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1.
An automatic sampling device, i.e., process sampling module (PSM), connected with a purge and trap-GC-FID system has been developed for real-time monitoring of VOCs in wastewater. The system was designed to simultaneously monitor 17 compounds, including one polar compound, i.e., acetone, and 16 non-polar compounds. The trapping tube is packed with two adsorbents, Carbopack B and Carbosieve III, to trap target compounds. For the purpose of in situ monitoring, the flush valve of the sampling tube is composed of two two-way valves and a time controller to prevent absorption interference of the residue. The optimal conditions for the analytical system include a 12 min purge time at a temperature of 60 °C, and 4 min of desorption time with a desorption temperature of 260 °C. Good chromatograms have been obtained with the analytical system even if a cryogenic device and de-misting were not used. The relative standards deviation (RSD) of the system is between 2% and 13.4%, and accuracies between 0.3 and 23.5% have been achieved. The detection limits of the method range from 0.32 to 2.39 ppb. In this system, the four parts, i.e., PSM, P&T, GC, and FID, were simple, reliable and rugged. Also, the interface of these four parts was simple and dependable.  相似文献   

2.
Summary A protocol combining purge-and-trap (P&T) and solid-phase microextraction (SPME) was established for the analysis of volatile organic compounds (VOCs) in the wastewater plant of high-tech industries. Over 60 VOCs could be analyzed by P&T coupled to gas chromatography/mass spectrometry (P&T-GC-MS). Four polar VOCs commonly used in the high-tech industries were determined by SPME coupled to gas chromatography/flame ionization detection (SPME-GC-FID). The limits of detection for the analytes were less than 1.1 μg L−1 with P&T-GC-MS, and between 1.5 and 12.5 μg L−1 with SPME-GC-FID. Satisfactory recoveries (83% to 130%) were obtained. Real samples were analyzed from a wastewater treatment plant during various stages of treatment. The major pollutant in the wastewater influent was found to be acetone (>4 ppm).  相似文献   

3.
Compound-specific isotope analysis (CSIA) has been established as a useful tool in the field of environmental science, in particular in the assessment of contaminated sites. What limits the use of gas chromatography/isotope ratio mass spectrometry (GC/IRMS) is the low sensitivity of the method compared with GC/MS analysis; however, the development of suitable extraction and enrichment techniques for important groundwater contaminants will extend the fields of application for GC/IRMS. So far, purge and trap (P&T) is the most effective, known preconcentration technique for on-line CSIA with the lowest reported method detection limits (MDLs in the low microg/L range). With the goal of improving the sensitivity of a fully automated GC/IRMS analysis method, a commercially available P&T system was modified. The method was evaluated for ten monoaromatic compounds (benzene, toluene, para-xylene, ethylbenzene, propylbenzene, isopropylbenzene, 1,2,3-trimethylbenzene, 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, fluorobenzene) and ten halogenated volatile organic compounds (VOCs) (dichloromethane, cis-1,2-dichloroethene, trans-1,2-dichloroethene, carbon tetrachloride, chloroform, 1,2-dichloroethane, trichloroethene, tetrachlorethene, 1,2-dibromoethane, bromoform). The influence of method parameters, including purge gas flow rates and purge times, on delta13C values of target compounds was evaluated. The P&T method showed good reproducibility, high linearity and small isotopic fractionation. MDLs were determined by consecutive calculation of the delta13C mean values. The last concentration for which the delta13C value was within this iterative interval and for which the standard deviation was lower than +/-0.5 per thousand for triplicate measurements was defined as the MDL. MDLs for monoaromatic compounds between 0.07 and 0.35 microg/L are the lowest values reported so far for continuous-flow isotope ratio measurements using an automated system. MDLs for halogenated hydrocarbons were between 0.76 and 27 microg/L. The environmental applicability of the P&T-GC/IRMS method in the low-microg/L range was demonstrated in a case study on groundwater samples from a former military air field contaminated with VOCs.  相似文献   

