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Sample records for spme sorbent coatings

  1. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.

    2014-01-01

    In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of

  2. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Zielińska, Katarzyna, E-mail: kzielinska@gmail.com; Leeuwen, Herman P. van

    2014-09-24

    Highlights: • For the first time SPME fiber is coated with polyelectrolyte layer. • Sorption of nanoparticles on the solid phase surface is prevented. • Polyelectrolyte-modified fiber enables extraction of free analyte in presence of sorbing nanoparticles. - Abstract: In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of poly(diallyldimethylammonium chloride), and poly(sodium 4-styrenesulfonate). The modified fiber provides reproducible, convenient and fast extraction capabilities toward the model analyte, triclosan (TCS). A negatively charged polyelectrolyte coating prevents sorbing oxidic nanoparticles from both partitioning into the PDMS phase and aggregation at its surface. The results for the TCS/nanoparticle sample show that the polyelectrolyte layer-modified solid phase extracts just the free form of the organic compound and enables dynamic speciation analysis of the nanoparticulate target analyte complex.

  3. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    International Nuclear Information System (INIS)

    Zielińska, Katarzyna; Leeuwen, Herman P. van

    2014-01-01

    Highlights: • For the first time SPME fiber is coated with polyelectrolyte layer. • Sorption of nanoparticles on the solid phase surface is prevented. • Polyelectrolyte-modified fiber enables extraction of free analyte in presence of sorbing nanoparticles. - Abstract: In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of poly(diallyldimethylammonium chloride), and poly(sodium 4-styrenesulfonate). The modified fiber provides reproducible, convenient and fast extraction capabilities toward the model analyte, triclosan (TCS). A negatively charged polyelectrolyte coating prevents sorbing oxidic nanoparticles from both partitioning into the PDMS phase and aggregation at its surface. The results for the TCS/nanoparticle sample show that the polyelectrolyte layer-modified solid phase extracts just the free form of the organic compound and enables dynamic speciation analysis of the nanoparticulate target analyte complex

  4. Coating membranes for a sorbent-based artificial liver: adsorption characteristics

    NARCIS (Netherlands)

    de Koning, H. W.; Chamuleau, R. A.; Bantjes, A.

    1982-01-01

    Techniques are described for the coating of sorbents to be used in an artificial liver support system based on mixed sorbent bed hemoperfusion. Activated charcoal has been coated with cellulose acetate (CA) by solvent evaporation. With Amberlite XAD-4, the Wurster technique was used for coating with

  5. A preconcentrator chip employing μ-SPME array coated with in-situ-synthesized carbon adsorbent film for VOCs analysis.

    Science.gov (United States)

    Wong, Ming-Yee; Cheng, Wei-Rui; Liu, Mao-Huang; Tian, Wei-Cheng; Lu, Chia-Jung

    2012-11-15

    We report the design, fabrication, and evaluation of a μ-preconcentrator chip that utilizes an array of solid-phase microextraction (SPME) needles coated with in-situ-grown carbon adsorbent film. The structure of the SPME needle (diameter=100 μm, height=250 μm) array inside the sampling chamber was fabricated using a deep reactive-ion etching (DRIE) process to enhance the attachable surface area for adsorbent film. Heaters and temperature sensors were fabricated onto the back of a μ-preconcentrator chip using lithography patterning and a metal lift-off process. The devices were sealed by anodic bonding and diced prior to the application of the adsorbent film. An adsorbent precursor, cellulose was dissolved in water and dynamically coated onto the SPME needle array. The coated cellulose film was converted into a porous carbon film via pyrolysis at 600 °C in a N(2) atmosphere. The surface area of the carbon adsorbent film was 308 m(2)/g, which is higher than that of a commercial adsorbent Carbopack X. A preconcentration factor as high as 13,637-fold was demonstrated using toluene. Eleven volatile organic compounds (VOCs) of different volatilities and functional groups were sampled and analyzed by GC-FID, and the desorption peak widths at half height were all less than 2.6 s after elution from a 15m capillary GC column. There was no sign of performance degradation after continuous operation for 50 cycles in air. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Determination of Pyrethroids in Tea Brew by GC-MS Combined with SPME with Multiwalled Carbon Nanotube Coated Fiber

    Directory of Open Access Journals (Sweden)

    Dongxia Ren

    2018-01-01

    Full Text Available A new method has been developed to simultaneously determine 7 pyrethroid residues in tea brew using gas chromatography-mass spectrometry (GC-MS combined with solid phase microextraction (SPME with multiwalled carbon nanotubes (MWCNTs coated fiber. The MWCNTs coated fiber of SPME was homemade by using stainless steel wire as coating carrier and polyacrylonitrile (PAN solution as adhesive glue. Under the optimized conditions, a good linearity was shown for bifenthrin, fenpropathrin, permethrin, and cyfluthrin in 1–50 ng mL−1 and for cypermethrin, fenvalerate, and deltamethrin in 5–50 ng mL−1. The correlation coefficients were in the range of 0.9948–0.9999. The average recoveries of 7 pyrethroids were 94.2%–107.3% and the relative standard deviations (RSDs were less than 15%. The detection limit of the method ranged from 0.12 to 1.65 ng mL−1. The tea brew samples made from some commercial tea samples were analyzed. Among them, bifenthrin, fenpropathrin, and permethrin were found. The results show that the method is rapid and sensitive and requires low organic reagent consumption, which can be well used for the detection of the pyrethroids in tea brew.

  7. Analysis of Organic Volatile Flavor Compounds in Fermented Stinky Tofu Using SPME with Different Fiber Coatings

    Directory of Open Access Journals (Sweden)

    Wei Guan

    2012-03-01

    Full Text Available The organic volatile flavor compounds in fermented stinky tofu (FST were studied using SPME-GC/MS. A total of 39 volatile compounds were identified, including nine esters, seven alcohols, five alkenes, four sulfides, three heterocycles, three carboxylic acids, three ketones, two aldehydes, one phenol, one amine and one ether. These compounds were determined by MS, and conformed by comparison of the retention times of the separated constituents with those of authentic samples and by comparison of retention indexes (RIs of separated constituents with the RIs reported in the literature. The predominant volatile compound in FST was indole, followed by dimethyl trisulfide, phenol, dimethyl disulfide and dimethyl tetrasulfide. In order to find a better extraction time, the extraction times was optimized for each type of SPME fiber; the results show that the best extraction time for Carboxen/PDMS is 60 min, for PDMS/DVB 30 min, for DVB/CAR/PDMS 60 min and for PDMS 75 min. Of the four fibers used in this work, Carboxen/PDMS is found to be the most suitable to extract the organic volatile flavor compounds in fermented stinky tofu.

  8. Sorbent-coated diffusion denuders for direct measurement of gas/particle partitioning by semi-volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Gundel, L.A. [Lawrence Berkeley National Lab., CA (United States); Lane, D.A. [Atmospheric Environment Service, North York, Ontario (Canada)

    1998-01-01

    Sorbent-coated annular denuder-based samplers have been developed for direct determination of both gaseous and particulate semi-volatile organic species. The first such sampler, the Integrated Organic Vapor/Particle Sampler, has been validated for sampling semi-volatile PAH in ambient air and environmental tobacco smoke. Multi-channel versions of the IOVPS have been used successfully for investigation of gas/particle partitioning of a variety of semi-volatile organic species in combustion source-enriched environmental chambers. Subsequent improvements have resulted in two new higher-capacity samplers, the IOGAPS and the jumbo-IOGAPS, that use the same sorbent for sampling trace organics in the ambient atmosphere for 24--48 hr periods over a wide temperature range. Construction of these new samplers began by incorporating the IOVPS coating technology onto the gas collection surfaces of the higher capacity GAP sampler. Substantial design effort aims to ensure that vapor phase components as volatile as naphthalene can be trapped efficiently and retained by the sorbent-coated surface while the particles pass through to the filter.

  9. Unsuitability of using the DNPH-coated solid sorbent cartridge for determination of airborne unsaturated carbonyls

    Science.gov (United States)

    Ho, Steven Sai Hang; Ho, K. F.; Liu, W. D.; Lee, S. C.; Dai, W. T.; Cao, J. J.; Ip, H. S. S.

    2011-01-01

    Measurements of aldehydes and ketones are typically conducted by derivatization using sorbent cartridges coated with 2,4-dinitrophenylhydrazine (DNPH). The collected samples are eluted with acetonitrile and analyzed by high-pressure liquid chromatography coupled with an ultra-violet detector (HPLC/UV). This paper intends to examine artifacts about its suitability in identification of unsaturated carbonyls. Kinetic tests for acrolein, crotonaldehyde, methacrolein and methyl vinyl ketone (MVK) showed formations of carbonyl-DNP-hydrazone during sampling, which could further react with DNPH, resulting in undesired UV absorption products [e.g., carbonyl-DNP-hydrazone-DNPH (dimer) and 2(carbonyl-DNP-hydrazone)-DNPH (trimer)]. The dimerization and trimerization occurred for acrolein and MVK whereas only dimerization for crotonaldehyde and methacrolein. The polymerization products undoubtedly affect the integrity of the chromatogram, leading to misidentification and inaccurate quantification. Whether precautions taken during sampling and/or sample treatment could avoid or minimize this artifact has not been thoughtfully investigated. More often, such artifacts are usually overlooked by scientists when the data are reported.

  10. Comparison of the atmospheric- and reduced-pressure HS-SPME strategies for analysis of residual solvents in commercial antibiotics using a steel fiber coated with a multiwalled carbon nanotube/polyaniline nanocomposite.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Nouriasl, Kolsoum; Yazdankhah, Fatemeh

    2018-01-01

    A low-cost, sensitive and reliable reduced-pressure headspace solid-phase microextraction (HS-SPME) setup was developed and evaluated for direct extraction of residual solvents in commercial antibiotics, followed by determination by gas chromatography with flame ionization detection (GC-FID). A stainless steel narrow wire was made porous and adhesive by platinization by a modified electrophoretic deposition method and coated with a polyaniline/multiwalled carbon nanotube nanocomposite. All experimental variables affecting the extraction efficiency were investigated for both atmospheric-pressure and reduced-pressure conditions. Comparison of the optimal experimental conditions and the results demonstrated that the reduced-pressure strategy leads to a remarkable increase in the extraction efficiency and reduction of the extraction time and temperature (10 min, 25 °Ϲ vs 20 min, 40 °Ϲ). Additionally, the reduced-pressure strategy showed better analytical performances compared with those obtained by the conventional HS-SPME-GC-FID method. Limit of detections, linear dynamic ranges, and relative standard deviations of the reduced-pressure HS-SPME procedure for benzene, toluene, ethylbenzene, and xylene (BTEX) in injectable solid drugs were obtained over the ranges of 20-100 pg g -1 , 0.02-40 μg g -1 , and 2.8-10.2%, respectively. The procedure developed was successful for the analysis of BTEX in commercial containers of penicillin, ampicillin, ceftriaxone, and cefazolin. Graphical abstract Schematic representation of the developed RP-HS-SPME setup.

  11. Improving the On-Line Extraction of Polar Compounds by IT-SPME with Silica Nanoparticles Modified Phases

    Directory of Open Access Journals (Sweden)

    Pascual Serra-Mora

    2018-02-01

    Full Text Available In the present work the extraction efficiency of in-tube solid-phase microextraction (IT-SPME for polar herbicides has been evaluated using extractive capillaries coated with different polymeric sorbents. For this purpose, aqueous solutions of herbicides with a wide range of polarities, including some highly polar compounds (log Kow < 1, have been directly processed by IT-SPME coupled on-line to capillary liquid chromatography with UV-diode array detection. For extraction, commercially available capillary columns coated with polydimethylsiloxane (PDMS and polyetilenglicol (PEG-based phases have been used, and the results have been compared with those obtained with a synthesized tetraethyl orthosilicate (TEOS-trimethoxyethylsilane (MTEOS polymer, as well as the same polymer reinforced with silica nanoparticles (SiO2 NPs. The SiO2 NPs functionalized TEOS-MTEOS coating provided the best results for most herbicides, especially for the most polar compounds. On the basis of the results obtained, conditions for the quantification of the herbicides tested are described using a SiO2 NPs reinforced TEOS-MTEOS coated capillary. The proposed method provided satisfactory linearity up to concentrations of 200 μg/L. The precision was also suitable, with relative standard deviations (RSDs values ≤9% (n = 3, and the limits of detection (LODs were within the 0.5–7.5 µg/L range. The method has been applied to different water samples and the extract obtained from an agricultural soil.

  12. Preparation of a chitosan-coated C(18)-functionalized magnetite nanoparticle sorbent for extraction of phthalate ester compounds from environmental water samples.

    Science.gov (United States)

    Zhang, Xiao Le; Niu, Hong Yun; Zhang, Sheng Xiao; Cai, Ya Qi

    2010-05-01

    Novel superparamagnetic chitosan-coated C(18)-functionalized magnetite nanoparticles (MNPs) were successfully synthesized and applied as an effective sorbent for the preconcentration of several typical phthalate ester compounds from environmental water samples. The MNPs were 20 nm in diameter and had a high magnetic saturation value (52 emu g(-1)), which endowed the sorbent with a large surface area and the convenience of isolation from water samples. Phthalate esters could be extracted by the interior octadecyl groups through hydrophobic interaction. The hydrophilic porous chitosan polymer coating promoted the dispersion of MNPs in water samples, and improved the anti-interference ability of the sorbent without influencing the adsorption of analytes. The main factors affecting the adsorption of phthalate esters, including the pH of the solution, humic acid, sample loading volume, adsorption time, and desorption conditions, were investigated and optimized. Under the conditions selected (pH 11, adsorption time 20 min, elution with 10 mL of acetonitrile, and concentration to 0.5 mL), concentration factors of 1,000 were achieved by extracting 500 mL of several environmental water samples with 0.1 g of MNP sorbent. The method detection limits obtained for di-n-propyl phthalate, di-n-butyl phthalate, dicyclohexyl phthalate, and di-n-octyl phthalate were 12.3, 18.7, 36.4, and 15.6 ng L(-1), respectively. The recoveries of spiked samples ranged from 60 to 100%, with a low relative standard deviation (1-8%), which indicated good method precision.

  13. Aerogel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Begag, Redouane; Rhine, Wendell E.; Dong, Wenting

    2018-04-03

    The current invention describes methods and compositions of various sorbents based on aerogels of various silanes and their use as sorbent for carbon dioxide. Methods further provide for optimizing the compositions to increase the stability of the sorbents for prolonged use as carbon dioxide capture matrices.

  14. Novel apatite-based sorbent for defluoridation: synthesis and sorption characteristics of nano-micro-crystalline hydroxyapatite-coated-limestone.

    Science.gov (United States)

    Kanno, Cynthia M; Sanders, Rebecca L; Flynn, Steven M; Lessard, Genevieve; Myneni, Satish C B

    2014-05-20

    Elevated levels of fluoride (F(-)) in groundwaters of granitic and basaltic terrains pose a major environmental problem and are affecting millions of people all over the world. Hydroxyapatite (HA) has been shown to be a strong sorbent for F(-); however, low permeability of synthetic HA results in poor sorption efficiency. Here we provide a novel method of synthesizing nano- to micrometer sized HA on the surfaces of granular limestone to improve the sorption efficiency of the HA-based filter. Our experiments with granular limestone (38-63, 125-500 μm) and dissolved PO4(3-) (0.5-5.3 mM) as a function of pH (6-8) and temperature (25-80 °C) indicated rapid formation of nano- to micrometer sized HA crystals on granular limestone with the maximum surface coverage at lower pH and in the presence of multiple additions of aqueous PO4(3-). The HA crystal morphology varied with the above variables. The sorption kinetics and magnitude of F(-) sorption by HA-coated-fine limestone are comparable to those of pure HA, and the F(-) levels dropped to below the World Health Organization's drinking water limit of 79 μM for F(-) concentrations commonly encountered in contaminated potable waters, suggesting that these materials could be used as effective filters. Fluorine XANES spectra of synthetic HA reacted with F(-) suggest that the mode of sorption is through the formation of fluoridated-HA or fluorapatite at low F(-) levels and fluorite at high F(-) loadings.

  15. Monitoring biogenic volatile compounds emitted by Eucalyptus citriodora using SPME.

    Science.gov (United States)

    Zini, C A; Augusto, F; Christensen, T E; Smith, B P; Caramão, E B; Pawliszy, J

    2001-10-01

    A procedure to monitor BVOC emitted by living plants using SPME technique is presented. For this purpose, a glass sampling chamber was designed. This device was employed for the characterization of biogenic volatile compounds emitted by leaves of Eucalyptus citriodora. After extraction with SPME fibers coated with PDMS/ DVB, it was possible to identify or detect 33 compounds emitted by this plant. A semiquantitative approach was applied to monitor the behavior of the emitted BVOC during 9 days. Circadian profiles of the variation in the concentration of isoprene were plotted. Using diffusion-based SPME quantitation, a recently introduced analytical approach, with extraction times as short as 15 s, it was possible to quantify subparts-per-billion amounts of isoprene emitted by this plant.

  16. Novel ion-imprinted polymer coated on nanoporous silica as a highly selective sorbent for the extraction of ultratrace quantities of gold ions from mine stone samples

    International Nuclear Information System (INIS)

    Ebrahimzadeh, H.; Moazzen, E.; Amini, M.; Sadeghi, O.

    2013-01-01

    We have developed a gold ion-imprinted polymer (GIP) by incorporating a dipyridyl ligand into an ethylene glycol dimethacrylate matrix which then was coated onto porous silica particles. The material was used for the selective extraction of ultratrace quantities of gold ion from mine stones, this followed by its quantitation by FAAS. The effects of concentration and volume of eluent, pH of the solution, flow rates of sample and eluent, and effect of potentially interfering ions, especially palladium and platinum, was investigated. The limit of detection is -1 , the precision (RSD%) is 1.03 %, and recoveries are >99 %. In order to show the high selectivity and efficiency of the new sorbent, the results were compared to those obtained with more simple sorbents possessing the same functional groups. The accuracy of the method was demonstrated by the accurate determination of gold ions in a certified reference material. To the best of our knowledge, there is no report so far on an imprint for gold ions that has such a selectivity over Pd(II) and Pt(II) ions. (author)

  17. A method for rapid sampling and characterization of smokeless powder using sorbent-coated wire mesh and direct analysis in real time - mass spectrometry (DART-MS).

