High-speed gas chromatography-multiplex coherent Raman analysis of BTEX

Gas chromatography-multiplex coherent Raman (GC-MCR) is a new tandem technique that can be used for the high-speed analysis of volatile mixtures. BTEX serves as a useful and challenging test sample because of the similarity in boiling point and spectroscopic properties of its constituents. The ability to spectroscopically resolve isomers (e.g., m-xylene and p-xylene) allows GC-MCR to sacrifice chromatographic resolution for speed. The result is the analysis of BTEX in less than 5 min, which is relatively fast compared with other tandem GC techniques.     

An analysis of synergistic and antagonistic behavior during BTEX removal in batch system using response surface methodology

The removal of benzene, toluene, ethylbenzene and xylene (BTEX) as quaternary mixtures were studied in batch systems using a well-defined mixed microbial culture. The synergistic and antagonistic effects of total BTEX removal (BTEXT-RE) due to the presence of mixed substrate was evaluated through experiments designed by response surface methodology (RSM). The low and high concentrations of individual BTEX were 15 and 75 mg l(-1), respectively. The results showed that, increasing the concentration of xylene increased the cumulative BTEX removal (BTEXT-RE), however the reverse occurred when benzene concentrations were increased from low to high levels. A mixed response of increasing and decreasing trend in the BTEXT-RE value was observed when either of toluene or ethylbenzene concentration was increased. When the concentrations of individual BTEX compounds were 30 mg l(-1), the BTEXT-RE was about 58%. Complete BTEXT-RE was achieved at optimal BTEX concentrations of 48.1, 45.6, 49.3 and 56.6 mg l(-1). The RSM approach was found efficient in explaining the main, squared and interaction effects among individual BTEX concentrations on the BTEXT-RE in a more statistically meaningful way.     

UV vapor generation for determination of selenium by heated quartz tube atomic absorption spectrometry

A new vapor generation technique utilizing UV irradiation coupled with atomic absorption for the determination of selenium in aqueous solutions is described. In the presence of low molecular weight organic acid solutions, inorganic selenium(IV) is converted by UV irradiation to volatile selenium species, which are then rapidly transported to a heated quartz tube atomizer for detection by atomic absorption spectrometry. Optimum conditions for photochemical vapor generation and interferences from concomitant elements were investigated. Identification of the volatile products using cryotrapping GC/MS analysis revealed that inorganic selenium(IV) is converted to volatile selenium hydride, selenium carbonyl, dimethyl selenide, and diethyl selenide in the presence of formic, acetic, propionic, and malonic acids, respectively. In acetic acid solution, the efficiency of generation was estimated to be 50 +/- 10%. No interference from Ni(2+) and Co(2+) at concentrations of 500 and 100 mg L(-)(1), respectively, was evident. A detection limit of 2.5 microg L(-)(1) and a relative sensitivity of 1.2 microg L(-)(1) (1% absorption) with a precision of 1.2% (RSD, n = 11) at 50 microg L(-)(1) were obtained.     

Simultaneous determination of trace cadmium and arsenic in biological samples by hydride generation-double channel atomic fluorescence spectrometry

Hydride generation atomic fluorescence spectrometry (HG-AFS) has been used for determination of hydride-forming elements because of its high sensitivity, simplicity, and low costs, but most of such work has been concentrated on single element analysis, and reports dealing with multielement determination by HG-nondispersive (ND)AFS are rare. In this work, a sensitive HG-NDAFS method was developed for simultaneous determination of trace cadmium and arsenic in biological materials. The conditions for the generation of volatile cadmium and arsenic species from the reaction with KBH4 in aqueous solution were investigated using a double-channel AFS integrated with an intermittent flow reactor. Like thiourea and Co(II), ascorbic acid was found to significantly enhance the generation efficiency of volatile Cd and As species. The interferences of coexisting ions were evaluated. Under optimal conditions, the detection limits for Cd and As were determined to be 10 and 150 ng L(-1), respectively. The precision for 11 replicate determinations at the 1 microg L(-1) Cd level and the 10 microg L(-1) As level were 3.5 and 2.7% (RSD), respectively. The recoveries of spike analytes in the biological samples studied ranged from 94 to 109%. The proposed method was successfully applied to the simultaneous determination of Cd and As in a variety of biological samples.     

