Headspace solid-phase microextraction with novel sol-gel permethylated-beta-cyclodextrin/hydroxyl-termination silicone oil fiber for determination of polybrominated diphenyl ethers by gas chromatography-mass spectrometry in soil

A simple, sensitive, and accurate method for determination of polybrominated diphenyl ethers (PBDEs) in soil has been developed based on headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS). Permethylated-beta-cyclodextrin/hydroxyl-termination silicone oil (PM-beta-CD/OH-TSO) fiber was first prepared by sol-gel technology and employed in SPME procedure. By exploiting the superiorities of sot-gel coating technique and the advantages of the high hydrophobic doughnut-shaped cavity of PM-beta-CD, the novel fiber showed desirable operational stability and extraction ability. After optimization on extraction conditions like water addition, extraction temperature, extraction time, salts effect, and solvents addition, the method was validated in soil samples, achieving good linearity (r>0.999), precision (R.S.D. < 10%), accuracy (recovery>78%), and detection limits (S/N =3) raging from 13.0 to 78.3 pg/g. (c) 2007 Published by Elsevier B.V.

Analysis of estrogens in environmental waters using polymer monolith in-polyether ether ketone tube solid-phase microextraction combined with high-performance liquid chromatography

A simple, rapid and sensitive on-line method for simultaneous determination of four endocrine disruptors (17 beta-estradiol, estriol, bisphenol A and 17 alpha-ethinylestradiol) in environmental waters was developed by coupling in-tube solid-phase microextraction (SPME) to high-performance liquid chromatography (HPLC) with fluorescence detection (FLD). A poly(acrylamide-vinylpyridine-NAP-methylene bisacrylamide) monolith, synthesized inside a polyether ether ketone (PEEK) tube, was selected as the extraction medium. To achieve optimum extraction performance, several parameters were investigated, including extraction flow-rate, extraction time, and pH value, inorganic salt and organic solvent content of the sample matrix. By simply filtered with nylon membrane filter and adjusting the pH of samples to 6.0 with phosphoric acid, the sample solution then could be directly injected into the device for extraction. Low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method were achieved in the range of 0.006-0.10 ng/mL and 0.02-0.35 ng/mL from spiked lake waters, respectively. The calibration curves of four endocrine disruptors showed good linearity ranging from quantification limits to 50 ng/mL with a linear coefficient R-2 value above 0.9913. Good method reproducibility was also found by intra- and inter-day precisions, yielding the RSDs less than 12 and 9.8%, respectively. Finally, the proposed method was successfully applied to the determination of these compounds in several environmental waters. (c) 2006 Elsevier B.V. All rights reserved.

A solid-phase microextraction fiber coated with diglycidyloxycalix[4]arene yields very high extraction selectivity and sensitivity during the analysis of chlorobenzenes in soil

A novel fiber coated with novel sol-gel (5,11,17,23-tetra-tert-butyl-25,27-dihydroxy-26,28-diglycidyloxycalix[4]arene/hydroxy-terminated silicone oil; diglycidyloxy-C[4]/OH-TSO) was prepared for use with headspace solid-phase microextraction (HS-SPME) combined with gas chromatography (GC) and electron capture detection (ECD), which was applied in order to determine nine chlorobenzenes in soil matrices. Due to the improved fiber preparation, which increases the percentage of calixarene in the coating, the new calixarene fiber exhibits very high extraction selectivity and sensitivity to chlorine-substituted compounds. Various parameters affecting the extraction efficiency were optimized in order to maximize the sensitivity during the chlorobenzene analysis. Interferences from different soil matrices with different characteristics were investigated, and the amount extracted was strongly influenced by the matrix. Therefore, a standard addition protocol was performed on the real soil samples. The linear ranges of detection for the chlorobenzenes tested covered three orders of magnitude, and correlation coefficients > 0.9976 and relative standard deviations (RSD) < 8% were observed. The detection limits were found at sub-ng/g of soil levels, which were about an order of magnitude lower than those given by the commercial poly(dimethylsiloxane) (PDMS) coating for most of the compounds. The recoveries ranged from 64 to 109.6% for each analyte in the real kaleyard soil matrix when different concentration levels were determined over the linear range, which confirmed the reliability and feasibility of the HS-SPME/GC-ECD approach using the fiber coated with diglycidyloxy-C[4]/OH-TSO for the ultratrace analysis of chlorobenzenes in complex matrices.