    Science.gov (United States)

    Li, Frederick; Tice, Joseph; Musselman, Brian D; Hall, Adam B

    2016-09-01

    Improvised explosive devices (IEDs) are often used by terrorists and criminals to create public panic and destruction, necessitating rapid investigative information. However, backlogs in many forensic laboratories resulting in part from time-consuming GC-MS and LC-MS techniques prevent prompt analytical information. Direct analysis in real time - mass spectrometry (DART-MS) is a promising analytical technique that can address this challenge in the forensic science community by permitting rapid trace analysis of energetic materials. Therefore, we have designed a qualitative analytical approach that utilizes novel sorbent-coated wire mesh and dynamic headspace concentration to permit the generation of information rich chemical attribute signatures (CAS) for trace energetic materials in smokeless powder with DART-MS. Sorbent-coated wire mesh improves the overall efficiency of capturing trace energetic materials in comparison to swabbing or vacuuming. Hodgdon Lil' Gun smokeless powder was used to optimize the dynamic headspace parameters. This method was compared to traditional GC-MS methods and validated using the NIST RM 8107 smokeless powder reference standard. Additives and energetic materials, notably nitroglycerin, were rapidly and efficiently captured by the Carbopack X wire mesh, followed by detection and identification using DART-MS. This approach has demonstrated the capability of generating comparable results with significantly reduced analysis time in comparison to GC-MS. All targeted components that can be detected by GC-MS were detected by DART-MS in less than a minute. Furthermore, DART-MS offers the advantage of detecting targeted analytes that are not amenable to GC-MS. The speed and efficiency associated with both the sample collection technique and DART-MS demonstrate an attractive and viable potential alternative to conventional techniques. Copyright © 2016 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights

  18. Application of Microextraction Techniques Including SPME and MESI to the Thermal Degradation of Polymers: A Review.

    Science.gov (United States)

    Kaykhaii, Massoud; Linford, Matthew R

    2017-03-04

    Here, we discuss the newly developed micro and solventless sample preparation techniques SPME (Solid Phase Microextraction) and MESI (Membrane Extraction with a Sorbent Interface) as applied to the qualitative and quantitative analysis of thermal oxidative degradation products of polymers and their stabilizers. The coupling of these systems to analytical instruments is also described. Our comprehensive literature search revealed that there is no previously published review article on this topic. It is shown that these extraction techniques are valuable sample preparation tools for identifying complex series of degradation products in polymers. In general, the number of products identified by traditional headspace (HS-GC-MS) is much lower than with SPME-GC-MS. MESI is particularly well suited for the detection of non-polar compounds, therefore number of products identified by this technique is not also to the same degree of SPME. Its main advantage, however, is its ability of (semi-) continuous monitoring, but it is more expensive and not yet commercialized.

  19. Rapid and sensitive detection of redspotted grouper nervous necrosis virus (RGNNV) infection by aptamer-coat protein-aptamer sandwich enzyme-linked apta-sorbent assay (ELASA).

    Science.gov (United States)

    Zhou, L; Li, P; Ni, S; Yu, Y; Yang, M; Wei, S; Qin, Q

    2017-12-01

    Redspotted grouper nervous necrosis virus (RGNNV) is one of the most devastating pathogens in the aquaculture of the grouper, Epinephlus sp., worldwide. The early and rapid diagnosis of RGNNV is important for the prevention of RGNNV infection. In this study, an aptamer (A10)-based sandwich enzyme-linked apta-sorbent assay (ELASA) was developed for RGNNV diagnosis. This sandwich ELASA showed high specificity for the RGNNV coat protein (CP) and virions in virus-infected cells and tissues. At the optimized working concentration of 200 nM of aptamer, the ELASA could detect RGNNV in the lysates of as few as 4 × 10 3 RGNNV-infected GB cells. Incubation for 10 min was sufficient to produce accurate results. The sandwich ELASA was most stable at incubation temperatures of 4-25°C, but could still distinguish RGNNV-infected samples from the controls at 37°C. It could detect RGNNV infection in brain lysates diluted 1/10, with results consistent with those of reverse transcription PCR, although with 10% less sensitivity. The main equipment required includes dissection tools, a water bath, Pierce™ Streptavidin Coated Plates and a microplate reader. The sandwich ELASA has great potential utility for the rapid and sensitive diagnosis of RGNNV in its early stages by fish farmers. © 2017 John Wiley & Sons Ltd.

  20. New Functionalized Sol-Gel Hybrid Sorbent Coating for Stir Bar Sorptive Extraction of Selected Non-Steroidal Anti Inflammatory Drugs in Human Urine Samples

    International Nuclear Information System (INIS)

    Mashkurah Abd Rahim; Wan Aini Wan Ibrahim; Zainab Ramli; Mohd Marsin Sanagi

    2015-01-01

    A new sol-gel hybrid material, methyltrimethoxysilane-cyanopropyltriethoxysilane (MTMOS-CNPrTEOS) was successfully synthesized and used as a coating material in stir bar sorptive extraction (SBSE) of selected non-steroidal anti-inflammatory drugs (NSAIDs) in urine samples. The MTMOS-CNPrTEOS hybrid was synthesized by hydrolysis and condensation of MTMOS and CNPrTEOS in the presence of trifluoroacetic acid as catalyst via sol-gel method. Several factors influencing the synthesized sol-gel hybrid MTMOS-CNPrTEOS process such as mole ratio of MTMOS-CNPrTEOS, NaOH concentrations as etching solution, etching time, coating time and water content were investigated and optimized in this study. The optimum synthesis conditions obtained were 1:1 mol ratio of MTMOS-CNPrTEOS, 1 M NaOH as etching solution, 60 min etching time, 2 h coating time and 6 mmol water. The sol-gel hybrid MTMOS-CNPrTEOS synthesized under the optimum conditions was used to determine selected NSAIDs in human urine samples using normal stacking mode capillary electrophoresis with ultraviolet detection. MTMOS-CNPrTEOS SBSE method demonstrated good linearity (60 to 20,000 μg L -1 ) with excellent coefficient of determination (r 2 > 0.9990). The sol-gel hybrid MTMOS-CNPrTEOS SBSE method showed low limit of detection (35 - 41 μg L -1 ) with good precision (RSD < 6 %, n = 3) and excellent extraction recoveries (83.5 - 98.9 %) for the selected NSAIDs. The sol-gel hybrid MTMOS-CNPrTEOS SBSE method demonstrated good potential as an alternative sorbent in SBSE method for NSAIDs. (author)

  1. A platinized stainless steel fiber with in-situ coated polyaniline/polypyrrole/graphene oxide nanocomposite sorbent for headspace solid-phase microextraction of aliphatic aldehydes in rice samples.

    Science.gov (United States)

    Ghiasvand, Alireza; Nasirian, Afagh; Koonani, Samira; Nouriasl, Kolsoum

    2017-12-01

    The surface of a stainless steel fiber was made larger, porous and cohesive by platinizing for tight attachment of its coating. Then it was coated by a polyaniline/polypyrrole/graphene oxide (PANI/PP/GO) nanocomposite film using electrochemical polymerization. The prepared PANI/PP/GO fiber was used for headspace solid-phase microextraction (HS-SPME) of linear aliphatic aldehydes in rice samples followed by GC-FID determination. To achieve the highest extraction efficiency, various experimental parameters including extraction time and temperature, matrix modifier and desorption condition were studied. The linear calibration curves were obtained over the range of 0.05-20 μg g -1 (R 2  > 0.99) for C 4 -C 11 aldehydes. The limits of detection were found to be in the range of 0.01-0.04 μg g -1 . RSD values were calculated to be <7.4 and 10.7% for intra- and inter-day, respectively. The superiority of the prepared nanocomposite SPME fiber was established by comparison of its results with those obtained by polydimethylsiloxane, carbowax-divinylbenzene, divinylbenzene-carboxen-polydimethylsiloxane and polyacrylate commercial ones. Finally, the nanocomposite fiber was used to extract and determine linear aliphatic aldehydes in 18 rice samples. Copyright © 2017 John Wiley & Sons, Ltd.

  2. Carbon coated titanium dioxide nanotubes: synthesis, characterization and potential application as sorbents in dispersive micro solid phase extraction.

    Science.gov (United States)

    García-Valverde, M T; Lucena, R; Galán-Cano, F; Cárdenas, S; Valcárcel, M

    2014-05-23

    In this article, carbon coated titanium dioxide nanotubes (c-TNTs) have been synthesized. The synthesis of the bare TNTs (b-TNTs) using anatase as precursor and their coating with a caramel layer have been performed by simple and cheap hydrothermal processes. The final conversion of the caramel layer in a carbon coating has been accomplished by a thermal treatment (600°C) in an inert (Ar) atmosphere. The c-TNTs have been characterized by different techniques including transmission microscopy, infrared spectroscopy, X-ray powder diffraction, thermogravimetry and Brunauer, Emmett and Teller (BET) adsorption isotherms. The extraction performance of the c-TNTs under a microextraction format has been evaluated and compared with that provided by b-TNTs and multiwalled carbon nanotubes (MWCNTs) using naproxen and ketoprofen as model analytes. c-TNTs provided better results than the other nanoparticles, especially at low acidic pH values. In addition, c-TNTs presented a better dispersibility than MWCNTs, which is very interesting for their use in dispersive micro-solid phase extraction. Finally, a microextraction format, adapted to low sample volumes, has been proposed and applied for the determination of naproxen and ketoprofen in saliva and urine samples by liquid chromatography with UV detection. The results indicate that this approach is promising for the analysis of biological samples. In fact, the recoveries were in the range between 96% and 119% while the precision, expressed as relative standard deviation, was better than 8.5% and 26.3% for urine and saliva, respectively. The detection limits were in the range 34.1-40.8μg/L for saliva samples and 81.1-110μg/L for urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Preparation and characterization of metal-organic framework MIL-101(Cr)-coated solid-phase microextraction fiber.

    Science.gov (United States)

    Xie, Lijun; Liu, Shuqin; Han, Zhubing; Jiang, Ruifen; Liu, Hong; Zhu, Fang; Zeng, Feng; Su, Chengyong; Ouyang, Gangfeng

    2015-01-01

    Metal-organic frameworks (MOFs) have received great attention as novel sorbents due to their fascinating structures and intriguing potential applications in various fields. In this work, a MIL-101(Cr)-coated solid-phase microextraction (SPME) fiber was fabricated by a simple direct coating method and applied to the determination of volatile compounds (BTEX, benzene, toluene, ethylbenzene, m-xylene and o-xylene) and semi-volatile compounds (PAHs, polycyclic aromatic hydrocarbons) from water samples. The extraction and desorption conditions of headspace SPME (HS-SPME) were optimized. Under the optimized conditions, the established methods exhibited excellent extraction performance. Good precision (<7.7%) and low detection limits (0.32-1.7 ng L(-1) and 0.12-2.1 ng L(-1) for BTEX and PAHs, respectively) were achieved. In addition, the MIL-101(Cr)-coated fiber possessed good thermal stability, and the fiber can be reused over 150 times. The fiber was successfully applied to the analysis of BTEX and PAHs in river water by coupling with gas chromatography-mass spectrometry (GC-MS). The analytes at low concentrations (1.7 and 10 ng L(-1)) were detected, and the recoveries obtained with the spiked river water samples were in the range of 80.0-113% and 84.8-106% for BTEX and PAHs, respectively, which demonstrated the applicability of the self-made fiber. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. UPTAKE OF RADIONUCLIDE METALS BY SPME FIBERS

    Energy Technology Data Exchange (ETDEWEB)

    Duff, M; S Crump, S; Robert02 Ray, R; Keisha Martin, K; Donna Beals, D

    2006-08-28

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) and fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of HE and FD residue involves using solid phase microextraction or SPME fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ({sup 239/240}Pu, {sup 238}U, {sup 237}Np, {sup 85}Sr, {sup 133}Ba, {sup 137}Cs, {sup 60}Co and {sup 226}Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Zr, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE and FD residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE and FD residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection.

  5. Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

    Science.gov (United States)

    Yassaa, N.; Custer, T.; Song, W.; Pech, F.; Kesselmeier, J.; Williams, J.

    2010-11-01

    A headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m-2 s-1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

  6. Direct determination of anabolic steroids in pig urine by a new SPME-GC-MS method.

    Science.gov (United States)

    Zhang, Zhuomin; Duan, Hongbin; Zhang, Lan; Chen, Xi; Liu, Wei; Chen, Guonan

    2009-05-15

    A new solid phase microextraction (SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid determination of four anabolic steroids such as 3alpha-hydroxy-5alpha-androstane-17-one (HA), dihydrotestosterone (DHT), androstenedione (AD) and methyltestosterone (MT) in pig urine. SPME was used to extract the four anabolic compounds directly without derivatization. The optimum SPME sampling conditions were based on the home-made carbowax-divinylbenzene (CW-DVB) fiber coating during extraction at 40 degrees C for 50 min with 0.18 g/mL NaCl solution and 750 rpm stirring speed. The linear ranges of the proposed method were in the range of 8-640 pg/mL for HA and DHT and 16-510 pg/mL for AD and MT, respectively. The detection limits (S/N=3) were from 2 to 8 pg/mL for the four anabolic steroids. This SPME method provided very high enrichment factors for the four anabolic steroids, which were 1063-fold and 965-fold for HA and DHT at the concentration of 8 pg/mL and 207-fold and 451-fold for AD and MT at the concentration of 16 pg/mL, respectively. The recoveries ranged from 71.3 to 121%, and the RSDs were lower than 12.9%. The method was sensitive and reliable for determination of trace anabolic steroids in biological samples.

  7. Evaluation of the volatile profile of Tuber liyuanum by HS-SPME with GC-MS.

    Science.gov (United States)

    Liu, Changjiao; Li, Yu

    2017-04-01

    The volatile components of Tuber liyuanum were determined by HS-SPME with GC-MS for the first time. The effects of different fibre coating, extraction time, extraction temperature and sample amount were studied to get optimal extraction conditions. The optimal conditions were SPME fibre of Carboxen/PDMS, extraction time of 40 min, extraction temperature of 80 °C, sample amount of 2 g. Under these conditions 57 compounds in volatile of T. liyuanum were detected with a resemblance percentage above 80%. Aldehydes and aromatics were the main chemical families identified. The contribution of 3-Octanone(11.67%), phenylethyl alcohol (10.60%), isopentana (9.29%) and methylbutana (8.06%) for the total volatile profile were more significant in T. liyuanum than other compounds.

  8. Sorbent Scoping Studies

    Energy Technology Data Exchange (ETDEWEB)

    Chancellor, Christopher John [Los Alamos National Lab. (LANL), Carlsbad, NM (United States). Difficult Waste Team

    2016-11-14

    The Los Alamos National Laboratory–Carlsbad Operations (LANL-CO) office was tasked by the DOE CBFO, Office of the Manager to perform a review of the acceptable knowledge (AK) to identify the oxidizers and sorbents in transuranic (TRU) waste streams, to conduct scoping studies on the oxidizers and sorbents identified in AK review to inform the Quality Level 1 (QL1) testing, and to conduct a series of QL1 tests to provide the scientific data to support a basis of knowledge document for determining the criteria for (1) accepting waste at the Waste Isolation Pilot Plant (WIPP) without treatment, (2) determining waste that will require treatment, and (3) if treatment is required, how the treatment must be performed. The purpose of this report is to present the results of the AK review of sorbents present in active waste streams, provide a technical analysis of the sorbent list, report the results of the scoping studies for the fastest-burning organic sorbent, and provide the list of organic and inorganic sorbents to be used in the development of a Test Plan for Preparation and Testing of Sorbents Mixed with Oxidizer found in Transuranic Waste (DWT-TP-001). The companion report, DWT-RPT-001, Oxidizer Scoping Studies, has similar information for oxidizers identified during the AK review of TRU waste streams. The results of the oxidizer and sorbent scoping studies will be used to inform the QL1 test plan. The QL1 test results will support the development of a basis of knowledge document that will evaluate oxidizing chemicals and sorbents in TRU waste and provide guidance for treatment.

  9. Mercury removal sorbents

    Science.gov (United States)

    Alptekin, Gokhan

    2016-03-29

    Sorbents and methods of using them for removing mercury from flue gases over a wide range of temperatures are disclosed. Sorbent materials of this invention comprise oxy- or hydroxyl-halogen (chlorides and bromides) of manganese, copper and calcium as the active phase for Hg.sup.0 oxidation, and are dispersed on a high surface porous supports. In addition to the powder activated carbons (PACs), this support material can be comprised of commercial ceramic supports such as silica (SiO.sub.2), alumina (Al.sub.2O.sub.3), zeolites and clays. The support material may also comprise of oxides of various metals such as iron, manganese, and calcium. The non-carbon sorbents of the invention can be easily injected into the flue gas and recovered in the Particulate Control Device (PCD) along with the fly ash without altering the properties of the by-product fly ash enabling its use as a cement additive. Sorbent materials of this invention effectively remove both elemental and oxidized forms of mercury from flue gases and can be used at elevated temperatures. The sorbent combines an oxidation catalyst and a sorbent in the same particle to both oxidize the mercury and then immobilize it.

  10. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

    Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

  11. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Israel D.; Melo, Lidervan P. [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Jardim, Isabel C.S.F. [Instituto de Química, Universidade Estadual de Campinas, Campinas, SP (Brazil); Monteiro, Juliana C.S.; Nakano, Ana Marcia S. [Escola de Enfermagem de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Queiroz, Maria Eugênia C., E-mail: mariaeqn@ffclrp.usp.br [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil)

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL{sup −1} (LLOQ) to 400 ng mL{sup −1} with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from −1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. - Highlights: • Molecularly imprinted polymer modified with a hydrophilic external layer (RAM-MIP) was synthesized in a silica capillary. • RAM-MIP capillary, used as sorbent for in-tube SPME, established specific interaction with parabens present in milk samples. • The matrix components that interacted only with the hydrophilic external layer (non-adsorptive network) were excluded.

  12. ADVANCED SORBENT DEVELOPMENT

    Energy Technology Data Exchange (ETDEWEB)

    Javad Abbasian

    2000-01-01

    The overall objective of this program was to develop regenerable sorbents for use in the temperature range of 343 to 538 C (650 to 1000 F) to remove hydrogen sulfide (H{sub 2}S) from coal-derived fuel gases in a fluidized-bed reactor. The goal was to develop sorbents that are capable of reducing the H{sub 2}S level in the fuel gas to less than 20 ppmv in the specified temperature range and pressures in the range of 1 to 20 atmospheres, with chemical characteristics that permit cyclic regeneration over many cycles without a drastic loss of activity, as well as physical, characteristics that are compatible with the fluidized bed application. This topical report focuses on the investigation directed toward preparation of zinc-based sorbents using the sol-gel approach that has been shown to require only a moderate temperature for calcination, while resulting in significantly more attrition-resistant sorbents. The sorbents prepared in this part of the investigation and the results from their evaluation in packed-bed and fluidized-bed reactors are described in this report.