Electrothermal atomic absorption spectrometric determination of gold by vapor formation and in situ trapping in graphite tubes

Gold was determined in ore samples following generation, separation, collection on a graphite cuvette inner wall, and atomization of its volatile species formed by combining an acidified sample solution with an aqueous sodium tetrahydroborate solution at room temperature. A detection limit of 2.6 microg L(-1) (3sigma) was obtained with a 5.0 mL sample volume. Precision of replicate measurements was typically 10% RSD. The overall efficiency of the volatile species generation, transport, and trapping process was 0.4%. Atomization of gold from Pd, Ir, Cu, Ag, and W coated graphite cuvettes, following by trapping of the gaseous volatile gold species on these surfaces, has been investigated. Pd coating was found to decrease the sensitivity. Five microg of Ir, 20 microg of Cu, 20 microg of Ag, and 5 microg of W were chosen as optimum masses. W treatment was the best one for sensitivity enhancement, having an improvement factor of 2.4. Silanization of glass surfaces significantly decreased memory effects; improved peak shapes were thus obtained for flow injection vapor generation atomic absorption spectrometry (FI-VGAAS). The method described in this study was used for the determination of gold in an ore reference material, Gold Ore (MA-1b), Canadian Reference Materials Program.     

Evaluation of persulfate oxidative wet scrubber for removing BTEX gases

Soil vapor extraction (SVE) coupled with air sparging of groundwater is a method commonly used to remediate soil and groundwater contaminated with volatile organic petroleum contaminants such as gasoline. These hazardous contaminants are mainly attributable to the compounds-benzene, toluene, ethylbenzene, and xylenes (known collectively as BTEX). Exhaust gas from SVE may contain BTEX, and therefore must be treated before being discharged. This study evaluated the use of iron-activated persulfate chemical oxidation in conjunction with a wet scrubbing system, i.e., a persulfate oxidative scrubber (POS) system, to destroy BTEX gases. The persulfate anions can be activated by citric acid (CA) chelated Fe(2+) to generate sulfate radicals (SO(4)(*-), E degrees =2.4V), which may rapidly degrade BTEX in the aqueous phase and result in continuous destruction of the BTEX gases. The results show that persulfate activation occurred as a result of continuous addition of the citric acid chelated Fe(2+) activator, which readily oxidized the dissolved BTEX. Based on initial results from the aqueous phase, a suitable Fe(2+)/CA molar ratio of 5/3 was determined and used to initiate activation in the subsequent POS system tests. In the POS system, using persulfate as a scrubber solution and with activation by injecting Fe(2+)/CA activators under two testing conditions, varying iron concentrations and pumping rates, resulted in an approximate 50% removal of BTEX gases. During the course of the tests which in corporate activation, a complete destruction of BTEX was achieved in the aqueous phase. It is noted that no removal of BTEX occurred in the control tests which did not include activation. The results of this study would serve as a reference for future studies into the practical chemical oxidation of waste gas streams.     

Use of a solution cathode glow discharge for cold vapor generation of mercury with determination by ICP-atomic emission spectrometry

A novel vapor-generation technique is described for mercury determination in aqueous solutions. Without need for a chemical reducing agent, dissolved mercury species are converted to volatile Hg vapor in a solution cathode glow discharge. The generated Hg vapor is then transported to an inductively coupled plasma for determination by atomic emission spectrometry. Mercury vapor is readily generated from a background electrolyte containing 0.1 M HNO 3. Vapor generation efficiency was found to be higher by a factor of 2-3 in the presence of low molecular weight organic acids (formic or acetic acids) or alcohols (ethanol). Optimal conditions for discharge-induced vapor generation and reduced interference from concomitant inorganic ions were also identified. However, the presence of chloride ion reduces the efficiency of Hg-vapor generation. In the continuous sample introduction mode, the detection limit was found to be 0.7 microg L (-1), and repeatability was 1.2% RSD ( n = 11) for a 20 microg L (-1) standard. In comparison with other vapor generation methods, it offers several advantages: First, it is applicable to both inorganic and organic Hg determination; organic mercury (thiomersal) can be directly transformed into volatile Hg species without the need for prior oxidation. Second, the vapor-generation efficiency is high; the efficiency (with formic acid as a promoter) is superior to that of conventional SnCl 2-HCl reduction. Third, the vapor generation is extremely rapid and therefore is easy to couple with flow injection. The method is sensitive and simple in operation, requires no auxiliary reagents, and serves as a useful alternative to conventional vapor generation for ultratrace Hg determination.     