4.
In this work the simultaneous purge-and-trap (P&;T) preconcentration of volatile fatty acids (acetic acid, propanoic acid, butanoic acid, iso-butanoic acid, pentanoic acid, iso-pentanoic acid, hexanoic acid and heptanoic acid), phenols (phenol, 4-methylphenol and 4-ethylphenol) and indoles (indole and 3-methylindole) from cow slurries was carried out in order to quantify them by gas chromatography flame ionisation detection (GC–FID). The optimisation of the preconcentration was performed using spiked cow slurries and the variables studied were the nature of the trap, the purge and heating time and the amount of inert salt (NaCl) added. Other parameters such as purge flow, sample volume, desorption time and temperature and baking time and temperature were kept constant. The first variable studied was the nature of the preconcentration trap. Four different commercially available traps (Vocarb 4000, Vocarb 3000, BTEXTRAP and Tenax/silica gel/carbon) were studied and Vocarb 3000 gave best results. Once the optimum trap was chosen, appearance of possible memory peaks were studied and significant signals were observed for 4-methylphenol, 4-ethylphenol, indole and 3-methylindole. In order to improve the blanks after each analysis the following actions were taken: (1) the needle sparger was located in the headspace of the sample and (2) all the replaceable parts of the P&;T (sample tube, needle sparger, Teflon ferrules, nuts, etc.) were washed, sonicated in acetone for 15 min and dried in an oven at 350 °C. Once the blank problems were minimised, the remaining variables (purge and heating time and the amount of NaCl) were optimised using the MultiSimplex® program, which enabled the study of several variables and responses simultaneously. Optimum conditions for the simultaneous preconcentration were obtained after 24 experiments and the final optimised preconcentration conditions were as follows: 0.4 g of NaCl were added to 10 mL sample which was heated at 80 °C for 10 min and purged for 20 min while the Vocarb 3000 trap remained at room temperature. Once the purge step was over, the trap was desorbed at 250 °C for 6 min and baked at 260 °C for 10 min. After the optimisation of the P&;T based preconcentration, the precision (within and among days), accuracy and detection limits of the method were studied.  相似文献   

5.
The purge and trap (P&T) method of analysis has been interfaced with fused silica capillary column gas chromatography. This interfacing has been accomplished without splitting the P&T trap desorption carrier gas. Thus, 100% of the purged compounds are transferred to the column. The analytes are cryofocussed on the column using whole column cryotrapping (WCC) at ?80°C. The resulting P&T/WCC procedure is extremely well-suited to the analysis of trace purgeable aqueous organic compounds. Samples and standards containing a variety of aromatic standard compounds were analyzed. The standards included benzene, toluene, ethylbenzene, xylenes, C3-C4-benzenes, and naphthalene, as well as three P&T internal standard compounds. Chromatographic peak widths were uniformly less than 6 s at the base and excellent precision was obtained in the relative retention time data for all compounds. The chromatogram of a groundwater sample contaminated with aromatic gasoline compounds is also presented. Since P&T/WCC works well with fused silica capillary columns, the full sensitivity and chromatographic efficiency of capillary gas chromatography is made available to P&T analyses.  相似文献   

6.
Summary A comparison of different isolation methods for volatile compounds from the leaves ofLedum palustre has been carried out. The aim of the investigation was not to identify all the isolated compounds, though some new compounds were found. Methods used were steam distillation, Soxhlet extraction with n-hexane and the purge & trap technique.The results obtained by the three methods of extraction were compared and it is was found that the very volatile compounds isolated by the purge & trap technique, could not be found by the more conventional methods. The very volatile compounds found by the purge & trap technique were mainly dienals.  相似文献   

7.
瞿白露  许雄飞  陈军 《广州化学》2010,35(4):39-42,77
用吹扫捕集和气相色谱―质谱联用技术对地表水中的26种挥发性有机污染物进行同时测定。实验结果在2.0~50.0μg/L范围内线性良好,相关系数均大于0.99,检出限在0.08~0.91μg/L范围内。方法的平均回收率为87.33%~116.68%,相对标准偏差(RSD)均小于5%。该方法前处理简单快速,采用内标法定量准确度高,重复性好,适用于清洁水中挥发性有机物的测定。  相似文献   

