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 共查询到10条相似文献,搜索用时 93 毫秒
1.
A solid-phase microextraction (SPME) fiber coated with single walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition and treated at 500 °C in H2 stream. In order to evaluate the characteristics of the obtained fiber, it was applied in the headspace solid-phase microextraction (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample and quantification by gas chromatography with flame ionization detection (GC-FID). The results indicated that the thermal treatment with H2 enhanced the extraction of the SWCNTs fiber for BTEX significantly. Thermal stability and durability of the fiber were also investigated, showing excellent stability up to 350 °C and life time over 120 times. In the comparison with the commercial CAR–PDMS fiber, the SWCNTs fiber showed similar and higher extraction efficiencies for BTEX. Under the optimized conditions, the linearity, LODs (S/N = 3) and LOQs (S/N = 10) of the method based on the SWCNTs fiber were 0.5–50.0, 0.005–0.026 and 0.017–0.088 μg/L, respectively. Repeatability for one fiber (n = 3) was in the range of 1.5–5.6% and fiber-to-fiber reproducibility (n = 3) was in the range of 4.2–8.3%. The proposed method was successfully applied in the analysis of BTEX compounds in seawater, tap water and wastewater from a paint plant.  相似文献   

2.
Feng J  Sun M  Xu L  Li J  Liu X  Jiang S 《Journal of chromatography. A》2011,1218(43):7758-7764
Polymeric 1-vinyl-3-octylimidazolium hexafluorophosphate was synthesized in situ on stainless steel wire by surface radical chain-transfer polymerization and used as sensitive coatings in solid-phase microextraction. The outer surface of the stainless steel wire was firstly coated with microstructured silver layer via silver mirror reaction and then functionalized with self-assembled monolayers of 1,8-octanedithiol, which acted as chain transfer agent in the polymerization. Coupled to gas chromatography, extraction performance of the fiber was studied with both headspace and direct-immersion modes using benzene, toluene, ethylbenzene and xylenes (BTEX), phenols and polycyclic aromatic hydrocarbon (PAHs) as model analytes. In combination with the microstructured silver layer, the PIL-coated fiber exhibited high extraction efficiency. Linear ranges for BTEX with headspace mode were in the range of 0.2-1000 μg L(-1) for benzene, and 0.1-1000 μg L(-1) for toluene, ethylbenzene and xylenes. Limits of detection (LODs) were from 0.02 to 0.05 μg L(-1). Wide linear ranges of direct-immersion mode for the extraction of several phenols and PAHs were also obtained with correlation coefficients (R) from 0.9943 to 0.9997. The proposed fiber showed good durability with long lifetime. RSDs of 56 times extraction were still in an acceptable range, from 8.85 to 22.8%.  相似文献   

3.
This paper presents a fully automated method for determining ten primary amines in wastewater at ng/L levels. The method is based on simultaneous derivatization with pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to ion trap tandem mass spectrometry (GC–IT-MS–MS). The influence of main factors on the efficiency of derivatization and of HS-SPME is described in detail and optimized by a central composite design. For all species, the highest enrichment factors were achieved using a 85 μm polyacrylate (PA) fiber exposed in the headspace of stirred water samples (750 rpm) at pH 12, containing 360 g/L of NaCl, at 40 °C for 15 min. Under optimized conditions, the proposed method achieved detection limits ranging from 10 to 100 ng/L (except for cyclohexylamine). The optimized method was then used to determine the presence of primary amines in various types of wastewater samples, such as influent and effluent wastewater from municipal and industrial wastewater treatment plants (WWTPs) and a potable water treatment plant. Although the analysis of these samples revealed the presence of up to 1500 μg/L of certain primary amines in influent industrial wastewater, the concentration of these compounds in the effluent and in municipal and potable water was substantially lower, at low μg/L levels. The new derivatization–HS-SPME–GC–IT-MS–MS method is suitable for the fast, reliable and inexpensive determination of primary amines in wastewater in an automated procedure.  相似文献   