Absolute quantification of specific proteins in complex mixtures using visible isotope-coded affinity tags

The identification of proteins in complex mixtures is most useful when quantitative information is also obtained. We describe a new type of protein tagging reagent called the visible isotope-coded affinity tag (VICAT) which allows the absolute amount of a target protein or proteins to be quantified in a complex biological sample such as a eukaryotic cell lysate. VICAT reagents tag thiol groups of cysteines or thioacetylated amino groups and introduce into the tryptic peptide a biotin affinity handle, a visible moiety for tracking the chromatographic location of the target peptide by a method other than mass spectrometry, a photocleavable linker for removing a portion of the tag, and an isotope tag for distinguishing sample and internal standard peptides. We demonstrate the use of VICAT reagents together with isoelectric focusing of peptides on an immobilized gel strip followed by combined micro-liquid chromatography/electrospray ionization mass spectrometry operating in selected reaction monitoring mode to determine the absolute abundance of a specific protein, human group V phospholipase A(2), in eukaryotic cell lysates. It is found that human lung macrophages contain 66 fmol of this protein per 100 microg of cell protein. Western blot analysis of human group V phospholipase A(2) in macrophages gave inconclusive data. VICAT reagents should be useful for numerous applications including the analysis of candidate disease markers in complex mixtures such as serum.     

Arsenic speciation in rice and soil containing related compounds of chemical warfare agents

Diphenylarsinic acid, phenylarsonic acid, methylphenylarsinic acid (MPAA), dimethylphenylarsine oxide (DMPAO), and methyldiphenylarsine oxide (MDPAO) in soil and rice were extracted, separated by reversed-phase chromatography, and quantified by ICPMS with a membrane desolvating system. For the extraction of arsenicals from rice grain and straw, 68% HNO3 provided better extraction efficiency than water, 50% methanol, or 2.0 mol L(-1) trifluoroacetic acid. For the extraction from soil, 68% HNO3 provided better extraction efficiency than H2O, 1 mol L(-1) H3PO4, or 1 mol L(-1) NaOH. The contaminated soil contained all five aromatic arsenicals along with inorganic arsenicals as main species (5.86 +/- 0.19 microg of As kg(-1): 60.8 +/- 2.0% of total extracted As). After pot experiments, rice straw contained mainly DMPAO (7.71 +/- 0.48 microg of As kg(-1): 60.5 +/- 3.7%), MDPAO (0.91 +/- 0.07 microg of As kg(-1): 7.2 +/- 0.5%), and inorganic As (2.85 +/- 0.20 microg of As kg(-1): 22.3 +/- 1.6%). On the other hand, rice grain contained mainly MPAA (1.17 +/- 0.04 microg of As kg(-1): 86.7 +/- 2.7%). The root uptake of each species from the soil and transport from straw to grains were significantly related to the calculated log K(ow) values.     

Equilibrium sampling through membranes of freely dissolved copper concentrations with selective hollow fiber membranes and the spectrophotometric detection of a metal stripping agent

A sensitive spectrophotometric method for the determination of freely dissolved copper concentrations in aqueous samples after preconcentration with hollow fiber membrane extraction has been developed. The method is based on the equilibrium sampling through a selective membrane into an acceptor solution containing 4-(pyridyl-2-azo)resorcinol (PAR), which serves as stripping agent and metal indicator. Negligible extraction of interferences and equilibrium enrichment of copper allowed for selective spectrophotometric determination of the Cu-PAR complex. Some important extraction parameters such as acceptor composition, shaking, equilibrium time, and sample volume were studied. The optimized methodology showed good linearity in the range of 5-100 microg/L, an enrichment factor of 93, good repeatability and reproducibility (RSDs < 6%, n = 6), and a detection limit of 4 microg/L. The cationic metals Ni2+, C(2+, Cd2+, Fe3+, Pb2+, Zn2+, and Mn2+ were shown not to interfere with the measurement of Cu2+. Measurements on samples containing mixtures of various ligands and cations were in good agreement with theoretically calculated concentrations, and the method was also applied to environmental samples. The developed technique requires less labor and less sophisticated equipment than conventional methods typically based on atomic absorption spectrometry or ICP.     