8.
Epichlorohydrin (ECH) can enter drinking-water supplies due to leaching from epoxy resins in contact with water and/or through the use of flocculating water treatment agents. Potential human exposure from drinking waters poses a particular concern on account of toxicological studies showing severe acute and long-term toxic effects of ECH. Recently a parametric value of 0.1 μg/L for ECH in drinking water has been established by European Union.A few methods for ECH determination in water are available. However, they usually adopt cumbersome procedures for sample preparation and provide sensitivity not matching the EU criteria for water monitoring purposes.In this study we investigated the analytical performance of gas extraction techniques, such as static headspace (HS) and purge and trap (P&T), coupled to gas chromatography (GC) with an electron capture detector (GC-ECD) for the determination of ECH in drinking water. The influence of different parameters affecting the analytical response was studied in details in order to enhance the method sensitivity, thus fulfilling the regulatory requirements.The P&T GC-ECD method was proved capable of determining ECH in water for human consumption at a detection limit of 0.01 μg/L fully complying the regulatory levels. On the contrary, the HS GC-ECD method is far less sensitive (LOD≅40 μg/L) than the previous cited method. The P&T GC-ECD method is simple, rapid, automated, safe for operators and does not require large sample volumes. Therefore, it is useful for routine laboratory activities both for control and research actions.  相似文献   

9.

Some aroma compounds found in alcoholic beverages are characteristic of a certain beverage (i.e. 2,4-decadienoic acid ethyl ester is characteristic of pear spirit and 5-butyltetrahydro-4-methylfuran-2-on “whiskey lactone” is characteristic of aged spirits like whiskey). These substances were detectable in beverages but not in blood samples. The aim of this investigation was to find a sensitive sampling technique for aroma compounds in whole blood samples. This technique may be used in forensic toxicology for examination of drinking claims. The method comprises dynamic headspace sampling using a purge and trap concentrator, followed by quantitative gas chromatography–mass spectrometry (dynamic HS–GC–MS). The influence of sample preparation, trap adsorbents and sample temperature as well as desorption time and purge time on the quality of the analytical results were investigated. The following optimal parameters were determined: stirred and diluted whole blood sample without salt addition, use of Carbotrap C as trap material, sample temperature at 80 °C, desorption time 20 min and purge time 30 min. These optimal parameters were used for the determination of detection limits (LOD). The LOD of aroma compounds by means of dynamic headspace sampling were compared with the results of conventional sampling: the static headspace technique. Limits of detection for the aroma compounds with conventional static headspace GC are in the range 400–10,000 μg L−1. Dynamic headspace–GC was found to be a more sensitive sampling technique for most of the aroma compounds investigated (e.g. C4–C8 ethyl esters, benzoic acid ethyl ester, linalool oxide and 4-ethylguaiacol) with detection limits between 1 and 50 μg L−1, but there were also limits to the sampling of substances with lower volatility like decanoic acid ethyl ester, 2,4-decadienoic acid ethyl ester, eugenol and whiskey lactone with detection limits of about 1,000 μg L−1.

  相似文献   

10.
Some aroma compounds found in alcoholic beverages are characteristic of a certain beverage (i.e. 2,4-decadienoic acid ethyl ester is characteristic of pear spirit and 5-butyltetrahydro-4-methylfuran-2-on “whiskey lactone” is characteristic of aged spirits like whiskey). These substances were detectable in beverages but not in blood samples. The aim of this investigation was to find a sensitive sampling technique for aroma compounds in whole blood samples. This technique may be used in forensic toxicology for examination of drinking claims. The method comprises dynamic headspace sampling using a purge and trap concentrator, followed by quantitative gas chromatography–mass spectrometry (dynamic HS–GC–MS). The influence of sample preparation, trap adsorbents and sample temperature as well as desorption time and purge time on the quality of the analytical results were investigated. The following optimal parameters were determined: stirred and diluted whole blood sample without salt addition, use of Carbotrap C as trap material, sample temperature at 80 °C, desorption time 20 min and purge time 30 min. These optimal parameters were used for the determination of detection limits (LOD). The LOD of aroma compounds by means of dynamic headspace sampling were compared with the results of conventional sampling: the static headspace technique. Limits of detection for the aroma compounds with conventional static headspace GC are in the range 400–10,000 μg L?1. Dynamic headspace–GC was found to be a more sensitive sampling technique for most of the aroma compounds investigated (e.g. C4–C8 ethyl esters, benzoic acid ethyl ester, linalool oxide and 4-ethylguaiacol) with detection limits between 1 and 50 μg L?1, but there were also limits to the sampling of substances with lower volatility like decanoic acid ethyl ester, 2,4-decadienoic acid ethyl ester, eugenol and whiskey lactone with detection limits of about 1,000 μg L?1.  相似文献   