4.
A novel sol–gel coating on a stainless‐steel fiber was developed for the first time for the headspace solid‐phase microextraction and determination of α‐bisabolol with gas chromatography and flame ionization detection. The parameters influencing the efficiency of solid‐phase microextraction process, such as extraction time and temperature, pH, and ionic strength, were optimized by the experimental design method. Under optimized conditions, the linear range was between 0.0027 and 100 μg/mL. The relative standard deviations determined at 0.01 and 1.0 μg/mL concentration levels (= 3), respectively, were as follows: intraday relative standard deviations 3.4 and 3.3%; interday relative standard deviations 5.0 and 4.3%; and fiber‐to‐fiber relative standard deviations 6.0 and 3.5%. The relative recovery values were 90.3 and 101.4% at 0.01 and 1.0 μg/mL spiking levels, respectively. The proposed method was successfully applied to various real samples containing α‐bisabolol.  相似文献   

5.
A new generation of solid-phase microextraction (SPME) fiber, an internally cooled fiber (cold fiber with polydimethylsiloxane loading) that allows heating the sample matrix and simultaneously cooling the fiber coating, was used to determine 2,4-dichloroanisole, 2,6-dichloroanisole, 2,4,6-trichloroanisole and pentachloroanisole in cork. A comparison between the cold fiber and regular SPME fiber was performed. An automated headspace solid-phase microextraction (HS-SPME) using commercial fibers and an internally cooled SPME fiber (CF-HS-SPME) coupled to gas chromatography-time-of-flight mass spectrometry (GC-TOF-MS) was used. The extraction conditions for both CF-HS-SPME and HS-SPME were optimized using full factorial design and Doehlert matrix. The best extraction conditions for CF-HS-SPME were obtained using 10 min of incubation time, 10 min of extraction time, and sample and fiber temperature of 130 and 10 degrees C, respectively. For HS-SPME, polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used with 10 min of incubation time, 75 min of extraction time, 85 degrees C of sample temperature, 8 ml of water was added and agitated at 500 rpm. The quantification limits for the target compounds using CF-HS-SPME procedure were between 0.8 and 1.6 ng g(-1) of cork, while for HS-SPME were between 4 and 6 ng g(-1) of cork. Furthermore, the CF-HS-SPME procedure could be used as a non-destructive method after minor modification of the agitator for the autosampler.  相似文献   

6.
The present work reports preparation of ordered mesoporous carbon (OMC) film supported on a graphite fiber as a new type of solid-phase microextraction (SPME) fiber for determination of benzene series from aqueous media. The strategy for the supported OMC film preparation was combined dip-coating technology with solvent evaporation-induced self-assembly (EISA) approach. A graphite fiber was immersed in an ethanol solution containing phenolic resin and Pluronic triblock copolymer. Upon solvent evaporation and subsequent pyrolysis under 700 °C, the phenolic resin and the surfactant self-assembled on the surface of the graphite fiber to form smooth OMC film. X-ray diffraction (XRD), transmission electron microscopy (TEM) and nitrogen isothermal adsorption results indicate that the resultant OMC film possesses well-ordered two dimensional hexagonal mesostructure with pore diameters of 4.5 nm and BET surfaces of 630 m2/g. Scanning electron microscopy (SEM) studies show the supported OMC film with thickness at 8.5 μm is continuous and defect-free. The SPME efficiency of the OMC fiber was evaluated by analysis of five benzene series (benzene, toluene, ethylbenzene, p-xylene and m-xylene) from water samples by gas chromatography-flame ionization detection (GC-FID). The analysis results indicate that the prepared OMC fiber has wide linear ranges (0.5–500 μg/L), low detection limits (0.01–0.05 μg/L) and good repeatabilities (4.0–5.8% for one fiber, 2.9–8.7% for fiber-to-fiber). Compared with commercial counterparts, the OMC fiber exhibits improved extraction efficiency for benzene series and PAHs.  相似文献   