Octadecyl immobilized surface for precipitate collection with a renewable microcolumn in a lab-on-valve coupled to an electrothermal atomic absorption spectrometer for ultratrace cadmium determination

Octadecyl immobilized surface was, for the first time, proved to be a superb precipitate-collecting medium. Surface charge effect was assumed to dominate the adsorption of cadmium hydroxide precipitate, facilitated by electrostatic interaction between the negatively charged C18 bead surface and positively charged cadmium hydroxide clusters. Residual silanol groups on the C18-immobilized silica surface did not contribute to precipitate adsorption. A novel procedure for ultratrace cadmium preconcentration was proposed by incorporating a renewable microcolumn in a lab-on-valve system. Cd(OH)(2) precipitate was adsorbed onto the C18 surface, which was afterward eluted with 20 microL of nitric acid (1%) and quantified with detection by electrothermal atomic absorption spectrometry. An enrichment factor of 28 and a limit of detection of 1.7 ng L(-1), along with a sampling frequency of 13 h(-1) were obtained with a sample consumption of 600 microL within the concentration range of 0.01-0.2 microg L(-1), achieving a precision of 2.1% RSD at the 0.05 microg L(-1) level. The enrichment factor was further enhanced to 44 by increasing the sample volume to 1200 microL. The procedure was validated by analyzing cadmium in three certified reference materials, that is, river sediment (CRM 320), sea lettuce (CRM 279), and frozen cattle blood (GBW 09140). Good agreement between the obtained results and the certified values was achieved.     

Speciation of mercury by hydrostatically modified electroosmotic flow capillary electrophoresis coupled with volatile species generation atomic fluorescence spectrometry

A novel method for speciation analysis of mercury was developed by on-line hyphenating capillary electrophoresis (CE) with atomic fluorescence spectrometry (AFS). The four mercury species of inorganic mercury Hg(II), methymercury MeHg(I), ethylmercury EtHg(I), and phenylmercury PhHg(I) were separated as mercury-cysteine complexes by CE in a 50-cm x 100-microm-i.d. fused-silica capillary at 15 kV and using a mixture of 100 mmol L(-1) of boric acid and 12% v/v methanol (pH 9.1) as electrolyte. A novel technique, hydrostatically modified electroosmotic flow (HSMEOF) in which the electroosmotic flow (EOF) was modified by applying hydrostatical pressure opposite to the direction of EOF was used to improve resolution. A volatile species generation technique was used to convert the mercury species into their respective volatile species. A newly developed CE-AFS interface was employed to provide an electrical connection for stable electrophoretic separations and to allow on-line volatile species formation. The generated volatile species were on-line detected with AFS. The precisions (RSD, n = 5) were in the range of 1.9-2.5% for migration time, 1.8-6.3% for peak area response, and 2.3-6.1% for peak height response for the four mercury species. The detection limits ranged from 6.8 to 16.5 microg L(-1) (as Hg). The recoveries of the four mercury species in the water samples were in the range of 86.6-111%. The developed technique was successfully applied to speciation analysis of mercury in a certified reference material (DORM-2, dogfish muscle).     

Calibration for on-site analysis of hydrocarbons in aqueous and gaseous samples using solid-phase microextraction

Rapid sampling and sample preparation methodology was investigated using adsorptive poly(dimethylsiloxane)/divinylbenzene and Carboxen/poly(dimethylsiloxane) solid-phase microextraction (SPME) fiber coatings and volatile aromatic hydrocarbons (BTEX: benzene, toluene, ethylbenzene, and o-xylene). A flow-through system was used to generate a standard aqueous solution of BTEX as model sample with known linear velocity. Parameters that affect the extraction process, including sampling time, concentration, water velocity, and temperature, were investigated. Very short sampling times from 10 s and sorbents with strong affinity and large capacity were used to ensure the effect of '"zero sink" and to calibrate the extraction process in the initial linear extraction region. Several different concentrations were investigated, and it was found that mass uptake changes with concentration linearly. The increase of water velocity increases mass uptake, though the increase is not linear. Temperature does not affect mass uptake significantly under typical field sampling conditions. To further accurately describe rapid SPME analysis of aqueous samples, a new model translated from heat transfer to a circular cylinder in cross-flow was used. An empirical correlation to this model was used to predict the mass-transfer coefficient. Findings indicate that predicted mass uptake compares well with experimental mass uptake. The new model was tested for rapid air sampling, and it was found that this new model also predicted rapid air sampling accurately. Findings presented in this study extend the existing fundamental knowledge related to rapid sampling/sample preparation with SPME.     