  13. Performance Evaluation of Engineered Structured Sorbents for Atmosphere Revitalization Systems On Board Crewed Space Vehicles and Habitats

    Science.gov (United States)

    Howard, David F.; Perry, Jay L.; Knox, James C.; Junaedi, Christian; Roychoudhury, Subir

    2011-01-01

    Engineered structured (ES) sorbents are being developed to meet the technical challenges of future crewed space exploration missions. ES sorbents offer the inherent performance and safety attributes of zeolite and other physical adsorbents but with greater structural integrity and process control to improve durability and efficiency over packed beds. ES sorbent techniques that are explored include thermally linked and pressure-swing adsorption beds for water-save dehumidification and sorbent-coated metal meshes for residual drying, trace contaminant control, and carbon dioxide control. Results from sub-scale performance evaluations of a thermally linked pressure-swing adsorbent bed and an integrated sub-scale ES sorbent system are discussed.

  14. Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

    Directory of Open Access Journals (Sweden)

    Sybille Merkle

    2015-06-01

    Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

  15. Separation and identification of volatile constituents in Artemisia argyi flowers by GC-MS with SPME and steam distillation.

    Science.gov (United States)

    Li, Ning; Mao, Yu; Deng, Chunhui; Zhang, Xiangmin

    2008-01-01

    Artemisia argyi leaf is a widely used traditional Chinese medicine (TCM). In this work, for the first time, the separation and identification of volatile constituents in Artemisia argyi flowers is performed. Gas chromatography-mass spectrometry (GC-MS) with solid-phase microextraction (SPME) is developed for the fast analysis of volatile constituents in the flowers. Several headspace SPME parameters, including fiber coating, extraction temperature, and extraction time, are optimized. Forty-nine compounds in the flowers are re-identified by SPME-GC-MS. At the same time, in order to compare with the SPME, steam distillation is used for analysis of the volatile constituents in the flowers, and forty-seven are detected. The total fifty-three compounds in the flowers, which mainly include cylcofenchene, alpha-pinene, alpha-myrcene, D-limonene, caryophyllene, and germacrene D, are identified by the two methods. Compared to the volatile components in Artemisia argyi leaves, the main components (including the two active compounds of borneol and borneol acetate) are also found in Artemisia argyi flowers. These results show that Artemisia argyi flowers as well as leaves might be used as TCM.

  16. A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

    Science.gov (United States)

    Hough, Rachael; Archer, Debra; Probert, Christopher

    2018-01-01

    Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

  17. Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1).

    Science.gov (United States)

    Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

    2009-05-30

    A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing.

  18. Sampling atmospheric pesticides with SPME: Laboratory developments and field study

    Energy Technology Data Exchange (ETDEWEB)

    Wang Junxia [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France); Tuduri, Ludovic [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France)], E-mail: l.tuduri@ism.u-bordeaux1.fr; Mercury, Maud [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France); Universites d' Aix-Marseille I, II et III-CNRS UMR 6264: Laboratoire Chimie Provence, Equipe Instrumentation et Reactivite Atmospherique (IRA), Universite de Provence Centre de Saint Jerome, Avenue Escadrille Normandie Niemen, 13397 Marseille Cedex 20 (France); Millet, Maurice [Centre de Geochimie de la Surface UMR 7517 CNRS-Universite Louis Pasteur (ULP), LPCA, 1 rue Blessig, 67084 Strasbourg Cedex (France); Briand, Olivier [AFSSET, 253 avenue du General Leclerc, 94701 Maisons-Alfort Cedex (France); Montury, Michel [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France)

    2009-02-15

    To estimate the atmospheric exposure of the greenhouse workers to pesticides, solid phase microextraction (SPME) was used under non-equilibrium conditions. Using Fick's law of diffusion, the concentrations of pesticides in the greenhouse can be calculated using pre-determined sampling rates (SRs). Thus the sampling rates (SRs) of two modes of SPME in the lab and in the field were determined and compared. The SRs for six pesticides in the lab were 20.4-48.3 mL min{sup -1} for the exposed fiber and 0.166-0.929 mL min{sup -1} for the retracted fiber. In field sampling, two pesticides, dichlorvos and cyprodinil were detected with exposed SPME. SR with exposed SPME for dichlorvos in the field (32.4 mL min{sup -1}) was consistent with that in the lab (34.5 mL min{sup -1}). SR for dichlorvos in the field (32.4 mL min{sup -1}) was consistent with that in the lab (34.5 mL min{sup -1}). The trends of temporal concentration and the inhalation exposure were also obtained. - SPME was proved to be a powerful and simple tool for determining pesticides' atmospheric concentration.

  19. Sampling atmospheric pesticides with SPME: Laboratory developments and field study

    International Nuclear Information System (INIS)

    Wang Junxia; Tuduri, Ludovic; Mercury, Maud; Millet, Maurice; Briand, Olivier; Montury, Michel

    2009-01-01

    To estimate the atmospheric exposure of the greenhouse workers to pesticides, solid phase microextraction (SPME) was used under non-equilibrium conditions. Using Fick's law of diffusion, the concentrations of pesticides in the greenhouse can be calculated using pre-determined sampling rates (SRs). Thus the sampling rates (SRs) of two modes of SPME in the lab and in the field were determined and compared. The SRs for six pesticides in the lab were 20.4-48.3 mL min -1 for the exposed fiber and 0.166-0.929 mL min -1 for the retracted fiber. In field sampling, two pesticides, dichlorvos and cyprodinil were detected with exposed SPME. SR with exposed SPME for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). SR for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). The trends of temporal concentration and the inhalation exposure were also obtained. - SPME was proved to be a powerful and simple tool for determining pesticides' atmospheric concentration

  20. Multiresidue analysis of oestrogenic compounds in cow, goat, sheep and human milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Socas-Rodríguez, Bárbara; Hernández-Borges, Javier; Herrera-Herrera, Antonio V; Rodríguez-Delgado, Miguel Ángel

    2018-03-01

    In this work, the suitability of Fe 3 O 4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d 5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d 5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55-11.8 μg L -1 for all samples. Graphical abstract General scheme of the multiresidue analysis of oestrogenic compounds in milk using core-shell polydopamine coated magnetic nanoparticles as extraction sorbent in μ-dSPE.

  1. Sorbents for mercury removal from flue gas

    Energy Technology Data Exchange (ETDEWEB)

    Granite, Evan J.; Hargis, Richard A.; Pennline, Henry W.

    1998-01-01

    A review of the various promoters and sorbents examined for the removal of mercury from flue gas is presented. Commercial sorbent processes are described along with the chemistry of the various sorbent-mercury interactions. Novel sorbents for removing mercury from flue gas are suggested. Since activated carbons are expensive, alternate sorbents and/or improved activated carbons are needed. Because of their lower cost, sorbent development work can focus on base metal oxides and halides. Additionally, the long-term sequestration of the mercury on the sorbent needs to be addressed. Contacting methods between the flue gas and the sorbent also merit investigation.

  2. Phosphate Adsorption using Modified Iron Oxide-based Sorbents in Lake Water: Kinetics, Equilibrium, and Column Tests

    Science.gov (United States)

    Adsorption behavior of Bayoxide ® E33 (E33) and three E33-modified sorbents for the removal of phosphate from lake water was investigated in this study. E33-modified sorbents were synthesized by coating with manganese (E33/Mn) and silver (E33/AgI and E33/AgII) nanoparticles. Adso...

  3. Analysis of organic micropollutants in drinking water using SPME and GC-MS

    International Nuclear Information System (INIS)

    Guidotti, M.; Ravaioli, G.

    1999-01-01

    In this work the purpose was to develop accurate and reproducible methods for the qualitative and quantitative analysis of pesticides/herbicides, phthalates, chlorinated solvents, trihalomethanes, polycyclic aromatic hydrocarbons (PAHs) and chlorophenols in drinking waters, using solid-phase micro extraction and GC-MS techniques. The SPME developed by J. Pawliszyn and co-workers, consists of an fused silica fibre, coated with an appropriate absorbent phase, hosted inside the needle of a holder that looks like a GC-syringe; the needle pierces the septum of a sealed vial and the fibre is lowered, by depressing the plunger of the holder, into the liquid (or in the headspace, if that is the case) that contains the analytes of interest. After a set period of time, necessary to reach the partitioning equilibrium, the fibre is retracted inside the needle, the needle is inserted into the GC injector port and the fibre pushed in the heated injector. Here the compounds of interest (that have adsorbed onto the fibre) are thermally desorbed and analysed by GC-MS. After three minutes the fibre is extracted and is ready for a new analysis. The SPME technique has already found many applications in food and environmental analysis. Many of the analytes investigated in this research are listed Italian legislation as possible pollutants of drinking waters and their presence and concentrations require monitoring. The list of compounds included in this work is reported in Table 1

  4. Method for sampling and analysis of volatile biomarkers in process gas from aerobic digestion of poultry carcasses using time-weighted average SPME and GC-MS.

    Science.gov (United States)

    Koziel, Jacek A; Nguyen, Lam T; Glanville, Thomas D; Ahn, Heekwon; Frana, Timothy S; Hans van Leeuwen, J

    2017-10-01

    A passive sampling method, using retracted solid-phase microextraction (SPME) - gas chromatography-mass spectrometry and time-weighted averaging, was developed and validated for tracking marker volatile organic compounds (VOCs) emitted during aerobic digestion of biohazardous animal tissue. The retracted SPME configuration protects the fragile fiber from buffeting by the process gas stream, and it requires less equipment and is potentially more biosecure than conventional active sampling methods. VOC concentrations predicted via a model based on Fick's first law of diffusion were within 6.6-12.3% of experimentally controlled values after accounting for VOC adsorption to the SPME fiber housing. Method detection limits for five marker VOCs ranged from 0.70 to 8.44ppbv and were statistically equivalent (p>0.05) to those for active sorbent-tube-based sampling. The sampling time of 30min and fiber retraction of 5mm were found to be optimal for the tissue digestion process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples

    Directory of Open Access Journals (Sweden)

    Pini Gláucia F.

    2004-01-01

    Full Text Available A Headspace Solid Phase Microextraction (HS-SPME procedure for isolation and determination of alkylpyrazines in cocoa liquor, using Gas Chromatography with Flame Ionization Detection (GC-FID for the separation and detection of the analytes, is presented here. The HS-SPME operational conditions were optimized using extractions of samples spiked with known amounts of alkylpyrazines typically found on cocoa products. The maximum extraction efficiency was obtained using SPME fibers coated with 65 µm Carbowax/divinylbenzene. Additionally, the best results were achieved with extraction temperature of 60 ºC, 15 min of sample/headspace equilibration time and 45 min extraction time. It was also observed that suspending the samples in saturated aqueous NaCl solution during extractions resulted in a significant increment on the peak areas. This procedure was found to be effective to determine the so-called pyrazinic ratios (quotient between peak areas of alkylpyrazines, which are useful as quality parameters for cocoa liquor.

  6. Catalyst functionalized buffer sorbent pebbles for rapid separation of carbon dioxide from gas mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Aines, Roger D

    2015-03-31

    A method for separating CO.sub.2 from gas mixtures uses a slurried media impregnated with buffer compounds and coating the solid media with a catalyst or enzyme that promotes the transformation of CO.sub.2 to carbonic acid. Buffer sorbent pebbles with a catalyst or enzyme coating are provided for rapid separation of CO.sub.2 from gas mixtures.

  7. Catalyst functionalized buffer sorbent pebbles for rapid separation of carbon dioxide from gas mixtures

    Science.gov (United States)

    Aines, Roger D.

    2013-03-12

    A method for separating CO.sub.2 from gas mixtures uses a slurried media impregnated with buffer compounds and coating the solid media with a catalyst or enzyme that promotes the transformation of CO.sub.2 to carbonic acid. Buffer sorbent pebbles with a catalyst or enzyme coating are provided for rapid separation of CO.sub.2 from gas mixtures.

  8. Further research on the photo-SPME of triclosan

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Prado, Lucia; Llompart, Maria; Lores, Marta; Fernandez-Alvarez, Maria; Garcia-Jares, Carmen; Cela, Rafael [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia. Facultad de Quimica, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2006-04-15

    In this study the photoinduced degradation of triclosan has been investigated by photo-solid-phase microextraction (photo-SPME). In photo-SPME, photodegradation is carried out on the SPME fibre containing the target compound. Triclosan was extracted from aqueous solutions by use of polydimethylsiloxane SPME fibres and these were subsequently exposed to UV irradiation (power 8 W, wavelength 254 nm) for different times (from 2 to 60 min). The photodegradation kinetics of triclosan were investigated, the photoproducts generated were tentatively identified, and the photochemical behaviour of these products was studied by use of this on-fibre approach followed by gas chromatographic-mass spectrometric analysis. Eight photoproducts were tentatively identified, including chlorinated phenols, chlorohydroxydiphenyl ethers, 2,8-dichlorodibenzo-p-dioxin, and a possible dichlorodibenzodioxin isomer or dichlorohydroxydibenzofuran. The main photodegradation mechanisms were postulated and photodegradation pathways proposed. The effect of pH on triclosan degradation and on triclosan-to-dioxin conversion was also investigated. Triclosan degradation occurred, and generation of 2,8-dichlorodibenzo-p-dioxin was confirmed, throughout the pH range studied (from 3 to 9). (orig.)

  9. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. Black-Right-Pointing-Pointer NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. Black-Right-Pointing-Pointer NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7-4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography-mass spectrometry (GC-MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient

  10. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

    Highlights: ► Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. ► NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. ► NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7–4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography–mass spectrometry (GC–MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient analytical method for the potential study of trace and small molecular

  11. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples.

    Science.gov (United States)

    Souza, Israel D; Melo, Lidervan P; Jardim, Isabel C S F; Monteiro, Juliana C S; Nakano, Ana Marcia S; Queiroz, Maria Eugênia C

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL(-1) (LLOQ) to 400 ng mL(-1) with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from -1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. SO2-Resistant Immobilized Amine Sorbents for CO2 Capture

    Energy Technology Data Exchange (ETDEWEB)

    Tumuluri, Uma [Univ. of Akron, OH (United States)

    2014-01-01

    The solid amine sorbent for CO2 capture process has advantages of simplicity and low operating cost compared to the MEA (monoethanolamine) process. Solid amine sorbents reported so far suffered from either low CO2 capture capacity or low stability in the flue gas environment. This project is aimed at developing a SO2-resistant solid amine sorbent for capturing CO2 from coal–fired power plants with SCR/FGD which emits SO2ranging from 15 to 30 ppm and NO ranging from 5 to 10 ppm. The amine sorbent we developed in a previous project degraded rapidly with 65% decrease in the initial capture capacity in presence of 1% SO2. This amine sorbent was further modified by coating with polyethyleneglycol (PEG) to increase the SO2-resistance. Polyethylene glycol (PEG) was found to decrease the SO2-amine interaction, resulting in the decrease in the maximum SO desorption temperature (Tmax ) of amine sorbent. The PEG-coated amine sorbent exhibited higher stability with only 40% decrease in the initial capture capacity compared to un-coated amine sorbents. The cost of the solid amine sorbent developed in this project is estimated to be less than $7.00/lb; the sorbent exhibited CO2 capture capacity more than 2.3 mmol/g. The results of this study provided the scientific basis for further development of SO2-resistant sorbents.

  13. Sol-gel derived sorbents

    Science.gov (United States)

    Sigman, Michael E.; Dindal, Amy B.

    2003-11-11

    Described is a method for producing copolymerized sol-gel derived sorbent particles for the production of copolymerized sol-gel derived sorbent material. The method for producing copolymerized sol-gel derived sorbent particles comprises adding a basic solution to an aqueous metal alkoxide mixture for a pH.ltoreq.8 to hydrolyze the metal alkoxides. Then, allowing the mixture to react at room temperature for a precalculated period of time for the mixture to undergo an increased in viscosity to obtain a desired pore size and surface area. The copolymerized mixture is then added to an immiscible, nonpolar solvent that has been heated to a sufficient temperature wherein the copolymerized mixture forms a solid upon the addition. The solid is recovered from the mixture, and is ready for use in an active sampling trap or activated for use in a passive sampling trap.

  14. Passive Sampling and Analysis of Naphthalene in Internal Combustion Engine Exhaust with Retracted SPME Device and GC-MS

    Directory of Open Access Journals (Sweden)

    Nassiba Baimatova

    2017-07-01

    Full Text Available Exhaust gases from internal combustion engines are the main source of urban air pollution. Quantification of Polycyclic aromatic hydrocarbons (PAHs in the exhaust gases is needed for emissions monitoring, enforcement, development, and testing of control technologies. The objective was to develop quantification of gaseous naphthalene in diesel engine exhaust based on diffusion-controlled extraction onto a retracted solid-phase microextraction (SPME fiber coating and analysis on gas chromatography-mass spectrometry (GC-MS. Extraction of naphthalene with retracted fibers followed Fick’s law of diffusion. Extracted mass of naphthalene was proportional to Cg, t, Dg, T and inversely proportional to Z. Method detection limit (p = 0.95 was 11.5 ppb (0.06 mg·m−3 at t = 9 h, Z = 10 mm and T = 40 °C, respectively. It was found that the % mass extracted of naphthalene by SPME needle assembly depended on the type of fiber. Storage time at different temperatures did not affect analyte losses extracted by polydimethylsiloxane (PDMS 100 µm fiber. The developed method was tested on exhaust gases from idling pickup truck and tractor, and compared side-by-side with a direct injection of sampled exhaust gas method. Time-weighted average (TWA concentrations of naphthalene in exhaust gases from idling pickup truck and a tractor ranged from 0.08 to 0.3 mg·m−3 (15.3–53.7 ppb.

  15. Ultra trace analysis of PAHs by designing simple injection of large amounts of analytes through the sample reconcentration on SPME fiber after magnetic solid phase extraction.

    Science.gov (United States)

    Khodaee, Nader; Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2016-01-15

    A simple solventless injection method was introduced based on the using of a solid-phase microextraction (SPME) fiber for injection of large amounts of the analytes extracted by the magnetic solid phase extraction (MSPE) procedure. The resulted extract from MSPE procedure was loaded on a G-coated SPME fiber, and then the fiber was injected into the gas chromatography (GC) injection port. This method combines the advantages of exhaustive extraction property of MSPE and the solvent-less injection of SPME to improve the sensitivity of the analysis. In addition, the analytes were re-concentrated prior to inject into the gas chromatography (GC) inlet because of the organic solvent removing from the remaining extract of MSPE technique. Injection of the large amounts of analytes was made possible by using the introduced procedure. Fourteen polycyclic aromatic hydrocarbons (PAHs) with different volatility were used as model compounds to investigate the method performance for volatile and semi-volatile compounds. The introduced method resulted in the higher enhancement factors (5097-59376), lower detection limits (0.29-3.3pgmL(-1)), and higher sensitivity for the semi-volatile compounds compared with the conventional direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Lanthanide Selective Sorbents: Self-Assembled Monolayers on Mesoporous Supports (SAMMS)

    Energy Technology Data Exchange (ETDEWEB)

    Fryxell, Glen E.; Wu, Hong; Lin, Yuehe; Shaw, Wendy J.; Birnbaum, Jerome C.; Linehan, John C.; Nie, Zimin; Kemner, Kenneth M.; Kelly, Shelley

    2004-11-01

    Through the marriage of mesoporous ceramics with self-assembled monolayer chemistry, the genesis of a powerful new class of environmental sorbent materials has been realized. By coating the mesoporous ceramic backbone with a monolayer terminated with a lanthanide-specific ligand, it is possible to couple high lanthanide binding affinity with the high loading capacity (resulting from the extremely high surface area of the support). This lanthanide-specific ligand field is created by pairing a “hard” anionic Lewis base with a suitable synergistic ligand, in a favorable chelating geometry. Details of the synthesis, characterization, lanthanide binding studies, binding kinetics, competition experiments and sorbent regeneration studies are summarized.