Determination of odorous compounds in water by headspace solid-phase microextraction-gas chromatography-mass spectrometry

Three major odorous compounds are 2-methylisoborneol ( 2-MIB), geosmin and beta-cyclocitral, which in water were determined by coupling headspace solid-phase microextraction ( HS-SPME) with gas chromatography-mass spectrometry (GC-MS). The operating conditions of HS-SPME, such as fibre type, salt concentration, water temperature, stirring, absorption time and desorption time were studied and discussed.The highest absorption of the odorous compounds were obtained under the following operating conditions as the addition of 30% ( m/V) NaCl, stirring at 60 degrees C for 40 min, using 65 mu m polydimethyl siloxane/divinylbenzene coated fibre. After the odorous compounds had been absorbed in the fibre under the optimal conditions of HSSPME, they were desorbed at 250 degrees C and determined by GC-MS. The limits of detection for geosmin, beta-cyclocitral and 2-MIB in water were 1. 0, 1. 3, 1. 7 ng/L, and the relative standard deviations for them were 4. 9%, 8. 4%, 6. 2%,respectively. There were good linear correlation (the calibration coefficients were all above 0. 997) for the three odorous compounds in the range of 5 similar to 1000 ng/ L. Therefore, trace levels of the odorous compounds at ng/L in water could be quantified by the simple method with satisfactory result.

Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography-mass selective detection

A macro matrix solid-phase dispersion (MSPD) method was developed to extract 266 pesticides from apple juice samples prior to gas chromatography-mass selective detection (GC-MSD) determination. A 10 g samples was mixed with 20 g diatomaceous earth. The mixture was transferred into a glass column. Pesticide residues were leached with a 160 mL hexane-dichloromethane (1:1) at 5 mL/min. Two hundred and sixty-six pesticides were divided into three groups and detected by GC-MSD under selective ion monitoring. The proposed method takes advantage of both liquid-liquid extraction and conventional MSPD methods. Application was illustrated by the analysis of 236 apple juice samples produced in Shaanxi province China mainland this year. (C) 2004 Elsevier B.V. All rights reserved.

Determination of phthalate acid esters plasticizers in plastic by ultrasonic solvent extraction combined with solid-phase microextraction using calix[4]arene fiber

Ultrasonic solvent extraction combined with solid-phase microextraction (SPME) with calix[4]arene/hydroxy-terminated silicone (C[4]/OHTSO) oil coated fiber was used to extract phthalate acid esters (PAEs) plasticizers in plastic, such as blood bags, transfusion tubing, food packaging bag, and mineral water bottle for analysis by gas chromatography (GC). Both extraction parameters (i.e. extraction time, extraction temperature, ionic strength) and conditions of the thermal desorption in a GC injector were optimized by analysis of eight phthalates. The fiber shows wonderful sensitivity and selectivity to the tested compounds. Owing to its high thermal stability (380 degreesC), the carryover effect that often encountered when using conventional fibers can be reduced by appropriately enhancing the injector temperature. The method showed linear response over two to four orders of magnitude with correlation coefficients (r) better than 0.996, and limits of detection (LOD) ranged between 0.006 and 0.084 mug l(-1). The relative standard deviation values obtained were less than or equal to 10%. bis-2-Ethylhexyl phthalate (DEHP) was the sole analyte detected in these plastics and recoveries were in the ranges 95.5-101.4% in all the samples. (C) 2004 Elsevier B.V. All rights reserved.

Determination of trace level microcystins in water using solid-phase extraction and high performance liquid chromatography

This paper presents a method for trace level analysis of microcystins in water using solid-phase extraction and high performance liquid chromatography. The optimized condition enabled the determination of common microcystins at levels as low as 0.02 similar to 0.05 mug/L, and the liner range is from 0.1 mug/L to 50 mug/L. The method has been applied to the analysis of field sample from Dianchi lake.

Analysis of organchlorine compounds in water by solid phase microextraction and gas chromatography

In this work, both,solid phase microextraction (SPME) and solid phase extraction(SPE) were used to enrich organochlorine compounds in water samples and analyzed by gas chromatography with electron capture detector. The operating conditions of SPME have been studied and different kinds of solid phase were compared. Linear alkybenzene sulfonate(LAS) was added to the samples to investigate its effect on the analysis. The results indicated that polyacrylate was better than other commercial solid phases in extraction of moderated polar organic compounds and the sensitivity of SPME was higher than SPE. LAS affect much in liquid-liquid extraction and headspace SPME; but it has little effect on SPE and direct-SPME method. The applications showed that SPME was a fast and effective method in sample preparation.

Sol-gel method for the preparation of solid-phase microextraction fibers

A novel sol-gel method is applied for the preparation of solid-phase microextraction (SPME) fibers. Scanning electron microscopy experiments suggested a porous structure for the poly(dimethylsiloxane) (PDMS) coating. SPME-GC analysis provided evidence that the sol-gel fibers have some advantages, such as high thermal stability, efficient extraction rates, high velocities of mass transfer, and spacious range of application.