11.
We have previously developed a purge‐and‐trap (P&T) preconcentrator, useful for the determination of trace amounts of ammonium ion in high‐salinity water samples by ion chromatography (IC). In this study, we succeeded in improving the P&T system to markedly enhance performance and efficiency for the determination of ammonium in high‐salinity water samples. Compared to the previous work, the background signal was reduced by a factor of 9. The maximum overall collection efficiency increased greatly from 64% to 97%. With the modified P&T system, this method can be applied to a wide ammonium concentration range of 5 orders of magnitude. These were attributed to the substitution of polypropylene vessels for glass ones, the improvement of the gastight of the P&T system, the increase of the liquid depth in the purge vessel, and the use of 10 mM sulfuric acid as the trapping solution for high ammonium concentration samples. Interferences of 20 native amino acids to the ammonium determination are slightly positive, but also negligible except asparagine and glutamine. The proposed method has been successfully applied to the accurate determination of wide levels of ammonium in seawater and sweat samples.  相似文献   

12.
The effects of trapping temperature and column film thickness were investigated with respect to their ability to promote effective cryofocusing on fused silica capillary columns. The study was a further development of the purge and trap with whole column cryotrapping (P&T/WCC) method. The rates at which compounds could be thermally desorbed from a P&T unit and transferred to a column (with zero split) were first examined. A near quantitative transfer of the desorbable analytes was obtained with a 4 min, 180°C, 20 mL/min desorption. The compounds tested included naphthalene. Columns with film thicknesses from 0.12 to 3.0 μm were then investigated in P&T/WCC analyses with WCC temperatures ranging from ?80 to 0°C. The trapping took place from a transfer line gas stream initially at 175°C. The volatilities of the compounds examined varied from that of 1,1-dichloroethene to 1,1,2,2-tetrachloroethane. A higher film thickness was found to ease the WCC temperature requirements. Within each column type, the warmest WCC temperatures which allowed good cryotrapping with no significant increases in peak width were: 0.25 μm, ?70°C; 1.0 μm, ?50°C; 3.0 μm, ?20°C. In addition to being quantitative, the trapping provided good chromatography.  相似文献   

13.
Partitioning and transmutation (P&T) technologies have been developed for minor actinides (MA) to reduce the high level waste (HLW) volume and long-term radiotoxicity. Although the MA P&T can reduce the potential radiotoxicity effectively by 1-3 orders of magnitude, the actual operation of P&T requires several tens of years for developing elemental technologies of nuclide separation, MA containing fuel fabrication, transmutation and their practical systematization. The high level liquid waste (HLLW) containing MA is presently vitrified immediately after spent fuel reprocessing, stored about 50 years at surface facility and will be disposed of at deep geological repository. Vitrified HLW form works as an excellent artificial barrier against nuclides release during storage and disposal. On the other hand, it is difficult to recover MA from the form. So the present waste management scheme has an issue of MA P&T technology application until its deployment, which will produce much amount of vitrified HLW including long-lived MA without P&T application. Thus the authors proposed the flexible waste management method to increase the effectiveness of the MA P&T. The system adopts the HLLW calcination instead of the vitrification to produce granule for its dry storage of about 50 years until the MA P&T technology will be applicable. The granule should be easily dissolved by the nitric acid solution to apply the typical aqueous MA partitioning technologies to be developed. This paper reports the purpose of the study, the feasibility evaluation results for the calcined granule storage and the evaluation results for the environmental burden reduction effect.  相似文献   