  17. HS-SPME-GC-MS Analysis of onion (Allium cepa L. and shallot (Allium ascalonicum L.

    Directory of Open Access Journals (Sweden)

    D’Auria, M.

    2017-06-01

    Full Text Available The volatile organic compounds of onion and shallot were determined via HS-SPME-GC-MS. The main components were dipropyldisulphide and allylpropyldisulphide. Thiopropanal S-oxide were detected only in onion volatiles. In shallot is interesting the presence of 2-methyl-2-pentenal, a compound with an intense fruity aroma, that can characterize the different aroma between onion and shallot. The SPME-GC-MS analysis of shallot after absorption on the SPME fiber at 50°C showed the presence of new compounds, whose structures have been discussed.

  18. New 3D-printed sorbent for extraction of steroids from human plasma preceding LC-MS analysis.

    Science.gov (United States)

    Konieczna, Lucyna; Belka, Mariusz; Okońska, Magdalena; Pyszka, Magdalena; Bączek, Tomasz

    2018-02-21

    In recent years, there has been an increasing worldwide interest in the use of alternative sample preparation methods that are proceeded by separation techniques. Fused deposition modeling (FDM) is a 3D printing technique that is based the consecutive layering of softened/melted thermoplastic materials. In this study, a group of natural steroids and sexual hormones - namely, aldosterone, cortisol, β-estradiol, testosterone, dihydrotestosterone, and synthetic methyltestosterone and betamethasone - were separated and determined using an optimized high-performance liquid chromatography coupled to mass spectrometry (LC-MS) method in positive ionization mode. 3D-printed sorbents were selected as the pre-concentration technique because they are generally low cost, fast, and simple to make and automate. Furthermore, the use of 3D-printed sorbents helps to minimize potential errors due to their repeatability and reproducibility, and their ability to eliminate carry over by using one printed sorbent for a single extraction of steroids from biological matrices. The extraction procedure was optimized and the parameters influencing 3D-printed Layfomm 60 ® based sorbent and LC-MS were studied, including the type of extraction solvent used, sorption and desorption times, temperature, and the salting-out effect. To demonstrate this method's applicability for biological sample analysis, the SPME-LC-MS method was validated for its ability to simultaneously quantify endogenous steroids. This evaluation confirmed good linearity and an R 2 that was between 0.9970 and 0.9990. The recovery rates for human plasma samples were 86.34-93.6% for the studied steroids with intra- and inter-day RSDs of 1.44-7.42% and 1.44-9.46%, respectively. To our knowledge, this study is the first time that 3D-printed sorbents have been used to extract trace amounts of endogenous low-molecular-weight compounds, such as steroids, from biological samples, such as plasma. Copyright © 2018 Elsevier B.V. All

  19. Sorbent Nanotechnologies for Water Cleaning

    Science.gov (United States)

    Ahmed, Snober

    Despite decades of regulatory efforts to mitigate water pollution, many chemicals, particularly heavy metals, still present risks to human health. In addition to direct exposure, certain metals such as mercury threaten public health due to its persistence, bioaccumulation and bioamplification throughout the food chain. A number of U.S. Federal and State regulations have been established to reduce the levels of mercury in water. Activated carbon (AC) has been widely explored for the removal of mercury. However, AC suffers from many limitations inherent to its chemical properties, and it becomes increasingly challenging to meet current and future regulations by simply modifying AC to enhance its performance. Recently, the performance of nanosorbents have been studied in order to removal pollutants. Nanosorbents utilize the ultra-high reactive surface of nanoparticles for rapid, effective and even permanent sequestration of heavy metals from water and air, thus showed promising results as compared to AC. The goal of this thesis research is to develop nanomaterial-based sorbents for the removal of mercury from water. It describes the development of a new solid-support assisted growth of selenium nanoparticles, their use for water remediation, and the development of a new nanoselenium-based sorbent sponge for fast and efficient mercury removal. The nanoselenium sorbent not only shows irreversible interaction with mercury but also exhibits remarkable properties by overcoming the limitations of AC. The nanoselenium sponge was shown to remove mercury to undetectable levels within one minute. This new sponge technology would have an impact on inspiring new stringent regulations and lowering costs to help industries meet regulatory requirements, which will ultimately help improve air and water quality, aquatic life and public health.

  20. Sorbent Structural Impacts Due to Humidity on Carbon Dioxide Removal Sorbents for Advanced Exploration Systems

    Science.gov (United States)

    Watson, David; Knox, James C.; West, Phillip; Stanley, Christine M.; Bush, Richard

    2015-01-01

    The Life Support Systems Project (LSSP) under the Advanced Exploration Systems (AES) program builds upon the work performed under the AES Atmosphere Resource Recovery and Environmental Monitoring (ARREM) project focusing on the numerous technology development areas. The CO2 removal and associated air drying development efforts are focused on improving the current state-of-the-art system on the International Space Station (ISS) utilizing fixed beds of sorbent pellets by seeking more robust pelletized sorbents, evaluating structured sorbents, and examining alternate bed configurations to improve system efficiency and reliability. A component of the CO2 removal effort encompasses structural stability testing of existing and emerging sorbents. Testing will be performed on dry sorbents and sorbents that have been conditioned to three humidity levels. This paper describes the sorbent structural stability screening efforts in support of the LSS Project within the AES Program.

  1. Lanthanide sorbent based on magnetite nanoparticles functionalized with organophosphorus extractants.

    Science.gov (United States)

    Basualto, Carlos; Gaete, José; Molina, Lorena; Valenzuela, Fernando; Yañez, Claudia; Marco, Jose F

    2015-06-01

    In this work, an adsorbent was prepared based on the attachment of organophosphorus acid extractants, namely, D2EHPA, CYANEX 272, and CYANEX 301, to the surface of superparamagnetic magnetite (Fe 3 O 4 ) nanoparticles. The synthesized nanoparticles were coated with oleic acid, first by a chemisorption mechanism and later by the respective extractant via physical adsorption. The obtained core-shell functionalized magnetite nanoparticle composites were characterized by dynamic light scattering, scanning electron microscopy, transmission electron microscopy, thermogravimetry, infrared absorption and vibrating sample magnetometry. All the prepared nanoparticles exhibited a high saturation magnetization capacity that varied between 72 and 46 emu g -1 and decreased as the magnetite nanoparticle was coated with oleic acid and functionalized. The scope of this study also included adsorption tests for lanthanum, cerium, praseodymium, and neodymium and the corresponding analysis of their results. Sorption tests indicated that the functionalized nanoparticles were able to extract the four studied lanthanide metal ions, although the best extraction performance was observed when the sorbent was functionalized with CYANEX 272, which resulted in a loading capacity of approximately 12-14 mg La /g MNP . The magnetization of the synthesized nanoparticles was verified during the separation of the lanthanide-loaded sorbent from the raffinate by using a conventional magnet.

  2. Lanthanide sorbent based on magnetite nanoparticles functionalized with organophosphorus extractants

    Science.gov (United States)

    Basualto, Carlos; Gaete, José; Molina, Lorena; Valenzuela, Fernando; Yañez, Claudia; Marco, Jose F.

    2015-06-01

    In this work, an adsorbent was prepared based on the attachment of organophosphorus acid extractants, namely, D2EHPA, CYANEX 272, and CYANEX 301, to the surface of superparamagnetic magnetite (Fe3O4) nanoparticles. The synthesized nanoparticles were coated with oleic acid, first by a chemisorption mechanism and later by the respective extractant via physical adsorption. The obtained core-shell functionalized magnetite nanoparticle composites were characterized by dynamic light scattering, scanning electron microscopy, transmission electron microscopy, thermogravimetry, infrared absorption and vibrating sample magnetometry. All the prepared nanoparticles exhibited a high saturation magnetization capacity that varied between 72 and 46 emu g-1 and decreased as the magnetite nanoparticle was coated with oleic acid and functionalized. The scope of this study also included adsorption tests for lanthanum, cerium, praseodymium, and neodymium and the corresponding analysis of their results. Sorption tests indicated that the functionalized nanoparticles were able to extract the four studied lanthanide metal ions, although the best extraction performance was observed when the sorbent was functionalized with CYANEX 272, which resulted in a loading capacity of approximately 12-14 mgLa/gMNP. The magnetization of the synthesized nanoparticles was verified during the separation of the lanthanide-loaded sorbent from the raffinate by using a conventional magnet.

  3. Sorbents for the oxidation and removal of mercury

    Science.gov (United States)

    Olson, Edwin S [Grand Forks, ND; Holmes, Michael J [Thompson, ND; Pavlish, John H [East Grand Forks, MN

    2008-10-14

    A promoted activated carbon sorbent is described that is highly effective for the removal of mercury from flue gas streams. The sorbent comprises a new modified carbon form containing reactive forms of halogen and halides. Optional components may be added to increase reactivity and mercury capacity. These may be added directly with the sorbent, or to the flue gas to enhance sorbent performance and/or mercury capture. Mercury removal efficiencies obtained exceed conventional methods. The sorbent can be regenerated and reused. Sorbent treatment and preparation methods are also described. New methods for in-flight preparation, introduction, and control of the active sorbent into the mercury contaminated gas stream are described.

  4. Sorbents for the oxidation and removal of mercur

    Energy Technology Data Exchange (ETDEWEB)

    Olson, Edwin S.; Holmes, Michael J.; Pavlish, John Henry

    2017-09-12

    A promoted activated carbon sorbent is described that is highly effective for the removal of mercury from flue gas streams. The sorbent comprises a new modified carbon form containing reactive forms of halogen and halides. Optional components may be added to increase reactivity and mercury capacity. These may be added directly with the sorbent, or to the flue gas to enhance sorbent performance and/or mercury capture. Mercury removal efficiencies obtained exceed conventional methods. The sorbent can be regenerated and reused. Sorbent treatment and preparation methods are also described. New methods for in-flight preparation, introduction, and control of the active sorbent into the mercury contaminated gas stream are described.

  5. Sorption of methylxanthines by different sorbents

    Science.gov (United States)

    Dmitrienko, S. G.; Andreeva, E. Yu.; Tolmacheva, V. V.; Terent'eva, E. A.

    2013-05-01

    Sorption of caffeine, theophylline, theobromine, diprophylline, and pentoxyphylline on different sorbents (supercross-linked polystyrene, surface-modified copolymer of styrene and divinylbenzene Strata-X, and carbon nanomaterials Taunit and Diasorb-100-C16T) was studied in a static mode in an effort to find new sorbents suitable for sorption isolation and concentration of methylxanthines. The peculiarities of sorption of methylxanthines were explained in relation to the solution acidity, the nature of the sorbates and their concentration, the nature of the solvent, and the structural characteristics of the sorbents.

  6. Research of Oil Product Sorption Processes by Ferromagnetic Sorbents

    OpenAIRE

    Mironovs, Viktors; Treijs, Juris; Teirumnieks, Edmunds

    2015-01-01

    In paper, is given overview of sorbents with ferromagnetic particles. The series of newly designed composite sorbents SOMSOR, are described. Described experiment of oil spill collection from water surface, which comprises of sorbent spreading and collection. Oil sorption by capillary forces, is discussed. Concluded that use of ferromagnetic sorbents a promising direction in the field of water purification from light oil products since it allows expanding the scope of the used powder sorbents,...

  7. JV Task 92 - Alcoa/Retec SFE and SPME

    Energy Technology Data Exchange (ETDEWEB)

    Steven Hawthorne

    2009-02-15

    This report summarizes the work performed by the Energy & Environmental Research Center (EERC) under the U.S. Department of Energy Jointly Sponsored Research Program JV Task 92, which is a continuation of JV9. Successful studies performed in 1999 through the end of 2008 demonstrated the potential for using selective supercritical fluid extraction (SFE) and a solid-phase microextraction (SPME) method for measuring sediment pore water polycyclic aromatic hydrocarbons (PAHs) to mimic the bioavailability of PAHs from manufactured gas plant and aluminum smelter soils and sediments both in freshwater and saltwater locations. The studies that the EERC has performed with the commercial partners have continued to generate increased interest in both the regulatory communities and in the industries that have historically produced or utilized coal tar products. Both ASTM International and the U.S. Environmental Protection Agency (EPA) have accepted the pore water method developed at the EERC as standard methods. The studies have demonstrated the effectiveness of our techniques in predicting bioavailability of PAHs from ca. 250 impacted and background field sediments and soils. The field demonstrations from the final years of the project continued to build the foundation data for acceptance of our methods by the regulatory communities. The JV92 studies provide the single largest database in the world that includes measures of PAH bioavailability along with biological end points. These studies clearly demonstrated that present regulatory paradigms based on equilibrium partitioning greatly overpredict bioavailability. These investigations also laid the foundation for present (non-JV) studies being applied to PAHs and polychlorinated biphenyls (PCBs) at EPA Superfund sites, investigations into PAH and PCB bioavailability at U.S Department of Defense sites, and the application of the techniques to investigating the bioavailability of chlorinated dioxins and furans from impacted

  8. Low-Cost Sorbents: A Literature Summary

    National Research Council Canada - National Science Library

    Bailey, Susan

    1997-01-01

    The capital and regeneration costs of activated carbon and ion exchange media suggest that better process economics may be achieved with disposable sorbents for the treatment of metals-contaminated...

  9. Sol-gel niobia sorbent with a positively charged octadecyl ligand providing enhanced enrichment of nucleotides and organophosphorus pesticides in capillary microextraction for online HPLC analysis.

    Science.gov (United States)

    Kesani, Sheshanka; Malik, Abdul

    2018-04-01

    A niobia-based sol-gel organic-inorganic hybrid sorbent carrying a positively charged C 18 ligand (Nb 2 O 5 -C 18 (+ve)) was synthesized to achieve enhanced enrichment capability in capillary microextraction of organophosphorus compounds (which include organophosphorus pesticides and nucleotides) before their online analysis by high-performance liquid chromatography. The sorbent was designed to simultaneously provide three different types of molecular level interactions: electrostatic, Lewis acid-base, and van der Waals interactions. To understand relative contributions of various molecular level analyte-sorbent interactions in the extraction process, two other sol-gel niobia sorbents were also created: (a) a purely inorganic sol-gel niobia sorbent (Nb 2 O 5 ) and (b) an organic-inorganic hybrid sol-gel niobia sorbent carrying an electrically neutral-bonded octadecyl ligand (Nb 2 O 5 -C 18 ). The extraction efficiency of the created sol-gel niobia sorbent (Nb 2 O 5 -C 18 (+ve)) was compared with that of analogously designed and synthesized titania-based sol-gel sorbent (TiO 2 -C 18 (+ve)), taking into consideration that titania-based sorbents present state-of-the-art extraction media for organophosphorus compounds. In capillary microextraction with high-performance liquid chromatography analysis, Nb 2 O 5 -C 18 (+ve) had shown 40-50% higher specific extraction values (a measure of extraction efficiency) over that of TiO 2 -C 18 (+ve). Compared to TiO 2 -C 18 (+ve), Nb 2 O 5 -C 18 (+ve) also provided superior analyte desorption efficiency (96 vs. 90%) during the online release of the extracted organophosphorus pesticides from the sorbent coating in the capillary microextraction capillary to the chromatographic column using reversed-phase high-performance liquid chromatography mobile phase. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. The antimicrobial efficiency of silver activated sorbents

    Science.gov (United States)

    Đolić, Maja B.; Rajaković-Ognjanović, Vladana N.; Štrbac, Svetlana B.; Rakočević, Zlatko Lj.; Veljović, Đorđe N.; Dimitrijević, Suzana I.; Rajaković, Ljubinka V.

    2015-12-01

    This study is focused on the surface modifications of the materials that are used for antimicrobial water treatment. Sorbents of different origin were activated by Ag+-ions. The selection of the most appropriate materials and the most effective activation agents was done according to the results of the sorption and desorption kinetic studies. Sorption capacities of selected sorbents: granulated activated carbon (GAC), zeolite (Z), and titanium dioxide (T), activated by Ag+-ions were following: 42.06, 13.51 and 17.53 mg/g, respectively. The antimicrobial activity of Ag/Z, Ag/GAC and Ag/T sorbents were tested against Gram-negative bacteria E. coli, Gram-positive bacteria S. aureus and yeast C. albicans. After 15 min of exposure period, the highest cell removal was obtained using Ag/Z against S. aureus and E. coli, 98.8 and 93.5%, respectively. Yeast cell inactivation was unsatisfactory for all three activated sorbents. The antimicrobial pathway of the activated sorbents has been examined by two separate tests - Ag+-ions desorbed from the activated surface to the aqueous phase and microbial cell removal caused by the Ag+-ions from the solid phase (activated surface sites). The results indicated that disinfection process significantly depended on the microbial-activated sites interactions on the modified surface. The chemical state of the activating agent had crucial impact to the inhibition rate. The characterization of the native and modified sorbents was performed by X-ray diffraction technique, X-ray photoelectron spectroscopy and scanning electron microscope. The concentration of adsorbed and released ions was determined by inductively coupled plasma optical emission spectroscopy and mass spectrometry. The antimicrobial efficiency of activated sorbents was related not only to the concentration of the activating agent, but moreover on the surface characteristics of the material, which affects the distribution and the accessibility of the activating agent.

  11. Comparative analysis of the aroma chemicals of Melissa officinalis using hydrodistillation and HS-SPME techniques

    Directory of Open Access Journals (Sweden)

    Shakeel-u- Rehman

    2017-05-01

    Full Text Available Headspace solid-phase micro extraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC–MS has been used for the chemical analysis of Melissa officinalis (leaves cultivated in Institute Germplasm. The HS-SPME analysis led to the identification of 22 components constituting 99.1% of the total volatile constituents present in the leaves whereas its hydrodistillate led to the identification of 24 volatile constituents constituting 98.1% of the volatile material. The chemical composition of the SPME and hydrodistilled extract of M. officinalis leaves comprised mainly of oxygenated monoterpenes (78.5% and 57.8% respectively and sesquiterpene hydrocarbons (14.9% and 29.7% respectively. The major components identified in the HS-SPME extract were citronellal (31.1%, citronellol (18.3%, β-caryophyllene (12.0%, (E-citral (11.9%, (Z-citral (9.6%, geraniol (3.6%, (Z-β-ocimene (3.1% and 1-octen-3-ol (2.0% whereas hydrodistilled essential oil was rich in (Z-citral (19.6%, β-caryophyllene (13.2%, (E-citral (11.2%, citronellal (10.2%, germacrene-d (8.3%, δ-3-carene (5.0%, 6-methyl-5-hepten-2-one (3.7% and citronellyl acetate (3.7%. The comparative analysis of volatile constituents of M. officinalis leaf extract using HS-SPME and hydrodistillation techniques shows both qualitative as well as quantitative differences. The current study is the first report involving rapid analysis of volatile components of M. officinalis by HS-SPME.