7.
Novel solid-phase microextraction fibers were prepared based on sol–gel technique. Commonly used fused silica substrate was replaced by titanium wire which provided high strength and longer fiber life cycle. Titanium isopropoxide was employed as the precursor which provides a sol solution containing Ti–OH groups and shows more tendencies to the molecularly similar group on the substrate. Three different polymers, poly (dimethylsiloxane) (PDMS), poly(ethylenepropyleneglycol)-monobutyl ether (Ucon) and polyethylene glycol (PEG) were employed as coating polymer in preparing three different fibers. The applicability of these fibers was assessed for the headspace SPME (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample followed by gas chromatography–mass spectrometry (GC–MS). Effects of different parameters such as fiber coating type, extraction condition, desorption condition were investigated and optimized. Under the optimized conditions, LODs and LOQs of 0.75–10 μg L−1 (S/N = 3) and 1–20 μg L−1 (S/N = 10) were respectively obtained. The method showed linearity in the range of 10–25,000 μg L−1 with correlation coefficient of >0.99. The relative standard deviation was less than 8%.  相似文献   

8.
A simple, low-cost, and effective cooling/heating-assisted headspace solid-phase microextraction (CHA–HS–SPME) device, capable of direct cooling the fiber to low temperatures and simultaneous heating the sample matrix to high temperatures, was fabricated and evaluated. It was able to cool down the commercial and handmade fibers for the effective tapping of volatile and semi-volatile species in the headspace of complex solid matrices, with minimal manipulation compared with conventional SPME. The CHA–HS–SPME system can create large temperature gaps (up to 200 °C) between the fiber and the sample matrix, because the cooling process is directly applied onto the fiber.  相似文献   

9.
A novel nanocomposite coating of poly(o‐toluidine) and oxidized multiwalled CNTs (MWCNTs, where CNTs is carbon nanotubes) was electrochemically prepared on a stainless‐steel wire. The applicability of the fiber was assessed for the headspace solid‐phase microextraction of benzene, toluene, ethylbenzene, and xylenes in aqueous samples followed by GC with flame ionization detection. In order to obtain an adherent and stable composite coating, several experimental parameters related to the coating process, such as polymerization potential and time, and the concentration of o‐toluidine and oxidized MWCNTs were optimized. The combination of MWCNTs and polymer in a nanocomposite form presents desirable opportunities to produce materials for new applications. The effects of various parameters on the efficiency of the headspace solid‐phase microextraction process, such as desorption temperature and time, extraction temperature and time, and ionic strength were also investigated. At the optimum conditions, LODs were 0.03–0.06 μg/L. The method showed linearity in the range of 0.5–300 μg/L with coefficients of determination >0.99. The intraday and interday RSDs obtained at a 5 μg/L concentration level (n = 5) using a single fiber were 1.2–5.2 and 3.2–7.5%, respectively. The fiber‐to‐fiber RSD (%; n = 3) at 5 μg/L was 6.1–9.2%.  相似文献   

10.
Ji J  Deng C  Shen W  Zhang X 《Talanta》2006,69(4):894-899
In this work, portable gas chromatography-microflame ionization detection (portable GC-μFID) coupled to headspace solid-phase microextraction (HS-SPME) was developed for the field analysis of benzene, toluene, ethylbenzene and xylene (BTEX) in water samples. The HS-SPME parameters such as fiber coating, extraction times, stirring rate, the ratio of headspace volume to sample volume, and sodium chloride concentration were studied. A 65 μm poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) SPME fiber, 900 rpm, 3.0 ml of headspace (1.0 ml water sample in 4.0 ml vial), and 35% sodium chloride concentration (w/v) were respectively chosen for the best extraction response. An extraction time of 1.0 min was enough to extract BTEX in water samples. The relative standard deviation (R.S.D.) for the procedure varied from 5.4% to 8.3%. The method detection limits (MDLs) found were lower than 1.5 μg/l, which was enough sensitive to detect the BTEX in water samples. The optimized method was applied to the field analysis of BTEX in wastewater samples. These experiment results show that portable GC-μFID combined with HS-SPME is a rapid, simple and effective tool for field analysis of BTEX in water samples.  相似文献   

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