14.
建立吹扫捕集–气相色谱–质谱联用法测定环境水中101种常见挥发性有机物(VOCs)的方法。通过加热吹扫,样品水中的VOCs富集于捕集管中,以DB–624(60 m×0.25 mm,1.4μm)色谱柱分离,内标法定量。结果表明,101种挥发性有机物(VOCs)色谱分离效果良好,质量浓度在0.5~50 ng/mL范围内与色谱峰面积均呈线性关系,高沸点VOCs线性范围较窄。方法定量限(10 S/N)为0.11~0.77 ng/mL,均低于GB 3838–2002《地表水环境质量标准》、GB 5749–2006《生活饮用水卫生标准》及国外相关标准的限值。平均加标回收率在70.3%~123.6%之间,测定结果的相对标准偏差不大于8.8%(n=6)。该方法快速、简便,适用于环境水中挥发性有机化合物的分析检测。  相似文献   

15.
Deng X  Liang G  Chen J  Qi M  Xie P 《Journal of chromatography. A》2011,1218(24):3791-3798
Production and fate of taste and odor (T&O) compounds in natural waters are a pressing environmental issue. Simultaneous determination of these complex compounds (covering a wide range of boiling points) has been difficult. A simple and sensitive method for the determination of eight malodors products of cyanobacterial blooms was developed using automatic purge and trap (P&T) coupled with gas chromatography-mass spectrometry (GC-MS). This extraction and concentration technique is solvent-free. Dimethylsulfide (DMS), dimethyltrisulfide (DMTS), 2-isopropyl-3-methoxypyrazine (IPMP), 2-isobutyl-3-methoxypyrazine (IBMP), 2-methylisoborneol (MIB), β-cyclocitral, geosmin (GSM) and β-ionone were separated within 15.3 min. P&T uses trap #07 and high-purity nitrogen purge gas. The calibration curves of the eight odors show good linearity in the range of 1-500 ng/L with a correlation coefficient above 0.999 (levels=8) and with residuals ranging from approximately 83% to 124%. The limits of detection (LOD) (S/N=3) are all below 1.5 ng/L that of GSM is even lower at 0.08 ng/L. The relative standard deviations (RSD) are between 3.38% and 8.59% (n=5) and recoveries of the analytes from water samples of a eutrophic lake are between 80.54% and 114.91%. This method could be widely employed for monitoring these eight odors in natural waters.  相似文献   

16.
张赟彬  缪存铅  崔俭杰 《化学学报》2009,67(20):2368-2374
采用同时蒸馏萃取提取得到荷叶挥发油, 通过吹扫/捕集-热脱附法(P&T-TD)对上述提取物中挥发性成分进行富集, 以气质联用(GC/MS)进行定性检测, 同时与直接进样GC/MS法分析的成分进行比较. 两种方法成功分离分析出有机酸、酯、醛、醇、酚、烷烃、芳香烃、烯烃以及含氮、硫、氧杂原子的化合物等共计84种成分, 其中P&T-TD GC/MS鉴定出63种有机化合物, GC/MS鉴定出41种有机化合物, 有20种成分共同检出. 对比分析表明: P&T-TD GC/MS的吹扫/捕集-热脱附过程能富集各种组分, 相比GC/MS分析, 可以鉴定出微量成分及更多挥发性和半挥发性成分, 在精油等挥发性成分的分析检测中使用优势明显.  相似文献   

17.
A purge and trap (P&T) continuous flow system was developed in order to concentrate high volumes of water for trace analyses and stable carbon isotope measurements of volatile halogenated organic compounds (VHOCs) in seawater. The P&T parameters were evaluated regarding quality parameters, extraction efficiency and isotope fractionation. Precision (about 20%), linearity (>0.9676), and recoveries (between 75% and 99%) were reasonable within the large concentration range tested. Isotope fractionation was between 1 per thousand and 3 per thousand. Finally, the developed system was successfully applied to the quantitative and stable carbon isotope analysis of three water samples of different origin.  相似文献   