  12. A novel method to make regenerable core-shell calcium-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    F.J. Liu; K.S. Chou; Y.K. Huang [National United University, Miao-Li (Taiwan). Department of Chemical Engineering

    2006-04-15

    A sorbent having a calcium oxide core and a clay shell was prepared and shown to be capable of reusable applications in absorption and desorption processes for carbon dioxide. The novelty of this sorbent is that only calcium carbonate and clay are used for its preparation with water as a binder. A two-step granulation procedure is used to get the core and then another step to coat the shell layer with the clay powder. A repeated wet-and-dry procedure probably makes the core porous yet strong enough to serve as a sorbent. The pellet is then calcined at 1200{sup o}C for 2 h to reach its final structure. The core-shell pellets have an overall diameter of 4.4 mm with average shell thickness of 0.45 mm, crush load of 35 N and attrition index of 0.035 wt%/h. These results indicate that the pellets will probably be capable of withstanding the stress in future applications. Carbon dioxide absorption at or below 300{sup o}C showed a maximum weight gain of 38% for our pellets. Finally, desorption in nitrogen at 80{sup o}C can restore the pellet to its original state and hence it is ready for re-use as a sorbent.

  13. Prediction of Partition Coefficients of Organic Compounds for SPME/PDMS

    Directory of Open Access Journals (Sweden)

    Liao Hsuan-Yu

    2016-01-01

    Full Text Available The partition coefficients of 51 organic compounds between SPME/PDMS and gas were compiled from the literature sources in this study. The effect of physicochemical properties and descriptors on the partitioning process of partition coefficients was explicated by the correlation analysis. The PDMS-gas partition coefficients were well correlated to the molecular weight of organic compounds (r = 0.832, p < 0.05. An empirical model, consisting of the molecular weight and the polarizability, was developed to appropriately predict the partition coefficients of organic compounds. The empirical model for estimating the PDMS-gas partition coefficient will contribute to the practical applications of the SPME technique.

  14. Quantitative Determination of Caffeine in Beverages Using a Combined SPME-GC/MS Method

    Science.gov (United States)

    Pawliszyn, Janusz; Yang, Min J.; Orton, Maureen L.

    1997-09-01

    Solid-phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MS) has been applied to the analysis of various caffeinated beverages. Unlike the current methods, this technique is solvent free and requires no pH adjustments. The simplicity of the SPME-GC/MS method lends itself to a good undergraduate laboratory practice. This publication describes the analytical conditions and presents the data for determination of caffeine in coffee, tea, and coke. Quantitation by isotopic dilution is also illustrated.

  15. Solid phase microextraction (SPME) for extraction of volatile oxidation products from complex food systems – Pros and cons

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    efficiency obtained with the SPME method can be affected by different factors such as fiber type, stirring of sample versus not stirring, extraction temperature and time. These factors can easily be controlled and optimized to obtain the highest possible extraction efficiency. However, extraction efficiency...... can also be affected by uncontrollable factors such as batch to batch variation between fibers of the same type and presence of compounds in the sample matrix, which competes with the compounds of interest for adsorption to the SPME fiber. The latter factor is particularly a problem when SPME is used...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  16. Is Solid Phase Microextraction (SPME) an appropriate method for extraction of volatile oxidation products from complex food systems

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    efficiency obtained with the SPME method can be affected by different factors such as fiber type, stirring of sample versus not stirring, extraction temperature and time. These factors can easily be controlled and optimized to obtain the highest possible extraction efficiency. However, extraction efficiency...... can also be affected by uncontrollable factors such as batch to batch variation between fibers of the same type and presence of compounds in the sample matrix, which competes with the compounds of interest for adsorption to the SPME fiber. The latter factor is particularly a problem when SPME is used...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  17. Sorbent Structural Testing on Carbon Dioxide Removal Sorbents for Advanced Exploration Systems

    Science.gov (United States)

    Watson, David; Knox, James C.; West, Phillip; Bush, Richard

    2016-01-01

    Long term space missions require carbon dioxide removal systems that can function with minimal downtime required for maintenance, low power consumption and maximum efficiency for CO2 removal. A major component of such a system are the sorbents used for the CO2 and desiccant beds. Sorbents must not only have adequate CO2 and H2O removal properties, but they must have the mechanical strength to prevent structural breakdown due to pressure and temperature changes during operation and regeneration, as well as resistance to breakdown due to moisture in the system from cabin air. As part of the studies used to select future CO2 sorbent materials, mechanical tests are performed on various zeolite sorbents to determine mechanical performance while dry and at various humidified states. Tests include single pellet crush, bulk crush and attrition tests. We have established a protocol for testing sorbents under dry and humid conditions, and previously tested the sorbents used on the International Space Station carbon dioxide removal assembly. This paper reports on the testing of a series of commercial sorbents considered as candidates for use on future exploration missions.

  18. Encapsulated liquid sorbents for carbon dioxide capture.

    Science.gov (United States)

    Vericella, John J; Baker, Sarah E; Stolaroff, Joshuah K; Duoss, Eric B; Hardin, James O; Lewicki, James; Glogowski, Elizabeth; Floyd, William C; Valdez, Carlos A; Smith, William L; Satcher, Joe H; Bourcier, William L; Spadaccini, Christopher M; Lewis, Jennifer A; Aines, Roger D

    2015-02-05

    Drawbacks of current carbon dioxide capture methods include corrosivity, evaporative losses and fouling. Separating the capture solvent from infrastructure and effluent gases via microencapsulation provides possible solutions to these issues. Here we report carbon capture materials that may enable low-cost and energy-efficient capture of carbon dioxide from flue gas. Polymer microcapsules composed of liquid carbonate cores and highly permeable silicone shells are produced by microfluidic assembly. This motif couples the capacity and selectivity of liquid sorbents with high surface area to facilitate rapid and controlled carbon dioxide uptake and release over repeated cycles. While mass transport across the capsule shell is slightly lower relative to neat liquid sorbents, the surface area enhancement gained via encapsulation provides an order-of-magnitude increase in carbon dioxide absorption rates for a given sorbent mass. The microcapsules are stable under typical industrial operating conditions and may be used in supported packing and fluidized beds for large-scale carbon capture.

  19. Long Life Moving-Bed Zinc Titanate Sorbent

    International Nuclear Information System (INIS)

    Copeland, Robert J.; Cesario, Mike; Feinberg, Daniel A.; Sibold, Jack; Windecker, Brian; Yang, Jing

    1997-01-01

    The objective of this work was to develop and test long-life sorbents for hot gas cleanup. Specifically, we measured the sulfur loading at space velocities typically used for absorption of H 2 S and regenerated the sorbent with diluted air for multiple cycles. Based on the experimental results, we prepared a conceptual design of the sorbent-fabrication system, and estimated the cost of sorbent production and of sulfur removal

  20. Desulfurization Sorbents for Transport-Bed Applications

    International Nuclear Information System (INIS)

    Gupta, Raghubir P.; Turk, Brian S.; Vierheilig, Albert A.

    1997-01-01

    This project extends the prior work on the development of fluidizable zinc titanate particles using a spray-drying technique to impart high reactivity and attrition resistance. The specific objectives are: (1) To develop highly reactive and attrition-resistant zinc titanate sorbents in 40- to 150-(micro)m particle size range for transport reactor applications; (2) To transfer sorbent production technology to private sector; and (3) To provide technical support to Sierra Pacific Clean Coal Technology Demonstration plant and FETC's Hot-Gas Desulfurization Process Development Unit (PDU), both employing a transport reactor system

  1. Alkaline sorbent injection for mercury control

    Science.gov (United States)

    Madden, Deborah A.; Holmes, Michael J.

    2002-01-01

    A mercury removal system for removing mercury from combustion flue gases is provided in which alkaline sorbents at generally extremely low stoichiometric molar ratios of alkaline earth or an alkali metal to sulfur of less than 1.0 are injected into a power plant system at one or more locations to remove at least between about 40% and 60% of the mercury content from combustion flue gases. Small amounts of alkaline sorbents are injected into the flue gas stream at a relatively low rate. A particulate filter is used to remove mercury-containing particles downstream of each injection point used in the power plant system.

  2. Topical Report 5: Sorbent Performance Report

    Energy Technology Data Exchange (ETDEWEB)

    Krutka, Holly; Sjostrom, Sharon

    2011-05-31

    ADA-ES has completed an extensive sorbent screening program funded primarily through DOE NETL cooperative agreement DE-NT0005649 with support from EPRI and industry cost-share participants. Tests were completed on simulated and actual flue gas. The overall project objective is to address the viability and accelerate development of a solid-based postcombustion CO2 capture technology that can be retrofit to the existing fleet of coal-fired power plants. An important component of the viability assessment was to evaluate the state of development of sorbents and measure key performance characteristics under realistic operating conditions.

  3. Silica Modified with Polyaniline as a Potential Sorbent for Matrix Solid Phase Dispersion (MSPD and Dispersive Solid Phase Extraction (d-SPE of Plant Samples

    Directory of Open Access Journals (Sweden)

    Ireneusz Sowa

    2018-03-01

    Full Text Available Polyaniline (PANI is one of the best known conductive polymers with multiple applications. Recently, it was also used in separation techniques, mostly as a component of composites for solid-phase microextraction (SPME. In the present paper, sorbent obtained by in situ polymerization of aniline directly on silica gel particles (Si-PANI was used for dispersive solid phase extraction (d-SPE and matrix solid–phase extraction (MSPD. The efficiency of both techniques was evaluated with the use of high performance liquid chromatography with diode array detection (HPLC-DAD quantitative analysis. The quality of the sorbent was verified by Raman spectroscopy and microscopy combined with automated procedure using computer image analysis. For extraction experiments, triterpenes were chosen as model compounds. The optimal conditions were as follows: protonated Si-PANI impregnated with water, 160/1 sorbent/analyte ratio, 3 min of extraction time, 4 min of desorption time and methanolic solution of ammonia for elution of analytes. The proposed procedure was successfully used for pretreatment of plant samples.

  4. Lanthanide Selective Sorbents: Self-Assembled Monolayers on Mesoporous Supports (SAMMS)

    Energy Technology Data Exchange (ETDEWEB)

    Fryxell, Glen E.; Wu, Hong; Lin, Yuehe; Shaw, Wendy J.; Birnbaum, Jerome C.; Linehan, John C.; Nie, Zimin; Kemner, K. M.; Kelly, Shelley

    2004-11-01

    Through the marriage of mesoporous ceramics with self-assembled monolayer chemistry, the genesis of a powerful new class of environmental sorbent materials has been realized. By coating the mesoporous ceramic backbone with a monolayer terminated with a lanthanide-specific ligand, it is possible to couple high lanthanide binding affinity with the high loading capacity (resulting from the extremely high surface area of the support). This lanthanide-specific ligand field is created by pairing a ''hard'' anionic Lewis base with a suitable synergistic ligand, in a favorable chelating geometry. Details of the synthesis, characterization, lanthanide binding studies, binding kinetics, competition experiments and sorbent regeneration studies are summarized

  5. EVALUATION OF SOLID SORBENTS AS A RETROFIT TECHNOLOGY FOR CO2 CAPTURE FROM COAL-FIRED POWER PLANTS

    Energy Technology Data Exchange (ETDEWEB)

    Holly Krutka; Sharon Sjostrom

    2011-07-31

    field sites. ADA designed and fabricated a slipstream pilot to allow an evaluation of the kinetic behavior of sorbents and provide some flexibility for the physical characteristics of the materials. The design incorporated a transport reactor for the adsorber (co-current reactor) and a fluidized-bed in the regenerator. This combination achieved the sorbent characterization goals and provided an opportunity to evaluate whether the potential cost savings associated with a relatively simple process design could overcome the sacrifices inherent in a co-current separation process. The system was installed at two field sites during the project, Luminant's Martin Lake Steam Electric Station and Xcel Energy's Sherburne County Generating Station (Sherco). Although the system could not maintain continuous 90% CO{sub 2} removal with the sorbents evaluated under this program, it was useful to compare the CO{sub 2} removal properties of several different sorbents on actual flue gas. One of the supported amine materials, sorbent R, was evaluated at both Martin Lake and Sherco. The 1 kWe pilot was operated in continuous mode as well as batch mode. In continuous mode, the sorbent performance could not overcome the limitations of the cocurrent adsorbent design. In batch mode, sorbent R was able to remove up to 90% CO{sub 2} for several cycles. Approximately 50% of the total removal occurred in the first three feet of the adsorption reactor, which was a transport reactor. During continuous testing at Sherco, CO{sub 2} removal decreased to approximately 20% at steady state. The lack of continuous removal was due primarily to the combination of a co-current adsorption system with a fluidized bed for regeneration, a combination which did not provide an adequate driving force to maintain an acceptable working CO{sub 2} capacity. In addition, because sorbent R consisted of a polymeric amine coated on a silica substrate, it was believed that the 50% amine loaded resulted in mass

  6. Method of making ionic liquid mediated sol-gel sorbents

    Science.gov (United States)

    Malik, Abdul; Shearrow, Anne M.

    2017-01-31

    Ionic liquid (IL)-mediated sol-gel hybrid organic-inorganic materials present enormous potential for effective use in analytical microextraction. One obstacle to materializing this prospect arises from high viscosity of ILs significantly slowing down sol-gel reactions. A method was developed which provides phosphonium-based, pyridinium-based, and imidazolium-based IL-mediated advanced sol-gel organic-inorganic hybrid materials for capillary microextraction. Scanning electron microscopy results demonstrate that ILs can serve as porogenic agents in sol-gel reactions. IL-mediated sol-gel coatings prepared with silanol-terminated polymers provided up to 28 times higher extractions compared to analogous sol-gel coatings prepared without any IL in the sol solution. This study shows that IL-generated porous morphology alone is not enough to provide effective extraction media: careful choice of the organic polymer and the precursor with close sol-gel reactivity must be made to ensure effective chemical bonding of the organic polymer to the created sol-gel material to be able to provide the desired sorbent characteristics.

  7. Thermally moderated hollow fiber sorbent modules in rapidly cycled pressure swing adsorption mode for hydrogen purification

    KAUST Repository

    Lively, Ryan P.

    2012-10-01

    We describe thermally moderated multi-layered pseudo-monolithic hollow fiber sorbents entities, which can be packed into compact modules to provide small-footprint, efficient H2 purification/CO2 removal systems for use in on-site steam methane reformer product gas separations. Dual-layer hollow fibers are created via dry-jet, wet-quench spinning with an inner "active" core of cellulose acetate (porous binder) and zeolite NaY (69 wt% zeolite NaY) and an external sheath layer of pure cellulose acetate. The co-spun sheath layer reduces the surface porosity of the fiber and was used as a smooth coating surface for a poly(vinyl-alcohol) post-treatment, which reduced the gas permeance through the fiber sorbent by at least 7 orders of magnitude, essentially creating an impermeable sheath layer. The interstitial volume between the individual fibers was filled with a thermally-moderating paraffin wax. CO2 breakthrough experiments on the hollow fiber sorbent modules with and without paraffin wax revealed that the "passively" cooled paraffin wax module had 12.5% longer breakthrough times than the "non-isothermal" module. The latent heat of fusion/melting of the wax offsets the released latent heat of sorption/desorption of the zeolites. One-hundred rapidly cycled pressure swing adsorption cycles were performed on the "passively" cooled hollow fiber sorbents using 25 vol% CO2/75 vol% He (H2 surrogate) at 60 °C and 113 psia, resulting in a product purity of 99.2% and a product recovery of 88.1% thus achieving process conditions and product quality comparable to conventional pellet processes. Isothermal and non-isothermal dynamic modeling of the hollow fiber sorbent module and a traditional packed bed using gPROMS® indicated that the fiber sorbents have sharper fronts (232% sharper) and longer adsorbate breakthrough times (66% longer), further confirming the applicability of the new fiber sorbent approach for H2 purification. © 2012, Hydrogen Energy Publications, LLC

  8. Carbon dioxide capture process with regenerable sorbents

    Science.gov (United States)

    Pennline, Henry W.; Hoffman, James S.

    2002-05-14

    A process to remove carbon dioxide from a gas stream using a cross-flow, or a moving-bed reactor. In the reactor the gas contacts an active material that is an alkali-metal compound, such as an alkali-metal carbonate, alkali-metal oxide, or alkali-metal hydroxide; or in the alternative, an alkaline-earth metal compound, such as an alkaline-earth metal carbonate, alkaline-earth metal oxide, or alkaline-earth metal hydroxide. The active material can be used by itself or supported on a substrate of carbon, alumina, silica, titania or aluminosilicate. When the active material is an alkali-metal compound, the carbon-dioxide reacts with the metal compound to generate bicarbonate. When the active material is an alkaline-earth metal, the carbon dioxide reacts with the metal compound to generate carbonate. Spent sorbent containing the bicarbonate or carbonate is moved to a second reactor where it is heated or treated with a reducing agent such as, natural gas, methane, carbon monoxide hydrogen, or a synthesis gas comprising of a combination of carbon monoxide and hydrogen. The heat or reducing agent releases carbon dioxide gas and regenerates the active material for use as the sorbent material in the first reactor. New sorbent may be added to the regenerated sorbent prior to subsequent passes in the carbon dioxide removal reactor.

  9. The antimicrobial efficiency of silver activated sorbents

    International Nuclear Information System (INIS)

    Đolić, Maja B.; Rajaković-Ognjanović, Vladana N.; Štrbac, Svetlana B.; Rakočević, Zlatko Lj.; Veljović, Đorđe N.; Dimitrijević, Suzana I.; Rajaković, Ljubinka V.

