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Determination of phthalate esters in liquor samples by vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction followed by GC–MS 下载免费PDF全文
Geng Leng Wenjin Chen Mingfang Zhang Fang Huang Qiming Cao 《Journal of separation science》2014,37(6):684-690
A novel method using vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction has been developed for the extraction of phthalate esters (PAEs) in Chinese liquor samples prior to analysis by GC–MS. In the proposed method, a high‐density extraction solvent (carbon tetrachloride) was dispersed into samples with the aid of a surfactant (Triton X‐100) and vortex agitation, resulting in a short extraction equilibrium (30 s). After centrifugation, a single microdrop of solvent was easily collected for GC–MS analysis. Key factors that affected the extraction efficiency were optimized. Under the optimum conditions, linearity was found in the range from 0.05 to 50 μg/L. Coefficients of determination varied from 0.9938 to 0.9971. LODs, based on an S/N of 3, ranged from 4.9 to 13 ng/L. Enrichment factors varied from 140 to 184. Reproducibility and recoveries were assessed by testing a series of three liquor samples that were spiked with different concentration levels. Finally, the proposed method was successfully applied to the determination of PAEs in 16 Chinese liquor samples. In this work, high‐density‐solvent vortex‐assisted surfactant‐enhanced‐emulsification liquid–liquid microextraction was applied for the first time for the extraction of PAEs in Chinese liquor samples and was proved to be simple, rapid, and sensitive. 相似文献
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The conversion efficiency of stimulated Raman scattering (SRS) in CH4 is studied by using a single longitudinal mode second-harmonic Nd:YAG laser (532 nm, linewidth 0.003 cm-1, pulse-width (FWHM) 6.5 ns).Due to the heat release from vibrationally excited particles, SRS processes often suffer from the thermal defocusing effect (TDE). In view of 6.5 ns laser pulse width is much shorter than the vibrational relaxation time of CH4 molecules, TDE can only affect the SRS processes afterwards. In the cases of low laser repetition, TDE will be not serious, because it will be removed by the thermal diffusion in Raman medium before the next pulse arrives. At the laser repetition rate 2 Hz, CH4 pressure 1.1 MPa and pump laser energy 95 m J, the quantum conversion efficiency of backward first-Stokes (BS1) has attained 73%. This represents the highest first-stokes conversion efficiency in CH4. Furthermore, due to the relaxation oscillation, the BS1pulses are narrowed to about 1.2 ns. As a result, the BS1 peak power turns out to be 2.7 times that of the pump. Its beam quality is also much better and is only slightly affected by TDE. This reason is that BS1 represents a wave-front-reversed replica of the pump beam, which can compensate the thermal distortions in Raman amplify process. Under the same conditions, but pump laser repetition rate as 10 Hz, the conversion efficiency of BS1 goes down to 36% due to TDE. From this study, we expect that a well-behaved 630 nm Raman laser may be designed by using a closed CH4/He circulating-cooling system, which may have some important applications. 相似文献
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Dean P Lim YL Valavanis A Kliese R Nikolić M Khanna SP Lachab M Indjin D Ikonić Z Harrison P Rakić AD Linfield EH Davies AG 《Optics letters》2011,36(13):2587-2589
We demonstrate terahertz (THz) frequency imaging using a single quantum cascade laser (QCL) device for both generation and sensing of THz radiation. Detection is achieved by utilizing the effect of self-mixing in the THz QCL, and, specifically, by monitoring perturbations to the voltage across the QCL, induced by light reflected from an external object back into the laser cavity. Self-mixing imaging offers high sensitivity, a potentially fast response, and a simple, compact optical design, and we show that it can be used to obtain high-resolution reflection images of exemplar structures. 相似文献
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Nga H. Nguyen Xuefei Leng Hao‐Jan Sun Virgil Percec 《Journal of polymer science. Part A, Polymer chemistry》2013,51(15):3110-3122
The efficient Cu(0) wire‐catalyzed single‐electron transfer‐living radical polymerization (SET‐LRP) of oligo(ethylene oxide) methyl ether methacrylate (OEOMA) in DMSO and binary mixtures of DMSO with H2O is reported. Addition of 10–80% H2O to DMSO resulted in an increase in the apparent rate constant of propagation ( ), corresponding to an increase in the polarity and extent of disproportionation. At higher H2O content, decreases, and in H2O is slightly lower than that in DMSO. This unexpected behavior was attributed to the physical inaccessibility of Cu(0) wire catalyst to the hydrophobic reactive centers of OEOMA and initiator which self‐assemble in H2O into micellar aggregates and vesicles. This hypothesis was confirmed by the faster polymerization in H2O than in DMSO during catalysis with Cu(0) nanoparticles generated by disproportionation of CuBr. SET‐LRP of OEOMA can be performed in protic and dipolar aprotic solvents in air by the addition of hydrazine hydrate. The polymerization exhibited no induction period and identical as in the degassed experiment, and led to polymers with narrow molecular weigh distribution. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 3110–3122 相似文献
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(μ3-S)FeCo2(CO)7(dppfe)的合成和晶体结构 总被引:1,自引:0,他引:1
通过简单取代反应,合成了一个新的混金属簇合物(μ3-S)FeCo2(CO)7(dppfe) (2) (dppfe=Ph2PC5H4FeC5H4PPh2).利用IR,1H NMR,MS 和 X-ray单晶衍射的方法对簇合物2进行了结构表征.簇合物2的晶体属于三斜晶系,空间群为Pī.晶胞参数: a=1.132 4(15) nm, b=1.3670(17) nm, c=1.5769(2) nm,α=114.646(2)°,β=100.340(2)°,γ=100.113(3)°, V=2.0953(5) nm3. 相似文献
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Summary An analytical method for the simultaneous determination of the pyrethroid metabolites cis and trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane carboxylic acid, cis 3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane carboxylic acid, 3-phenoxybenzoic acid and 4-fluoro-3-phenoxybenzoic acid in human urine samples is described. The urine is subjected to acid-induced hydrolysis followed by exhaustive solvent extraction, covering both conjugated and free acids, followed by a common derivatisation step yielding the corresponding methyl esters. Quantitation was by diastereomeric, capillary gas chromatography-mass spectrometry. It appears that 4-fluoro-3-phenoxybenzoic acid is a characteristic urinary marker for cyfluthrin exposure. The limits of determination are 0.5–1.0 g L–1 urine depending on the metabolites concerned. The applicability of the method was tested on urine samples from pest control operators exposed occupationally to cypermethrin and cyfluthrin. 相似文献