pesticides and metabolites i.e. 3,4-dichloroaniline, dimethoate, f and g -endosulfan, lindane, molinate and prometryn were also detected but at lower occurrences. Pesticides were detected mainly in ground water wells used for irrigation purposes, although in some locations they were also found in water wells used for human consumption. In this study, it was also observed a seasonal variation of pesticide residues in ground water of shallow and deep wells. 相似文献
994.
Effect of viscosity of a liquid membrane containing oleyl alcohol on the pertraction of butyric acid
Marek Blahušiak Ján Marták Fernando Miranda Štefan Schlosser José A. Teixeira 《Chemical Papers》2013,67(12):1560-1568
Solvent formulation is important in the optimization of the mass-transfer through supported liquid membranes (SLM) in pertraction and membrane extraction. Oleyl alcohol (OA) is frequently used as the solvent or diluent in the extraction of carboxylic acids. A disadvantage of OA is its relatively high viscosity of 28.32 mPa s at 25°C. This can be decreased by the application of a less viscous OA diluent, e.g. dodecane. The relationship between the ratio of the distribution coefficient of butyric acid (BA), D F, and the viscosity of OA-dodecane solvents, µ, as extraction and transport characteristics, and the overall mass-transfer coefficient, K p, through SLMs was analyzed. Dependence of the D F/µ ratio on the OA concentration showed a maximum at the OA concentration of 15 mass % to 30 mass %. The OA concentration dependence of K p for SLMs exhibited also a maximum at about 30 mass % and 20 mass % of OA at the BA concentration driving force of 0.12 kmol m?3 and 0.3 kmol m?3, respectively. Shifting of the maximum in K p dependences towards lower OA concentrations by increasing the BA concentration driving force is in agreement with the D F/µ ratio dependence. Using pure OA as the solvent or diluent is not preferable and a mixture of a low viscosity diluent with the OA concentration below 40 mass % should be used. The presented results show the potential of the D F/µ ratio in the screening and formulation of solvents in extraction and SLM optimization. 相似文献
995.
996.
997.
Vera Homem Raquel Sousa José Luís Moreira Lúcia Santos 《International journal of environmental analytical chemistry》2013,93(2):166-189
A new method for the simultaneous determination of 12 volatile organic compounds (trans-1,2-dichloroethene, 1,1,1-trichloroethane, benzene, 1,2-dichloroethane, trichloroethene, toluene, 1,1,2-trichloroethane, tetrachloroethene, ethylbenzene, m-, p-, o-xylene) in water samples by headspace solid phase microextraction (HS–SPME)–gas chromatography mass spectrometry (GC–MS) was described, using a 100?µm PDMS (polydimethylsiloxane) coated fibre. The response surface methodology was used to optimise the effect of the extraction time and temperature, as well as the influence of the salt addition in the extraction process. Optimal conditions were extraction time and temperature of 30?min and ?20°C, respectively, and NaCl concentration of 4?mol?L?1. The detection limits were in the range of 1.1?×?10?3–2.3?µg?L?1 for the 12 volatile organic compounds (VOCs). Global uncertainties were in the range of 4–68%, when concentrations decrease from 250?µg?L?1 down to the limits of quantification. The method proved adequate to detect VOCs in six river samples. 相似文献
998.
José L. Arias Pankaj Sharma Armando Cabrera Fernando Beristain Rafael Sampere Cesar Arizmendi 《Transition Metal Chemistry》2013,38(7):787-792
In the cobalt-catalysed hydroformylation of 3,4-dihydro[2H]pyran, the influence of different reaction parameters such as time, pressure, triphenylphosphine addition, catalyst and substrate concentration has been investigated. 2-formyl-tetrahydropyran, tetrahydropyran and a hydroalkylcarbonylation product were the main reaction products. The selectivity towards 2-formyl-tetrahydropyran formation is favoured at constant catalyst and substrate concentration. The coordination of the pyran’s oxygen to the cobalt atom seems to be an important intermediate for the formation of 2-formyl-tetrahydropyran. Different substrate or catalyst concentrations promote the formation of other reduced products. The addition of triphenylphosphine to the catalyst leads to a less active species, which decreases the yield and promotes the hydroalkylcarbonylation reaction. 相似文献
999.
The mechanism of α-acetyl-γ-butyrolactone (ABL) synthesis from γ-butyrolactone (GBL) and ethyl acetate (EtOAc) was explored by detecting the material changes involved and the enthalpies of formation of the synthons, products, and possible intermediates were calculated using the density functional theory. GBL forms a carbanion of γ-butyrolactone by losing an α-H under strongly alkaline conditions. ABL is then obtained via two reaction mechanisms. One of the reaction mechanisms involves direct reaction of the carbanion of GBL with EtOAc to produce ABL. The other involves the formation of a carbanion of α-(2-hydroxy-tetrahydrofuran-2-yl)-γ-butyrolactone through the reaction of two molecules of GBL, and the subsequent combination of this anion with EtOAc to produce ABL. ABL is thus formed through the above two kinds of competitive ester condensation reactions. It is unnecessary to take into account synthons’ local thickness, and their self-condensation under these conditions. Both reactions of the carbanion of GBL with EtOAc and GBL are exothermic, so the control of their reaction rate is the key to their security. Considering the reasons above, this work applied synthon as the solvent, and avoided environmental pollution by alkylbenzene; also, accidents such as red material and fire were avoided by specific surface area of sodium metal control. Effective isolation of the organic and aqueous phases was performed using the salting out method. Thus, an environmentally friendly, safe, simple, and efficient new method for the synthesis of ABL with the yield higher than 90 % has been established. 相似文献
1000.
Amelia P. Rauter José A. Figueiredo Isabel Ismael Maria S. Pais António G. Gonzalez Jesus Diaz 《Journal of carbohydrate chemistry》2013,32(2):259-272
Abstract Synthesis of stereoisomeric α-methylene-γ-lactones in furanose-and furanuronoamide derivatives was easily accomplished by Reformatsky Reaction with ethyl bromcmethylacrylic ester and zinc. Pyridinium chlorochromate/3Å molecular sieve powder showed to be an excellent reagent for the oxidation of secondary hydroxyl groups of a furanose system and of α-hydroxy amides. 相似文献