    2015-01-01

    Highlights: • Different sorbents were activated by Ag + -ions and modified sorbents were determined by sorption capacities, in range of values: 42.06–3.28 mg/g. • Granulated activated carbon (GAC), natural zeolit (Z) and titanium dioxide (T) activated by Ag + -ions were tested against E. coli, S. aureus and C. albicans. • The most successful bacteria removal was obtained using Ag/Z against S. aureus and E. coli, while the yeast cell reduction reached unsatisfactory effect for all three activated sorbents. • XRD, XPS and FE-SEM analysis showed that the chemical state of the silver activating agent affects the antimicrobial activity, as well as the structural properties of the material. • An overall microbial cell reduction, which is performed by separated antimicrobial tests on the Ag + -activated surface and Ag + -ions in aquatic solutions, is a consequence of both mechanisms. - Abstract: This study is focused on the surface modifications of the materials that are used for antimicrobial water treatment. Sorbents of different origin were activated by Ag + -ions. The selection of the most appropriate materials and the most effective activation agents was done according to the results of the sorption and desorption kinetic studies. Sorption capacities of selected sorbents: granulated activated carbon (GAC), zeolite (Z), and titanium dioxide (T), activated by Ag + -ions were following: 42.06, 13.51 and 17.53 mg/g, respectively. The antimicrobial activity of Ag/Z, Ag/GAC and Ag/T sorbents were tested against Gram-negative bacteria E. coli, Gram-positive bacteria S. aureus and yeast C. albicans. After 15 min of exposure period, the highest cell removal was obtained using Ag/Z against S. aureus and E. coli, 98.8 and 93.5%, respectively. Yeast cell inactivation was unsatisfactory for all three activated sorbents. The antimicrobial pathway of the activated sorbents has been examined by two separate tests – Ag + -ions desorbed from the activated surface to the

  10. The antimicrobial efficiency of silver activated sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Đolić, Maja B., E-mail: mirkovic.maja@gmail.com [Vinča Institute of Nuclear Sciences, University of Belgrade, P.O. Box 522, 11001 Belgrade (Serbia); Rajaković-Ognjanović, Vladana N. [Faculty of Civil Engineering, University of Belgrade, Bulevar Kralja Aleksandra 73, 11000 Belgrade (Serbia); Štrbac, Svetlana B. [ICTM-Institute of Electrochemistry, University of Belgrade, Njegoševa 12, 11001 Belgrade (Serbia); Rakočević, Zlatko Lj. [Vinča Institute of Nuclear Sciences, University of Belgrade, P.O. Box 522, 11001 Belgrade (Serbia); Veljović, Đorđe N.; Dimitrijević, Suzana I.; Rajaković, Ljubinka V. [Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11000 Belgrade (Serbia)

    2015-12-01

    Highlights: • Different sorbents were activated by Ag{sup +}-ions and modified sorbents were determined by sorption capacities, in range of values: 42.06–3.28 mg/g. • Granulated activated carbon (GAC), natural zeolit (Z) and titanium dioxide (T) activated by Ag{sup +}-ions were tested against E. coli, S. aureus and C. albicans. • The most successful bacteria removal was obtained using Ag/Z against S. aureus and E. coli, while the yeast cell reduction reached unsatisfactory effect for all three activated sorbents. • XRD, XPS and FE-SEM analysis showed that the chemical state of the silver activating agent affects the antimicrobial activity, as well as the structural properties of the material. • An overall microbial cell reduction, which is performed by separated antimicrobial tests on the Ag{sup +}-activated surface and Ag{sup +}-ions in aquatic solutions, is a consequence of both mechanisms. - Abstract: This study is focused on the surface modifications of the materials that are used for antimicrobial water treatment. Sorbents of different origin were activated by Ag{sup +}-ions. The selection of the most appropriate materials and the most effective activation agents was done according to the results of the sorption and desorption kinetic studies. Sorption capacities of selected sorbents: granulated activated carbon (GAC), zeolite (Z), and titanium dioxide (T), activated by Ag{sup +}-ions were following: 42.06, 13.51 and 17.53 mg/g, respectively. The antimicrobial activity of Ag/Z, Ag/GAC and Ag/T sorbents were tested against Gram-negative bacteria E. coli, Gram-positive bacteria S. aureus and yeast C. albicans. After 15 min of exposure period, the highest cell removal was obtained using Ag/Z against S. aureus and E. coli, 98.8 and 93.5%, respectively. Yeast cell inactivation was unsatisfactory for all three activated sorbents. The antimicrobial pathway of the activated sorbents has been examined by two separate tests – Ag{sup +}-ions desorbed from

  11. Polyetherimide Nanofibres as Sorbents for Organochlorinated Pesticides Determination

    Directory of Open Access Journals (Sweden)

    Antoš Vojtěch

    2016-01-01

    Full Text Available Electrospun polyetherimide (PEI nanofibres were fixed on a steel wire solid phase microextraction (SPME assembly. The basic properties of the prepared nanofibres were determined by thermogravimetry, differential scanning calorimetry, adsorption, and SEM. The analytical performance of prepared PEI SPME fibres was compared with three commercially available SPME fibres, 7 μm PDMS, 100 μm PDMS, and DVB/Carboxene/PDMS. As model water pollutants, persistent organochlorinated pesticides hexachlorocyclohexanes (HCH and chlorobenzene (ClB were chosen as model water pollutants. The fibres were compared in the headspace- (HS- SPME mode of GC-MS/MS instrumentation. The comparison omitted other method parameters and focused exclusively on the extraction time variability. Lab-made PEI SPME fibres showed significantly better response for the target compounds than the other tested fibres from industrial production. Based on the results, the extraction time could be shortened from 50 to 10 min, if PEI SPME fibres were used as a modification of existing analytical protocol.

  12. Comparison of SPME Methods for Determining Volatile Compounds in Milk, Cheese, and Whey Powder

    Directory of Open Access Journals (Sweden)

    Michael H. Tunick

    2013-11-01

    Full Text Available Solid phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but conditions have to be adjusted to maximize release while not generating new compounds that are absent in the original sample. Queso Fresco, a fresh non-melting cheese, may be heated at 60 °C for 30 min; in contrast, compounds are produced in milk when exposed to light and elevated temperatures, so milk samples are heated as little as possible. Products such as dehydrated whey protein are more stable and can be exposed to longer periods (60 min of warming at lower temperature (40 °C without decomposition, allowing for capture and analysis of many minor components. The techniques for determining the volatiles in dairy products by SPME and GC-MS have to be optimized to produce reliable results with minimal modifications and analysis times.

  13. SPME-GC analysis of THC in saliva samples collected with "EPITOPE" device.

    Science.gov (United States)

    Fucci, N; De Giovanni, N; Chiarotti, M; Scarlata, S

    2001-07-15

    In this study we examined the presence of cannabinoids in saliva samples obtained from 24 drug-abusers. The saliva specimens were collected by "EPITOPE" system and the subsequent elution of samples was achieved by centrifugation. The resulting ultrafiltrates have been directly sampled with solid phase micro-extraction (SPME) and then analyzed by GC/MS. Saliva sampling is less invasive than collection of blood.

  14. Layered solid sorbents for carbon dioxide capture

    Science.gov (United States)

    Li, Bingyun; Jiang, Bingbing; Gray, McMahan L; Fauth, Daniel J; Pennline, Henry W; Richards, George A

    2013-02-25

    A solid sorbent for the capture and the transport of carbon dioxide gas is provided having at least one first layer of a positively charged material that is polyethylenimine or poly(allylamine hydrochloride), that captures at least a portion of the gas, and at least one second layer of a negatively charged material that is polystyrenesulfonate or poly(acryclic acid), that transports the gas, wherein the second layer of material is in juxtaposition to, attached to, or crosslinked with the first layer for forming at least one bilayer, and a solid substrate support having a porous surface, wherein one or more of the bilayers is/are deposited on the surface of and/or within the solid substrate. A method of preparing and using the solid sorbent is provided.

  15. SPME as a promising tool in translational medicine and drug discovery: From bench to bedside.

    Science.gov (United States)

    Goryński, Krzysztof; Goryńska, Paulina; Górska, Agnieszka; Harężlak, Tomasz; Jaroch, Alina; Jaroch, Karol; Lendor, Sofia; Skobowiat, Cezary; Bojko, Barbara

    2016-10-25

    Solid phase microextraction (SPME) is a technology where a small amount of an extracting phase dispersed on a solid support is exposed to the sample for a well-defined period of time. The open-bed geometry and biocompatibility of the materials used for manufacturing of the devices makes it very convenient tool for direct extraction from complex biological matrices. The flexibility of the formats permits tailoring the method according the needs of the particular application. Number of studies concerning monitoring of drugs and their metabolites, analysis of metabolome of volatile as well as non-volatile compounds, determination of ligand-protein binding, permeability and compound toxicity was already reported. All these applications were performed in different matrices including biological fluids and tissues, cell cultures, and in living animals. The low invasiveness of in vivo SPME, ability of using very small sample volumes and analysis of cell cultures permits to address the rule of 3R, which is currently acknowledged ethical standard in R&D labs. In the current review systematic evaluation of the applicability of SPME to studies required to be conduct at different stages of drug discovery and development and translational medicine is presented. The advantages and challenges are discussed based on the examples directly showing given experimental design or on the studies, which could be translated to the models routinely used in drug development process. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Analysis of Ethane and Diethylbenzene Bridged Sorbents

    Science.gov (United States)

    2017-12-13

    Textiles modified in this manner have been shown to reduce or eliminate transport of chemical warfare agents and simulants across the fabric barrier...Thermogravimetric Analyzer under a N2 atmosphere ; temperature was ramped 5°C/min to 800°C. This process is used to verify the removal of surfactant from the...without modifications. The pore size distribution was also wider than that of the NRL sorbent and indicated significantly larger pores. The modified

  17. Adsorption of Ammonia on Regenerable Carbon Sorbents

    Science.gov (United States)

    Wójtowicz, Marek A.; Cosgrove, Jesph E.; Serio, Michael A..; Wilburn, Monique

    2015-01-01

    Results are presented on the development of reversible sorbents for the combined carbon dioxide, moisture, and trace-contaminant (TC) removal for use in Extravehicular Activities (EVAs), and more specifically in the Primary Life Support System (PLSS). The currently available life support systems use separate units for carbon dioxide, trace contaminants, and moisture control, and the long-term objective is to replace the above three modules with a single one. Data on sorption and desorption of ammonia, which is a major TC of concern, are presented in this paper. The current TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal, which is non-regenerable, and the carbon-based sorbent under development in this project can be regenerated by exposure to vacuum at room temperature. In this study, several carbon sorbents were fabricated and tested for ammonia sorption. Ammonia-sorption capacity was related to carbon pore structure characteristics, and the temperature of oxidative carbon-surface treatment was optimized for enhanced ammonia-sorption performance.

  18. Sorbents based on carbonized rice peel

    International Nuclear Information System (INIS)

    Mansurova, R. M.; Taipova, R. A.; Zhylybaeva, N. K.; Mansurov, Z. A.; Bijsenbaev, M. A.

    2004-01-01

    The process receiving of sorbents based on carbonized rice peel (RP) was received and their sorption properties were investigated. Processing carbonization of samples leading on station, this was developed in laboratory of hybrid technology. Carbonization of samples was realized in nitric atmosphere on 400-8000 deg. C. On raising temperature of carbonization content of carbon in samples is rice, hydrogen and oxygen is reduce as a result isolation of volatility products is discover. The samples carbonized on 650 deg. C (910 m 2 /g) owners with maximum removed surface is discover. On carbonization temperature 600-800 deh. C the sorption of ions, which carbonized by sorbents based on rice peel is run to 95-100 %. Electron-microscopic investigation of samples leaded on EM-125 mechanism by accelerating pressure 100 kV. From electron-microscopic print of original samples of RP it is evident, that sample consists of carbonic fractions of different species: carbonic fiber of rounded fractions, fractions of ellipsoid form and of more thickly carbonic structure. Increasing sizes of pores and modification structure of synthesized sorbent is occur during carbonization process. The RP-samples, which carbonized by 650 deg. C has the higher specific surface. Samples consist of thin carbonic scum and reducing specific surface, by higher temperature

  19. CO2 Capacity Sorbent Analysis Using Volumetric Measurement Approach

    Science.gov (United States)

    Huang, Roger; Richardson, Tra-My Justine; Belancik, Grace; Jan, Darrell; Knox, Jim

    2017-01-01

    In support of air revitalization system sorbent selection for future space missions, Ames Research Center (ARC) has performed CO2 capacity tests on various solid sorbents to complement structural strength tests conducted at Marshall Space Flight Center (MSFC). The materials of interest are: Grace Davison Grade 544 13X, Honeywell UOP APG III, LiLSX VSA-10, BASF 13X, and Grace Davison Grade 522 5A. CO2 capacity was for all sorbent materials using a Micromeritics ASAP 2020 Physisorption Volumetric Analysis machine to produce 0C, 10C, 25C, 50C, and 75C isotherms. These data are to be used for modeling data and to provide a basis for continued sorbent research. The volumetric analysis method proved to be effective in generating consistent and repeatable data for the 13X sorbents, but the method needs to be refined to tailor to different sorbents.

  20. Advanced sorbent development progam; development of sorbents for moving-bed and fluidized-bed applications

    International Nuclear Information System (INIS)

    Ayala, R.E.; Venkataramani, V.S.

    1998-01-01

    The integrated gasification combined cycle (IGCC) power system using high-temperature coal gas cleanup is one of the most promising advanced technologies for the production of electric power from coal in an environmentally acceptable manner. Unlike conventional low-temperature cleanup systems that require costly heat exchangers, high-temperature coal gas cleanup systems can be operated near 482-538 C (900-1000F) or higher, conditions that are a closer match with the gasifier and turbine components in the IGCC system, thus resulting is a more efficient overall system. GE is developing a moving-bed, high-temperature desulfurization system for the IGCC power cycle in which zinc-based regenerable sorbents are currently being used as desulfurization sorbents. Zinc titanate and other proprietary zinc-based oxides are being considered as sorbents for use in the Clean Coal Technology Demonstration Program at Tampa Electric Co.s (TECo) Polk Power Station. Under cold startup conditions at TECo, desulfurization and regeneration may be carried out at temperatures as low as 343 C (650 F), hence a versatile sorbent is desirable to perform over this wide temperature range. A key to success in the development of high-temperature desulfurization systems is the matching of sorbent properties for the selected process operating conditions, namely, sustainable desulfurization kinetics, high sulfur capacity, and mechanical durability over multiple cycles. Additionally, the sulfur species produced during regeneration of the sorbent must be in a form compatible with sulfur recovery systems, such as sulfuric acid or elemental sulfur processes. The overall objective of this program is to develop regenerable sorbents for hydrogen sulfide removal from coal-derived fuel gases in the temperature range 343-538 C (650-1000 F). Two categories of reactor configurations are being considered: moving-bed reactors and fluidized-bed (bubbling and circulating) reactors. In addition, a cost assessment and

  1. ADVANCED SORBENT DEVELOPMENT PROGRAM DEVELOPMENT OF SORBENTS FOR MOVING-BED AND FLUIDIZED-BED APPLICATIONS

    Energy Technology Data Exchange (ETDEWEB)

    R.E Ayala; V.S. Venkataramani; Javad Abbasian; Rachid B. Slimane; Brett E. Williams; Minoo K. Zarnegar; James R. Wangerow; Andy H. Hill

    2000-03-31

    The integrated gasification combined cycle (IGCC) power system using high-temperature coal gas cleanup is one of the most promising advanced technologies for the production of electric power from coal in an environmentally acceptable manner. Unlike conventional low-temperature cleanup systems that require costly heat exchangers, high-temperature coal gas cleanup systems can be operated near 482-538 C (900-1000 F) or higher, conditions that are a closer match with the gasifier and turbine components in the IGCC system, thus resulting is a more efficient overall system. GE is developing a moving-bed, high-temperature desulfurization system for the IGCC power cycle in which zinc-based regenerable sorbents are currently being used as desulfurization sorbents. Zinc titanate and other proprietary zinc-based oxides are being considered as sorbents for use in the Clean Coal Technology Demonstration Program at Tampa Electric Co.'s (TECo) Polk Power Station. Under cold startup conditions at TECo, desulfurization and regeneration may be carried out at temperatures as low as 343 C (650 F), hence a versatile sorbent is desirable to perform over this wide temperature range. A key to success in the development of high-temperature desulfurization systems is the matching of sorbent properties for the selected process operating conditions, namely, sustainable desulfurization kinetics, high sulfur capacity, and mechanical durability over multiple cycles. Additionally, the sulfur species produced during regeneration of the sorbent must be in a form compatible with sulfur recovery systems, such as sulfuric acid or elemental sulfur processes. The overall objective of this program is to develop regenerable sorbents for hydrogen sulfide removal from coal-derived fuel gases in the temperature range 343-538 C (650-1000 F). Two categories of reactor configurations are being considered: moving-bed reactors and fluidized-bed (bubbling and circulating) reactors. In addition, a cost

  2. Nanostructure conducting molecularly imprinted polypyrrole film as a selective sorbent for benzoate ion and its application in spectrophotometric analysis of beverage samples.

    Science.gov (United States)

    Manbohi, Ahmad; Shamaeli, Ehsan; Alizadeh, Naader

    2014-07-15

    The benzoate anion was selectively extracted by electrochemically controlled solid-phase microextraction (EC-SPME) using a electro-synthesised nanostructure conducting molecularly imprinted polypyrrole (CMIP) film that imprinted for benzoate ions (template ion). The sorbent behaviors of CMIP were characterised using spectrophotometry analysis. The effect of pH, uptake and released times and potentials, template ion concentration, and interference were investigated, and experimental conditions optimised. The film exhibited excellent selectivity in the presence of potential interference from anions including salicylate, sorbate, citrate, phosphate, acetate and chloride ions. The calibration graph was linear (R(2)⩾ 0.993) in the range 1.1 × 10(-5)-5.5 × 10(-4) mol L(-1) and detection limit was 5.2 × 10(-6) mol L(-1). The relative standard deviation was less than 4.5% (n=3). The CMIP film, as a solid-phase micro-extraction absorbent, was applied for the selective clean up and quantification of benzoate in beverage samples using the EC-SPME-spectrophotometric method. The results were in agreement with those obtained using HPLC analysis. This method has a good selectivity and mechanical stability and is disposable simple to construct. However, HPLC method is more selective for determination of benzoate in some food products which have interference compounds such as vanilla and flavoring agents. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. New Methyltrimethoxysilane-(3-Mercaptopropyl)- Trimethoxysilane Coated Hollow Fiber-Solid Phase Micro extraction for Hexanal and Heptanal Analysis

    International Nuclear Information System (INIS)

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

    Determination of volatile organic compounds (VOCs) in various matrices is often accomplished using solid phase micro extraction (SPME) as a superior mode of extraction. Alternatively, another configuration of solid phase micro extraction (SPME) namely hollow fiber-solid phase micro extraction (HF-SPME) is a great approach to redress some limitations of the ordinary SPME fibers including fiber breakage, coating stripping and sample carry over. The HF-SPME technique highlights the use of hollow polypropylene (PP) membrane to hold and protect the adsorbent inside its lumen. Unlike the conventional SPME, the inexpensive HF device can be disposed after single use. Introducing extracting phase via sol-gel technology has gained great interest owing to its simple preparation method and promising way to obtain materials with good characteristics. In the present work, a new hybrid silica material based on methyltrimethoxysilane-(3-mercaptopropyl)trimethoxysilane (MTMOS-MPTMOS) was introduced as a new extractant of HF-SPME and the effectiveness of the proposed method was tested for analysis of hexanal and heptanal as the target VOC analytes. Preparation of the HF-SPME MTMOS-MPTMOS was simple in which the hybrid material was synthesized via sol-gel method and was self-polymerized in small segments of HF. Parameters affecting the efficiency of the HF-SPME MTMOS-MPTMOS in extracting both aldehydes were thoroughly investigated and analyzed by gas chromatography-flame ionization detection (GC-FID). It was found that the highest efficiency was achieved as the extraction was conducted in 30 min at a stirring rate of 1000 rpm in a 10 mL of sample solution whereby the back-extraction was performed via vortex for 3 min using 100 μL methanol as desorption solvent. Under the optimal conditions, linearity was observed over a range of 0.020-10.00 μg mL -1 with detection limits of 0.015 μg mL -1 and 0.010 μg mL -1 for hexanal and heptanal, respectively. The applicability of the HF-SPME

  4. Simple test guidelines for screening oilspill sorbents for toxicity

    International Nuclear Information System (INIS)

    Blenkinsopp, S.A.; Sergy, G.; Doe, K.; Jackman, P.; Huybers, A.