Structural, electrical, and optical properties of InAsxSb1-x epitaxial films grown by liquid-phase epitaxy

The InAsxSb1-x films were grown on (100) GaSb substrates by liquid-phase epitaxy, and their structural, electrical, and optical properties were investigated. The high-resolution x-ray diffraction results reveal that the single crystalline InAsxSb1-x films with a midrange composition are epitaxially grown on the GaSb substrates. Temperature dependence of the Hall mobility was theoretically modeled by considering several predominant scattering mechanisms. The results indicate that ionized impurity and dislocation scatterings dominate at low temperatures, while polar optical phonon scattering is important at room temperature (RT). Furthermore, the InAsxSb1-x films with the higher As composition exhibit the better crystalline quality and the higher mobility. The InAs0.35Sb0.65 film exhibits a Hall mobility of 4.62x10(4) cm(2) V-1 s(-1). The cutoff wavelength of photoresponse is extended to about 12 mu m with a maximum responsivity of 0.21 V/W at RT, showing great potential for RT long-wavelength infrared detection. (C) 2008 American Institute of Physics. [DOI: 10.1063/1.2989116]

Microstructure and Optical Properties of Nonpolar m-Plane GaN Films Grown on m-Plane Sapphire by Hydride Vapor Phase Epitaxy

Thick nonpolar (10 (1) over bar0) GaN layers were grown on m-plane sapphire substrates by hydride vapor phase epitaxy (HVPE) using magnetron sputtered ZnO buffers, while semipolar (10 (1) over bar(3) over bar) GaN layers were obtained by the conventional two-step growth method using the same substrate. The in-plane anisotropic structural characteristics and stress distribution of the epilayers were revealed by high. resolution X-ray diffraction and polarized Raman scattering measurements. Atomic force microscopy (AFM) images revealed that the striated surface morphologies correlated with the basal plane stacking faults for both (10 (1) over bar0) and (10 (1) over bar(3) over bar) GaN films. The m-plane GaN surface showed many triangular-shaped pits aligning uniformly with the tips pointing to the c-axis after etching in boiled KOH, whereas the oblique hillocks appeared on the semipolar epilayers. In addition, the dominant emission at 3.42eV in m-plane GaN films displayed a red shift with respect to that in semipolar epilayers, maybe owing to the different strain states present in the two epitaxial layers. [DOI: 10.1143/JJAP.47.3346]

Growth of (10(1)over-bar(3)over-bar) semipolar GaN on m-plane sapphire by hydride vapor phase epitaxy

The crystalline, surface, and optical properties of the (10 (1) over bar(3) over bar) semipolar GaN directly grown on m-plane sapphire substrates by hydride vapor phase epitaxy (HVPE) were investigated. It was found that the increase of V/III ratio led to high quality (10 (1) over bar(3) over bar) oriented GaN epilayers with a morphology that may have been produced by step-flow growth and with minor evidence of anisotropic crystalline structure. After etching in the mixed acids, the inclined pyramids dominated the GaN surface with a density of 2 X 10(5) cm(-2), revealing the N-polarity characteristic. In the low-temperature PL spectra, weak BSF-related emission at 3.44eV could be observed as a shoulder of donor-bound exciton lines for the epilayer at high V/III ratio, which was indicative of obvious reduction of BSFs density. In comparison with other defect related emissions, a different quenching behavior was found for the 3.29 eV emission, characterized by the temperature-dependent PL measurement. (C) 2009 Elsevier B.V. All rights reserved.

Strain status in ZnO film on sapphire substrate with a GaN buffer layer grown by metal-source vapor phase epitaxy

ZnO film of 8 mu m thickness was grown on a sapphire (0 0 1) substrate with a GaN buffer layer by a novel growth technique called metal-source vapor phase epitaxy (MVPE). The surface of ZnO film measured by scanning electron microscope (SEM) is smooth and shows many regular hexagonal features. The full width at half maximum (FWHM) of ZnO(0 0 2) and (1 0 2) omega-scan rocking curves are 119 and 202 arcsec, corresponding a high crystal quality. The status of the strain in ZnO thick film was particularly analyzed by X-ray diffraction (XRD) omega-20 scanning. The results show that the strain in ZnO film is compressive, which is also supported by Raman scattering spectroscopy. The compressive strain can solve the cracking problem in the quick growth of ZnO thick film. (c) 2008 Elsevier Ltd. All rights reserved.

Liquid phase epitaxy of Al0.3Ga0.7As islands

Self-organized Al0.3Ga0.7As islands generated on the (100) facet are achieved by liquid phase epitaxy. Three particularly designed experimental conditions-partial oxidation, deficient solute and air quenching-result in defect-free nucleation. Micron-sized frustums and pyramids are observed by a scanning electron microscope. The sharp end of the tip has a radius of curvature less than 50 nm. It is proposed that such Al0.3Ga0.7As islands may be potentially serviceable in microscale and nanoscale fabrication and related spheres. (C) 2004 Elsevier B.V. All rights reserved.