18.
Headspace solid-phase microextraction (HS-SPME) followed by gas chromatography–mass spectrometry analysis (GC-MS) was used to investigate the volatile compounds from oxidised phosphatidylcholine molecular species. 1-stearoyl-2-oleoyl-sn-glycero-3-phosphocholine (SOPC) and 1-stearoyl-2-linoleoyl-sn-glycero-3-phosphocholine (SLPC) were chosen as models. The influence of several parameters on the efficiency of volatile oxidised compounds (VOCs) microextraction, such as type of fibre, extraction duration and temperature were studied. The best results were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre used at 50 °C during 25 min. The effect of oxidation temperature on the yield of VOCs from SOPC and SLPC was investigated. Oxidative kinetics of SOPC and SLPC were investigated by measuring both the production of VOCs and the degradation of starting materials. More than 30 VOCs were detected by means of the reference mass spectra of the National Institute of Standards and Technology mass spectral library, and most of them were further confirmed by comparing their mass spectra and retention time with those obtained from authentic reference compounds under the same analytical conditions. Moreover, the origins of VOCs from oxidised PLs were studied by comparing those obtained from their corresponding triacylglycerides under the same experimental conditions. The main VOCs identified from oxidised SOPC were (E)-2-decenal, nonanal and octanal and from oxidised SLPC were (E)-2-heptenal, (E)-2-octenal and (E, E)-2,4-decadienal. The proposed method was applied to a real food sample, soy lecithin.
Figure
Production of volatiles from oxidised phospholipid  相似文献   

19.
A new method for the growth-dependent headspace analysis of bacterial cultures by needle trap (NT)-gas chromatography-mass spectrometry (GC-MS) was established. NTs were used for the first time as enrichment technique for volatile organic compounds (VOCs) in the headspace of laboratory cultures. Reference strains of Escherichia coli and Pseudomonas aeruginosa were grown in different liquid culture media for 48 h at 36 °C. In the course of growth, bacterial culture headspace was analysed by NT-GC-MS. In parallel, the abiotic release of volatile organic compounds (VOC) from nutrient media was investigated by the same method. By examination of microbial headspace samples in comparison with those of uninoculated media, it could be clearly differentiated between products and compounds which serve as substrates. Specific microbial metabolites were detected and quantified during the stationary growth phase. P. aeruginosa produced dimethyl sulfide (max. 125 μg L?1??1) and 2-nonanone (max. 200 μg L?1), whereas E. coli produced carbon disulfide, butanal and indole (max. 149 mg L?1). Both organisms produced isoprene. Graphical Abstract
MVOCs produced by P. aeruginosa and E. coli at T = 36 °C in autoclaved LB + TRP medium   相似文献   

20.
Currently, bleached eucalypt pulps are largely used for printing and writing (P&W) and sanitary (tissue) paper grades. Among the many pulp quality requirements for P&W and tissue paper production the xylan content is one of the most significant. For P&W papers, increasing xylans improve pulp refinability and strength properties but negatively affect bulk and drainability. For tissue paper, xylans are purportedly advantageous during paper drying in the Yankee cylinder but negatively affect paper bulk and may increase dusting during paper manufacture. On the other hand, bleachability is a very important parameter for both P&W and tissue grade pulps since bleaching cost is the second most significant in eucalypt bleached kraft pulp production. The aim of this study was evaluating the influence of eucalyptus pulp xylan content on its bleachability, refinability and drainability. A sample of industrial unbleached eucalyptus kraft pulp containing 15.6?% xylans was treated with various alkali charges at room temperature in order to obtain materials with different xylan contents. The pulps were bleached to 90 % ISO brightness with the O–DHT–(EP)–D sequence and evaluated for their refinability and drainability. By increasing the alkali concentration in the range of 10–70 g/L pulps of 14.5–5.9 % xylans were produced with no significant impact on cellulose crystallinity. The decrease of xylan content significantly decreased pulp bleaching chemical demand, water retention value and refinability and increased pulp drainability.  相似文献   

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