    1998-01-01

    Environment Canada's Emergencies Science Division has established a program to develop a standard test method suitable for evaluating the toxicity of common sorbent materials. Sorbents are used to absorb or adsorb spilled oil and other hazardous materials. They vary widely in composition and packaging. They are often treated with oleophilic and hydrophobic compounds to improve performance and have been used in large quantities during oil spills. Until now, their potential toxicity has never been considered. Three tests have been evaluated to determine how appropriate they are in screening the toxicity of sorbents. Seven toxicity test recommendations for sorbents were presented. 7 refs., 3 tabs., 2 figs

  5. Introduction of coiled solid phase microextraction fiber coated by mesoporous silica/cetyltrimethylammonium bromide for ultra-trace environmental analysis.

    Science.gov (United States)

    Razmi, Habib; Khosrowshahi, Elnaz Marzi; Farrokhzadeh, Samaneh

    2017-07-14

    In this study, a tiny coiled cupper wire as a novel solid phase microextraction (SPME) fiber was coated with mesoporous silica/cetyltrimethylammonium bromide (MCM-41/CTAB) as an adsorbent by electrochemically assisted self-assembly method and used for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) as model analytes prior to chromatographic determination. Deposition of MCM-41/CTAB on the coiled SPME (C-SPME) fiber resulted in easily controlled and reproducible SPME coatings. Non-calcined MCM-41/CTAB on C-SPME plays a key role in the adsorption of PAHs. Under the optimized experimental conditions, low detection limits (36-1220pgL -1 ), and wide linear dynamic ranges (R 2 >0.98) were achieved in the range of 0.25-25,000, 0.12-15,000, 0.56-32,000, 4.1-100,000ngL -1 for phenanthrene, anthracene, fluoranthene and pyrene respectively. The reusability of proposed fiber as well as relative standard deviations for repetitive determination of the target analytes was evaluated. The proposed method was successfully applied for determination of PAHs in several real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C 12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L -1 limit of detections (LOD

  7. Functionalized sorbent for chemical separations and sequential forming process

    Science.gov (United States)

    Fryxell, Glen E [Kennewick, WA; Zemanian, Thomas S [Richland, WA

    2012-03-20

    A highly functionalized sorbent and sequential process for making are disclosed. The sorbent includes organic short-length amino silanes and organic oligomeric polyfunctional amino silanes that are dispersed within pores of a porous support that form a 3-dimensional structure containing highly functionalized active binding sites for sorption of analytes.

  8. Analysis of flavor-related compounds from tabacco using SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Park, G.B.; Lee, S.G. [Korea Research Institute of Chemical Technology, Taejeon (Korea)

    2001-04-01

    The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry (GC-MS). Flavor-related compounds were estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin More than one of the flavor-related compounds were detected in the range of 0.001-1.3 {mu}g/g from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%. (author). 19 refs., 4 tabs., 2 figs.

  9. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS

    DEFF Research Database (Denmark)

    Hansen, Anne-Mette Sølvbjerg; Frandsen, Henrik Lauritz; Fromberg, Arvid

    2015-01-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers the naturalness of a raspberry...... flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. 27 food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry...

  10. Poly(Dimethylsiloxane)-Poly(Vinyl Alcohol) Coated Solid Phase Micro extraction Fiber for Chloropyrifos Analysis

    International Nuclear Information System (INIS)

    Wan Aini Wan Ibrahim; Nor Fairul Zukry Ahmad Rasdy; Norfazilah Muhamad

    2016-01-01

    Traditional liquid - liquid extraction of pesticides consumes large volumes of organic solvent which are hazardous to the operator and is not environment friendly. Solid phase micro extraction (SPME) is a solvent less extraction method which is safer to the operator and is environmental friendly. A sol-gel hybrid fibre coating material, poly(dimethylsiloxane)-poly(vinyl alcohol) (PDMS-PVA) was synthesized and used in head space solid phase micro extraction (HS-SPME) of chloropyrifos. The thickness of the synthesised PDMS-PVA fiber coating was 13.5 μm and it is thermally stable up to 400 degree Celsius. The PDMS-PVA sol-gel hybrid fiber was also stable to two organic solvents tested; acetonitrile and dichloromethane (1 hour dipping) and showed no significant changes in extraction performance for chloropyrifos. Extracted chloropyrifos was analysed using gas chromatography electron capture detector (GC-ECD). Optimum SPME parameters affecting the PDMS-PVA HS-SPME performance namely extraction time (15 min), extraction temperature (50 degree Celsius), desorption time (5 min), desorption temperature (260 degree Celsius) and stirring rate (120 rpm) were used for extraction. It was found that HSSPME using PDMS-PVA sol-gel fiber gave significantly better extraction performance of chloropyrifos compared to commercial 100 μm PDMS fiber. The PDMS-PVA fiber showed excellent operational performances such as temperature stability (up to 380 degree Celsius), coating lifetime (up to 170 times use) and organic solvent stability. The PDMS-PVA-HS-SPME method showed excellent recovery for chloropyrifos from tomatoes (98.0 %, 5.9 % RSD) at 0.01 μg/ g spiked level (5 times lower than maximum residue limit set by European Union). (author)

  11. MQ NMR and SPME analysis of nonlinearity in the degradation of a filled silicone elastomer

    Energy Technology Data Exchange (ETDEWEB)

    Chinn, S C; Alviso, C T; Berman, E S; Harvey, C A; Maxwell, R S; Wilson, T S; Cohenour, R; Saalwachter, K; Chasse, W

    2008-10-10

    Radiation induced degradation of polymeric materials occurs via numerous, simultaneous, competing chemical reactions. Though degradation is typically found to be linear in adsorbed dose, some silicone materials exhibit non-linear dose dependence due to dose dependent dominant degradation pathways. We have characterized the effects of radiative and thermal degradation on a model filled-PDMS system, Sylgard 184 (commonly used as an electronic encapsulant and in biomedical applications), using traditional mechanical testing, NMR spectroscopy, and sample headspace analysis using Solid Phase Micro-Extraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS). The mechanical data and {sup 1}H spin-echo NMR indicated that radiation exposure leads to predominantly crosslinking over the cumulative dose range studies (0 to 250 kGray) with a rate roughly linear with dose. {sup 1}H Multiple Quantum NMR detected a bimodal distribution in the network structure, as expected by the proposed structure of Sylgard 184. The MQ-NMR further indicated that the radiation induced structural changes were not linear in adsorbed dose and competing chain scission mechanisms contribute more largely to the overall degradation process in the range of 50 -100 kGray (though crosslinking still dominates). The SPME-GC/MS data were analyzed using Principal Component Analysis (PCA), which identified subtle changes in the distributions of degradation products (the cyclic siloxanes and other components of the material) as a function of age that provide insight into the dominant degradation pathways at low and high adsorbed dose.

  12. SPME-Based Ca-History Method for Measuring SVOC Diffusion Coefficients in Clothing Material.

    Science.gov (United States)

    Cao, Jianping; Liu, Ningrui; Zhang, Yinping

    2017-08-15

    Clothes play an important role in dermal exposure to indoor semivolatile organic compounds (SVOCs). The diffusion coefficient of SVOCs in clothing material (D m ) is essential for estimating SVOC sorption by clothing material and subsequent dermal exposure to SVOCs. However, few studies have reported the measured D m for clothing materials. In this paper, we present the solid-phase microextraction (SPME) based C a -history method. To the best of our knowledge, this is the first try to measure D m with known relative standard deviation (RSD). A thin sealed chamber is formed by a circular ring and two pieces of flat SVOC source materials that are tightly covered by the targeted clothing materials. D m is obtained by applying an SVOC mass transfer model in the chamber to the history of gas-phase SVOC concentrations (C a ) in the chamber measured by SPME. D m 's of three SVOCs, di-iso-butyl phthalate (DiBP), di-n-butyl phthalate (DnBP), and tris(1-chloro-2-propyl) phosphate (TCPP), in a cotton T-shirt can be obtained within 16 days, with RSD less than 3%. This study should prove useful for measuring SVOC D m in various sink materials. Further studies are expected to facilitate application of this method and investigate the effects of temperature, relative humidity, and clothing material on D m .

  13. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

    Science.gov (United States)

    Musumeci, Lauren E; Ryona, Imelda; Pan, Bruce S; Loscos, Natalia; Feng, Hui; Cleary, Michael T; Sacks, Gavin L

    2015-07-06

    Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  14. New insight on biological interaction analysis: new nanocrystalline mixed metal oxide SPME fiber for GC-FID analysis of BTEX and its application in human hemoglobin-benzene interaction studies.

    Directory of Open Access Journals (Sweden)

    Reza Hosseinzadeh

    Full Text Available Nanocrystalline mixed metal oxides (MMO of various metal cations were synthesized and were used for coating a piece of copper wire as a new high sensitive solid phase micro extraction (SPME fiber in extraction and determination of BTEX compounds from the headspace of aqueous samples prior to GC-FID analysis. Under optimum extraction conditions, the proposed fiber exhibited low detection limits, and quantification limits, good reproducibility, simple and fast preparation method, high fiber capacity and high thermal and mechanical durability. These are some of the most important advantages of the new fiber. The proposed fiber was used for human hemoglobin upon interaction with benzene. Binding isotherm, Scatchard and Klotz logarithmic plots were constructed using HS-SPME-GC data, accurately. The obtained binding isotherm analyzed using Hill method. The Hill parameters have been obtained by calculating saturation parameter from the ratio of measured chromatographic peak areas in the presence and absence of hemoglobin. In this interaction, Hill coefficient and Hill constant determined as (nH = 6.14 and log KH = 6.47 respectively. These results reveal the cooperativity of hemoglobin upon interaction with benzene.

  15. Analysis of enantiomeric and non-enantiomeric monoterpenes in plant emissions using portable dynamic air sampling/solid-phase microextraction (PDAS-SPME) and chiral gas chromatography/mass spectrometry

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

    A portable dynamic air sampler (PDAS) using a porous polymer solid-phase microextraction (SPME) fibre has been validated for the determination of biogenic enantiomeric and non-enantiomeric monoterpenes in air. These compounds were adsorbed in the field, and then thermally desorbed at 250 °C in a gas chromatograph injector port connected via a β-cyclodextrin capillary separating column to a mass spectrometer. The optimized method has been applied for investigating the emissions of enantiomeric monoterpenes from Pseudotsuga menziesii (Douglas-fir), Rosmarinus officinalis (Rosemary) and Lavandula lanata (Lavender) which were selected as representative of coniferous trees and aromatic plants, respectively. The enantiomers of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, β-phellandrene, 4-carene and camphor were successfully determined in the emissions from the three plants. While Douglas-fir showed a strong predominance toward (-)-enantiomers, Rosemary and Lavender demonstrated a large variation in enantiomeric distribution of monoterpenes. The simplicity, rapidity and sensitivity of dynamic sampling with porous polymer coated SPME fibres coupled to chiral capillary gas chromatography/mass spectrometry (GC/MS) makes this method potentially useful for in-field investigations of atmosphere-biosphere interactions and studies of optically explicit atmospheric chemistry.

  16. Development and validation of an SPME-GC method for a degradation kinetics study of propiconazole I, propiconazole II and tebuconazole in blueberries in Concordia, the main production area of Argentina.

    Science.gov (United States)

    Munitz, Martín S; Medina, María B; Montti, María I T

    2017-05-01

    An analytical method for the simultaneous determination of propiconazole isomers and tebuconazole residues in blueberries was developed using solid-phase microextraction (SPME) coupled to gas chromatography. Confirmation was performed by gas chromatography-mass spectrometry in selected-ion monitoring mode. The SPME fibre coating selected was CWX-DVB, and the pH was adjusted to 7 with NaOH. The method is selective with adequate precision and high accuracy and sensitivity. Recoveries ranged between 97.4% and 98.9% for all compounds; and detection and quantification limits were respectively 0.21 and 0.49 μg kg -1 for propiconazole I; 0.16 and 0.22 μg kg -1 for propiconazole II; and 0.16 and 0.48 μg kg -1 for tebuconazole. The degradation of these fungicides in blueberries followed first-order rate kinetics. The half-life times for flowering and fruit set applications were respectively 4.0 and 10.3 days for propiconazole I, 4.0 and 11.4 days for propiconazole II, and 3.5 and 12.4 days for tebuconazole.

  17. Freeze-thaw method improves the detection of volatile compounds in insects using Headspace Solid-Phase Microextraction (HS-SPME)

    Science.gov (United States)

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) is commonly used in analyzing insect volatiles. In order to improve the detection of volatiles in insects, a freeze-thaw method was applied to insect samples before the HS-SPME-GC-MS analysis. ...

  18. In vitro evaluation of new biocompatible coatings for solid-phase microextraction: implications for drug analysis and in vivo sampling applications.

    Science.gov (United States)

    Vuckovic, Dajana; Shirey, Robert; Chen, Yong; Sidisky, Len; Aurand, Craig; Stenerson, Katherine; Pawliszyn, Janusz

    2009-04-13

    A new line of solid-phase microextraction (SPME) coatings suitable for use with liquid chromatography applications was recently developed to address the limitations of the currently available coatings. The proposed coatings were immobilized on the metal fiber core and consisted of a mixture of proprietary biocompatible binder and various types of coated silica (octadecyl, polar embedded and cyano) particles. The aim of this research was to perform in vitro assessment of these new SPME fibers in order to evaluate their suitability for drug analysis and in vivo SPME applications. The main parameters examined were extraction efficiency, solvent resistance, preconditioning, dependence of extraction kinetics on coating thickness, carryover, linear range and inter-fiber reproducibility. The performance of the proposed coatings was compared against commercial Carbowax-TPR (CW-TPR) coating, when applicable. The fibers were evaluated for the extraction of drugs of different classes (carbamazepine, propranolol, pseudoephedrine, ranitidine and diazepam) from plasma and urine. The analyses were performed using liquid chromatography-tandem mass spectrometry. The results show that the fibers perform very well for the extraction of biological fluids with no sample pre-treatment required and can also be used for in vivo sampling applications of flowing blood. A coating thickness of 45 microm was found to be a good compromise between extraction capacity and extraction kinetics. Due to the high extraction efficiency of these coatings, pre-equilibrium SPME with very short extraction times (2 min) can be employed to increase sample throughput. Inter-fiber reproducibility was drugs examined in plasma, which is a significant improvement over polypyrrole coatings reported in literature, and permits single fiber use for in vivo applications.

  19. Sorbent-based Oxygen Production for Energy Systems

    Energy Technology Data Exchange (ETDEWEB)

    Sethi, Vijay [Western Research Inst. (WRI), Laramie, WY (United States)

    2017-01-31

    Project DE-FE0024075 deals with the development of a moderate-temperature sorbent-based oxygen production technology. Sorbent-based oxygen production process utilizes oxygen-storage properties of Perovskites to (1) adsorb oxygen from air in a solid sorbent, and (2) release the adsorbed oxygen into a sweep gas such as CO2 and/or steam for gasification systems or recycled flue gas for oxy-combustion systems. Pure oxygen can be produced by the use of vacuum instead of a sweep gas to affect the pressure swing. By developing more efficient and stable, higher sorption capacity, newer class of materials operating at moderate temperatures this process represents a major advancement in air separation technology. Newly developed perovskite ceramic sorbent materials with order-disorder transition have a higher O2 adsorption capacity, potentially 200 °C lower operating temperatures, and up to two orders of magnitude faster desorption rates than those used in earlier development efforts. The performance advancements afforded by the new materials lead to substantial savings in capital investment and operational costs. Cost of producing oxygen using sorbents could be as much as 26% lower than VPSA and about 13% lower than a large cryogenic air separation unit. Cost advantage against large cryogenic separation is limited because sorbent-based separation numbers up sorbent modules for achieving the larger capacity.

  20. Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

    Science.gov (United States)

    Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

    2016-10-01

    A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

  1. NIFSIL - a composite sorbent for caesium - properties and application

    International Nuclear Information System (INIS)

    Rajec, P.; Orechovska, J.