Automated enzymatic assays in a renewable fashion using the multisyringe flow injection scheme with soluble enzymes

In this paper, a novel flowing stream scheme based upon the multisyringe flow injection (MSFI) technique is presented as a powerful tool to perform automated enzymatic assays. The exploitation of enzymes in homogeneous phase circumvents typical drawbacks associated with the commonly used packed-bead or open tubular permanent columns, namely, malfunctions of the reactor, carryover effects, flow resistance, loss of binding sites, large reagent consumption, and use of harmful organic solvents during immobilization procedures.The proposed MSFI system is able to handle minute volumes of soluble enzymes and accommodate reactions with divergent kinetic and pH demands, as demonstrated via the indirect chemiluminescence determination of trace levels of glucose. The procedure is based on the on-line glucose oxidase-catalyzed oxidation of beta-glucose in homogeneous phase to beta-glucono-delta-lactone and hydrogen peroxide. Subsequently, the generated oxidant merges downstream with an alkaline slug of 3-aminopthalhydrazide and a metal-catalyst zone (viz., Co(II)) at a total flow rate as high as 72 mL/min aiming to warrant maximum light collection from the fast CL reaction. Under optimum conditions for both sequentially occurring reactions, a glucose concentration as low as 90 microg/L may be easily detected at a 1000-fold photomultiplier gain. A second-order polynomial regression equation of light emission versus substrate concentration is found over the range 90 microg/L-2.7 mg/L glucose, although a maximum concentration of 180 mg/L may be determined by suitable gain selection without requiring manifold reconfiguration. An injection throughput of 20 h(-1), a repeatability better than 2.5% at the 1 mg/L level, and a 3sigma detection limit of 72 microg/L are the analytical features of the designed analyzer. The proposed approach was applied to the analysis of ultralow glucose content soft drinks as well as fruit juices suitable for diabetic consumers. The accuracy was assessed using the spectrophotometric batch glucose-Trinder method as an external reference methodology for the determination of the target species in parenteral solutions.     

Speciation of dissolved iron(III) and iron(II) in water by on-line coupling of flow injection separation and preconcentration with inductively coupled plasma mass spectrometry

A method has been developed for the speciation of trace dissolved Fe(II) and Fe(II) in water by on-line coupling of flow injection separation and preconcentration with inductively coupled plasma mass spectrometry (ICPMS). Selective determination of Fe(III) in the presence of Fe(II) was made possible by on-line formation and sorption of the Fe(III)-pyrrolidinecarbodithioate (PDC) complex in a PTFE knotted reactor over a sample acidity range of 0.07-0.4 mol L(-1) HCl, elution with 1 mol L(-1) HNO3, and detection by ICPMS. Over a sample acidity range of 0.001-0.004 mol L(-1) HCl, the sum of Fe(III) and Fe(II), i.e., Fe(III + II), could be determined without the need for preoxidation of Fe(II) to Fe(III). The concentration of Fe(II) was obtained as the difference between those of Fe(III + II) and Fe(III). With a sample flow rate of 5 mL min(-1) and a 30-s preconcentration time, an enhancement factor of 12, a retention efficiency of 80%, and a detection limit (3s) of 0.08 microg L(-1) were obtained at a sampling frequency of 21 samples h(-1). The relative standard deviation (n = 11) was 2.9% at the 10 microg L(-1) Fe(III) level. Recoveries of spiked Fe(III) and Fe(II) in local tap water, river water, and groundwater samples ranged from 95% to 103%. The concentrations of Fe(III) and Fe(II) in synthetic aqueous mixtures obtained by the proposed method were in good agreement with the spiked values. The result for total iron concentration in the river water reference material SLRS-3 was in good agreement with the certified value. The method was successfully applied to the determination of trace dissolved Fe(III) and Fe(II) in local tap water, river water, and groundwater samples.     

Completely automated system for determining halogenated organic compounds by multisyringe flow injection analysis

A new, multisyringe flow injection setup was designed to develop the first completely automated flow methodology for the expeditious, accurate in-line determination of halogenated organic compounds (HOCs) in water. The target compounds are preconcentrated and isolated by solid-phase extraction. Following elution, previously organically bound halogens are released as free hydrogen halides by the combined action of UV light and a chemical oxidant for their subsequent spectrophotometric determination by reaction with Hg(SCN) 2 and Fe(3+). Optimizing the major hydrodynamic and chemical variables resulted in improved performance. Recovery of various HOCs was assessed, and potential interferents were examined. Under the selected operating conditions, the proposed method exhibits variable analytical performance depending on the particular sample volume used (e.g., a sample volume of 5 mL provides a linear working range of 140-2000 microg L(-1), a LOD of 100 microg L(-1), and a throughput of 9 samples h(-1)). The method was successfully used to determine total adsorbable organic halogens (AOX) in well water and leachates, and the results validated against an AOX reference method. The role of the proposed system in the environmental analytical field is critically discussed.     

Determination of phosphoric acid mono- and diesters in municipal wastewater by solid-phase extraction and ion-pair liquid chromatography-tandem mass spectrometry

The first analytical method for the determination of 13 phosphoric acid mono- and diesters from aqueous samples is presented. The method consists of solid-phase extraction (SPE) and ion-pair liquid chromatographic separation with tri-n-butylamine coupled to electrospray ionization tandem mass spectrometry in the negative ion mode. Due to a lack of pure standards, only 3 of the 13 esters could be quantified. SPE recoveries ranged from 71 to 112% for di-n-butyl phosphate, diphenyl phosphate, and di-(2-ethylhexyl) phosphate (DEHP) with limits of quantification from 7 to 14 ng/L for 100-mL samples. At analyte concentrations >or=1 microg/L, aqueous samples can be analyzed by direct injection without extraction. In municipal wastewater, six diesters and one monoester were unambiguously identified by comparison with synthesized reference material. DEHP showed highest concentrations of 60 and 5 microg/L in raw and treated wastewater, respectively. The detection of monoethylhexyl phosphate was confirmed by LC-Q-TOF-MS analysis, and it was found at a concentration level comparable to DEHP. Laboratory degradation tests show that phosphoric acid diesters can be formed as intermediates in the microbial degradation of trialkyl phosphates that are being used as flame retardants and plasticizers.     

Adsorption of BTEX from aqueous solution by macroreticular resins

Theoretical and experimental investigations were conducted on the adsorption of benzene, toluene, ethylbenzene and xylene (BTEX) by macroreticular resins. A mass transfer model based on the squared-driving force principle is presented for describing the BTEX transfer between the aqueous and solid phases. Also proposed is a theoretical model for describing the BTEX breakthrough curves of the adsorption column. While the mass transfer model involves only an overall mass transfer coefficient, the column adsorption model has two model parameters. Those parameters are conveniently estimated using the observed mass transfer and breakthrough data. The predictions using the proposed models were found to compare well with the experimental data of batch and column BTEX adsorption tests.     

Preconcentration system for cadmium and lead determination in environmental samples using polyurethane foam/Me-BTANC

In this work, polyurethane foam (PUF) loaded with 2-(6'-methyl-2'-benzothiazolylazo)chromotropic acid (Me-BTANC) was packed in a minicolumn and it was used in an on-line preconcentration system for cadmium and lead determination. Optimum hydrodynamic and chemical conditions for metal sorption were investigated. The effects of several foreign substances on the adsorption of cadmium and lead were also reported. The enrichment factor obtained was 37 (Cd and Pb) for 180 s preconcentration time. The proposed procedures allowed the determination of metals with detection limits (3 sigma) of 0.80 and 3.75 microg L(-1) (0.10 and 0.47 microg g(-1) of solid sample) for cadmium and lead, respectively. The precision of the procedures was also calculated: 3.1 (Cd 10 microg L(-1)) and 4.4% (Pb 100 microg L(-1)). The accuracy of the procedure was checked by analysis of the certified reference materials Spinach Leaves and Fish Tissue. Cadmium and lead contents in environmental samples (black tea, spinach leaves, natural and tap water) were determined by applying the proposed procedure.     

A sol-gel based solid phase microextraction fiber for analysis of aromatic hydrocarbons

A sol-gel based solid phase microextraction fiber for headspace sampling (HP-SPME) and GC determination of benzene, toluene, ethylbenzene and xylenes (BTEX) is introduced. The influences of fiber composition, microextraction conditions such as temperature and time on the fiber performance and desorption temperature and time were investigated. Under optimal conditions, the use of proposed fiber was thermally stable up to 250 degrees C and demonstrated high sensitive and fast sampling of BTEX from gaseous phase. Depending on the analysed substance, the linear range for a selected fiber and the applied GC-FID technique was from 4 to 80 ng mL(-1)with limit of detection (LOD) 0.2-0.7 ng mL(-1) and 100-1000 ng mL(-1) with LOD 8-20 ng mL(-1) for gaseous and soil samples, respectively. HP-SPME-GC analysis was highly reproducible-relative standard deviations (R.S.D.) were between 5.0 and 7.9%. The proposed fiber was successfully used for BTEX sampling from indoor air and headspace of soil samples.