    1998-01-01

    Samples of the potassium-nickel ferrocyanides K 2 NiFe(CN) 6 , KNi 1,5 Fe(CN) 6 and Ni 2 Fe(CN) 6 were prepared and their properties studied with respect to their use as sorbents for caesium. Caesium is fixed on mixed alkaline-nickel ferrocyanide without structural change. The capacity of Cs retention never reached the theoretic value corresponding to a total release of the monovalent ions of the solid. High distribution coefficients (K D in the order of 10 4 cm 3 /g) determined in batch experiments show that these sorbents have a very high affinity for caesium ions, even in the presence of competing K + , Na + and Ca 2+ ions. The sorbents have a good chemical stability in a wide pH-range (2-12). The irradiation of some sorbent samples with high energy gamma-rays ( 60 Co) of a total dose of 1.10 5 Gy caused no remarkable changes in the sorbent properties (K D , sorption capacity and kinetics, mechanical stability). The sorbents were also tested for 85 Sr and 239 Pu and the results carried out under dynamic and batch experiments have shown that sorbents are not suitable for removal of these radionuclides. Potassium nickel hexacyanoferrate incorporated in silica-gel matrix could compete with others sorbents based on insoluble hexacyanoferrates, has the advantage of good radiation stability and suitable granulometry. The sorbent was prepared on a pilot scale with a capacity about 1000 kg per year with the prospect that it could be easily upgraded to an industrial scale

  2. Evaluation of Solid Sorbents As A Retrofit Technology for CO{sub 2} Capture from Coal-Fired Power Plants

    Energy Technology Data Exchange (ETDEWEB)

    Krutka, Holly; Sjostrom, Sharon

    2011-07-31

    field sites. ADA designed and fabricated a slipstream pilot to allow an evaluation of the kinetic behavior of sorbents and provide some flexibility for the physical characteristics of the materials. The design incorporated a transport reactor for the adsorber (co-current reactor) and a fluidized-bed in the regenerator. This combination achieved the sorbent characterization goals and provided an opportunity to evaluate whether the potential cost savings associated with a relatively simple process design could overcome the sacrifices inherent in a co-current separation process. The system was installed at two field sites during the project, Luminant’s Martin Lake Steam Electric Station and Xcel Energy’s Sherburne County Generating Station (Sherco). Although the system could not maintain continuous 90% CO{sub 2} removal with the sorbents evaluated under this program, it was useful to compare the CO{sub 2} removal properties of several different sorbents on actual flue gas. One of the supported amine materials, sorbent R, was evaluated at both Martin Lake and Sherco. The 1 kWe pilot was operated in continuous mode as well as batch mode. In continuous mode, the sorbent performance could not overcome the limitations of the co-current adsorbent design. In batch mode, sorbent R was able to remove up to 90% CO{sub 2} for several cycles. Approximately 50% of the total removal occurred in the first three feet of the adsorption reactor, which was a transport reactor. During continuous testing at Sherco, CO{sub 2} removal decreased to approximately 20% at steady state. The lack of continuous removal was due primarily to the combination of a co-current adsorption system with a fluidized bed for regeneration, a combination which did not provide an adequate driving force to maintain an acceptable working CO{sub 2} capacity. In addition, because sorbent R consisted of a polymeric amine coated on a silica substrate, it was believed that the 50% amine loaded resulted in mass diffusion

  3. Octahedral molecular sieve sorbents and catalysts

    Science.gov (United States)

    Li, Liyu [Richland, WA; King, David L [Richland, WA

    2010-04-20

    Octahedral molecular sieve sorbents and catalysts are disclosed, including silver hollandite and cryptomelane. These materials can be used, for example, to catalyze the oxidation of CO.sub.x (e.g., CO), NO.sub.x (e.g., NO), hydrocarbons (e.g., C.sub.3H.sub.6) and/or sulfur-containing compounds. The disclosed materials also may be used to catalyze other reactions, such as the reduction of NO.sub.2. In some cases, the disclosed materials are capable of sorbing certain products from the reactions they catalyze. Silver hollandite, in particular, can be used to remove a substantial portion of certain sulfur-containing compounds from a gas or liquid by catalysis and/or sorption. The gas or liquid can be, for example, natural gas or a liquid hydrocarbon.

  4. Sorbent-Based Atmosphere Revitalization System

    Science.gov (United States)

    Knox, James C (Inventor); Miller, Lee A. (Inventor)

    2017-01-01

    The present invention is a sorbent-based atmosphere revitalization (SBAR) system using treatment beds each having a bed housing, primary and secondary moisture adsorbent layers, and a primary carbon dioxide adsorbent layer. Each bed includes a redirecting plenum between moisture adsorbent layers, inlet and outlet ports connected to inlet and outlet valves, respectively, and bypass ports connected to the redirecting plenums. The SBAR system also includes at least one bypass valve connected to the bypass ports. An inlet channel connects inlet valves to an atmosphere source. An outlet channel connects the bypass valve and outlet valves to the atmosphere source. A vacuum channel connects inlet valves, the bypass valve and outlet valves to a vacuum source. In use, one bed treats air from the atmosphere source while another bed undergoes regeneration. During regeneration, the inlet, bypass, and outlet valves sequentially open to the vacuum source, removing accumulated moisture and carbon dioxide.

  5. Evaluation of passive samplers with neutral or ion-exchange polymer coatings to determine freely dissolved concentrations of the basic surfactant lauryl diethanolamine: Measurements of acid dissociation constant and organic carbon-water sorption coefficient.

    Science.gov (United States)

    Wang, Fang; Chen, Yi; Hermens, Joop L M; Droge, Steven T J

    2013-11-08

    A passive sampler tool (solid-phase microextraction, SPME) was optimized to measure freely dissolved concentrations (Cw,free) of lauryl diethanolamine (C12-DEA). C12-DEA can be protonated and act as a cationic surfactant. From the pH-dependent sorption to neutral SPME coatings (polyacrylate and PDMS), a pKa of 8.7 was calculated, which differs more than two units from the value of 6.4 reported elsewhere. Polyacrylate coated SPME could not adequately sample largely protonated C12-DEA in humic acid solutions of pH 6. A new hydrophobic SPME coating with cation-exchange properties (C18/SCX) sorbed C12-DEA 100 fold stronger than polyacrylate, because it specifically sorbs protonated C12-DEA species. The C18/SCX-SPME fiber showed linear calibration isotherms in a concentration range of acid at pH 6 (ionic strength 0.015 M) were measured over a broad concentration range with a sorption coefficient of 10(5.3). Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Metal-organic aerogel as a coating for solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Saraji, Mohammad, E-mail: saraji@cc.iut.ac.ir; Shahvar, Ali

    2017-06-22

    An iron-based metal-organic aerogel was synthesized using metal-organic framework nanoparticles and applied as a fiber coating for solid-phase microextraction (SPME). Chemical, thermal and morphological characteristics of the material were investigated. Headspace SPME followed by gas chromatography-electron capture detection was used for the determination of chlorobenzenes in the environmental samples. The key experimental factors affecting the extraction efficiency of the analytes, such as ionic strength, extraction and desorption temperature, and extraction time were investigated and optimized. The applicability of the coating for the extraction of chlorobenzenes from the environmental samples including river and tap water, sludge, and coastal soil was evaluated. The detection limits were in the range of 0.1–60 ng L{sup −1}. The relative standard deviations were between 2.0 and 5.0%. The extraction recovery of the analytes was in the range of 88–100%. Compared to the commercial PDMS fiber, the present fiber showed better extraction efficiency. - Highlights: • Metal-organic aerogel was synthesized and used as a novel fiber coating for SPME. • The new coating material showed high surface area and good thermal stability. • GC-ECD was used for determination of chlorobenzenes in environmental samples. • The method showed fast extraction and better efficiency than PDMS commercial fiber.

  7. Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC-MS

    NARCIS (Netherlands)

    Kenessov, B.N.; Koziel, J.A.; Grotenhuis, J.T.C.; Carlsen, L.

    2010-01-01

    The paper describes a novel SPME-based approach for sampling and analysis of transformation products of highly reactive and toxic unsymmetrical dimethylhydrazine (UDMH) which is used as a fuel in many Russian, European, Indian, and Chinese heavy cargo carrier rockets. The effects of several

  8. Characterization of Fish Sauce Aroma Impact Compounds Using GC-MS, SPME-Osme-GCO, and Stevens' Power Law Exponents

    Science.gov (United States)

    The objectives of this study were to characterize volatile compounds and to determine the characteristic aromas associated with impact compounds in 4 fish sauces using solid-phase micro-extraction, gas chromatography-mass spectrometry, Osme, and gas chromatography olfactometry (SPME-Osme-GCO) couple...

  9. HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

    Directory of Open Access Journals (Sweden)

    Esmeraldo A. Cappelaro

    2015-03-01

    Full Text Available This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS of dried leaves of Mikania glomerata Sprengel (Asteraceae, also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS, polydimethylsiloxane/divinylbenzene (PDMS/DVB and polyacrylate (PA. Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

  10. Evaluation of 137Cs sorbents for fixation in concrete

    International Nuclear Information System (INIS)

    Plodinec, M.J.

    1976-01-01

    As part of the long-term waste management program at the Savannah River Laboratory, several 137 Cs sorbents were evaluated for incorporation into concrete. The sorbents studied were: Linde AW-300, AW-500, 13-X, and SK-40; Norton Zeolon 200, 500, and 900; clinoptilolite; and vermiculite. The parameters studied were sorption kinetics, leachability, and compressive strength of the concrete. The best sorbents identified were Linde AW-500 and Norton Zeolon 900. In all tests, these two sorbents performed almost identically; sorption kinetics were acceptable; both strengthened the concrete, and both gave relatively leach-resistant concrete. Vermiculite that had been heated to collapse its lattice around 137 Cs gave the most leach-resistant concrete. However, it sorbed cesium slowly, and the resulting concrete was very weak. When silica gel was added to concrete to react with free calcium, the addition had no effect on cesium leachability

  11. Novel Sorbent to Clean Up Biogas for CHPs

    Energy Technology Data Exchange (ETDEWEB)

    Alptekin, Gökhan O. [TDA Research, Incorporated, Wheat Ridge, CO (United States); Jayataman, Ambalavanan [TDA Research, Incorporated, Wheat Ridge, CO (United States); Schaefer, Matthew [TDA Research, Incorporated, Wheat Ridge, CO (United States); Ware, Michael [TDA Research, Incorporated, Wheat Ridge, CO (United States); Hunt, Jennifer [FuelCell Energy, Inc., Danbury, CT (United States); Dobek, Frank [FuelCell Energy, Inc., Danbury, CT (United States)

    2015-05-30

    In this project, TDA Research Inc. (TDA) has developed low-cost (on a per unit volume of gas processed basis), high-capacity expendable sorbents that can remove both the H2S and organic sulfur species in biogas to the ppb levels. The proposed sorbents will operate downstream of a bulk desulfurization system as a polishing bed to provide an essentially sulfur-free gas to a fuel cell (or any other application that needs a completely sulfur-free feed). Our sorbents use a highly dispersed mixed metal oxides active phase with desired modifiers prepared over on a mesoporous support. The support structure allows the large organic sulfur compounds (such as the diethyl sulfide and dipropyl sulfide phases with a large kinetic diameter) to enter the sorbent pores so that they can be adsorbed and removed from the gas stream.

  12. Oil sorbents from plastic wastes and polymers: A review.

    Science.gov (United States)

    Saleem, Junaid; Adil Riaz, Muhammad; Gordon, McKay

    2018-01-05

    A large volume of the waste produced across the world is composed of polymers from plastic wastes such as polyethylene (HDPE or LDPE), polypropylene (PP), and polyethylene terephthalate (PET) amongst others. For years, environmentalists have been looking for various ways to overcome the problems of such large quantities of plastic wastes being disposed of into landfill sites. On the other hand, the usage of synthetic polymers as oil sorbents in particular, polyolefins, including polypropylene (PP) and polyethylene (PE) have been reported. In recent years, the idea of using plastic wastes as the feed for the production of oil sorbents has gained momentum. However, the studies undertaking such feasibility are rather scattered. This review paper is the first of its kind reporting, compiling and reviewing these various processes. The production of an oil sorbent from plastic wastes is being seen to be satisfactorily achievable through a variety of methods Nevertheless, much work needs to be done regarding further investigation of the numerous parameters influencing production yields and sorbent qualities. For example, differences in results are seen due to varying operating conditions, experimental setups, and virgin or waste plastics being used as feeds. The field of producing oil sorbents from plastic wastes is still very open for further research, and seems to be a promising route for both waste reduction, and the synthesis of value-added products such as oil sorbents. In this review, the research related to the production of various oil sorbents based on plastics (plastic waste and virgin polymer) has been discussed. Further oil sorbent efficiency in terms of oil sorption capacity has been described. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Features of sorption process on fibers filled by inorganic sorbents

    International Nuclear Information System (INIS)

    Mikheeva, M.N.; Novikov, Yu.P.; Komarevskiy, V.M.; Myasoedov, B.F.; Mezhirov, M.S.; Idiatulov, R.K.; Fedorova, A.N.

    1986-01-01

    For the extraction of micro components from sea water the fibrous polyacrylonitrile material filled by fine-grained sorbent was proposed. As a sorbent the material on the basis of titanium dioxde was used. The kinetics and thermodynamics of sorption was studied at temperature range 20-65 deg C. According to obtained data the distribution ratio and limiting volumes of fibers at metal sorption from sea water were evaluated.

  14. REMOVAL OF ANIONIC SURFACTANTS FROM WASTEWATER BY MAGNETIC MINERAL SORBENTS

    Directory of Open Access Journals (Sweden)

    Oksana Vladimirova Makarchuk

    2016-07-01

    Full Text Available The simplest and most effective method of removing low concentrations of anionic surfactants such as sodium dodecyl benzenesulfonate (SDBS and sodium lauryl sulfate (SLS is adsorption. Among adsorbents the natural clays are cheap and promising for these purposes. However, there are significant difficulties in removal of spent sorbent after the adsorption process. So, the creation of magnetic sorbents that can be effectively removed from water after sorption by magnetic separation will be a successful decision. The aim of this investigation is the creation of cheap and efficient magnetic sorbents based on natural clays and magnetite for anionic surfactant removal from wastewater. We have synthesized a series of magnetic sorbents from different natural clays with a content of magnetite from 2 to 10 wt%. The ability of magnetic sorbents to remove SDBS and SLS from aqueous solutions has been studied for different adsorbate concentrations by varying the amount of adsorbent, temperature and shaking time. Thermodynamic parameters were calculated from the slope and intercept of the linear plots of ln K against 1/T. Analysis of adsorption results obtained at different temperatures showed that the adsorption pattern on magnetic sorbents correspond to the Langmuir isotherm. It is shown that with increasing the content of magnetite in the magnetic sorbents improves not only their separation from water by magnetic separation, but adsorption capacity to SDBS and SLS. Thus, we obtained of cheap magnetic sorbents based on natural clays and magnetite by the easy way, which not only quickly separated from the solution by magnetic separation, but effectively remove anionic surfactants.

  15. Use of solid phase microextraction (SPME) for profiling the volatile metabolites produced by Glomerella cingulata.

    Science.gov (United States)

    Miyazawa, Mitsuo; Kimura, Minako; Yabe, Yoshito; Tsukamoto, Daisuke; Sakamoto, Masaya; Horibe, Isao; Okuno, Yoshiharu

    2008-01-01

    The profile of volatile organic compounds (VOCs) released from Glomerella cingulata using solid phase microextraction (SPME) with different fibers, Polydimethylsiloxane (PDMS), Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), Carboxen/Polydimethylsiloxane (CAR/PDMS) and Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), was investigated. C4-C6 aliphatic alcohols were the predominant fraction of VOCs isolated by CAR/PDMS fiber. Sesquiterpene hydrocarbons represented 20.3% of VOCs isolated by PDMS fiber. During the growth phase, Ochracin was produced in the large majority of VOCs. 3-Methylbutanol and phenylethyl alcohol were found in the log phase of it. Alcohols were found in cultures of higher age, while sesquiterpenes were found to be characteristic of initial growth stage of G. cingulata.

  16. [Analyze on volatile compounds of Antrodia camphorata using HS-SPME-GC-MS].

    Science.gov (United States)

    He, Zhe; Lu, Zhen-Ming; Xu, Hong-Yu; Shi, Jing-Song; Xu, Zheng-Hong

    2011-11-01

    To analyze the volatile compounds of Antrodia camphorata in solid-state and submerged cultures. A headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry(GC-MS) were used to evaluate the profile of the volatile compounds. 49 volatile compounds were identified in A. camphorata mycelia in submerged culture, while 43 volatile compounds were identified in mycelia in solid-state culture. 1-octen-3-ol, 3-octanone, 1-octen-3-ylacetate, acetic acid octyl ester and ethanol were the main volatile compounds in A. camphorata mycelia in submerged culture, while 1-octen-3-ol, 3-octanone, 3-methyl-butyraldenhyde, gamma-podecalactone and methyl 2-furozte were the most potent key volatile compounds in mycelia in solid-state culture. The volatile compounds in the mycelia of A. camphorata in solid-state and submerged cultures are similar but their relative contents are different.

  17. Engineered sorbent barriers for low-level waste disposal.

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, H.D.; Mitchell, S.J.; Buelt, J.L.

    1986-12-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is investigating sorbent materials to prevent the migration of soluble radio nuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Laboratory studies identifield promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite or clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent and was adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and local soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow-land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 7 refs., 14 figs., 12 tabs.

  18. Engineered sorbent barriers for low-level waste disposal

    International Nuclear Information System (INIS)

    Freeman, H.D.; Mitchell, S.J.; Buelt, J.L.

    1986-12-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is investigating sorbent materials to prevent the migration of soluble radio nuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Laboratory studies identifield promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite or clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent and was adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and local soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow-land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 7 refs., 14 figs., 12 tabs

  19. Engineered sorbent barriers for low-level waste disposal

    International Nuclear Information System (INIS)

    Mitchell, S.J.; Freeman, H.D.; Buelt, J.L.

    1987-01-01

    The Engineered Sorbent Barriers Program at Pacific Northwest Laboratory is developing sorbent materials to prevent the migration of radionuclides from low-level waste sites. These materials would allow water to pass, preventing the bathtub effect at humid sites. Screening studies identified promising sorbent materials for three key radionuclides: for cesium, greensand; for cobalt, activated charcoal; and for strontium, synthetic zeolite of clinoptilolite. Mixtures of these sorbent materials were tested in 0.6-m-diameter columns using radioactive leachates. To simulate expected worst-case conditions, the leachate solution contained the radionuclides, competing cations, and a chelating agent, adjusted to a pH of 5. A sorbent barrier comprised of greensand (1 wt%), activated charcoal (6 wt%), synthetic zeolite (20 wt%), and soil (73 wt%) achieved the decontamination factors necessary to meet the regulatory performance requirements established for this study. Sorbent barriers can be applied to shallow land burial, as backfill around the waste or engineered structures, or as backup to other liner systems. 2 references, 6 figures, 3 tables

  20. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

    Directory of Open Access Journals (Sweden)

    Lauren E. Musumeci

    2015-07-01

    Full Text Available Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH, 3-mercaptohexylacetate (3-MHA, and 4-mercapto-4-methyl-2-pentanone (4-MMP are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS. We describe a method in which thiols are converted to pentafluorobenzyl (PFB derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109% and precision (5%–11% RSD were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines, V. labruscana (Niagara, and Vitis spp. (Cayuga White. Mean 4-MMP concentrations in New York Niagara (17 ng/L were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  1. Novel polystyrene/antibody nanoparticle-coated capillary for immunoaffinity in-tube solid-phase microextraction.

    Science.gov (United States)

    Xu, Bei; Cheng, Shuai; Wang, Xianhua; Wang, Dongmei; Xu, Liang

    2015-04-01

    Antibody-coated polystyrene (PS) nanoparticles (denoted as PS/IgG) were prepared and chemically immobilized for the first time onto a capillary inner wall for immunoaffinity in-tube solid-phase microextraction (SPME) of β2-microglobin (β2MG) and cystatin C (Cys-C). Scanning electron microscopy images of the prepared capillary showed that the nanoparticles were evenly coated onto the capillary inner surface, resulting in the undulating surface of the capillary inner wall. The extraction capacity of the nanoparticle-coated capillary was nearly five times higher than that of a monolayer antibody-immobilized capillary. The in-tube SPME recovery of β2MG (or Cys-C) by the nanoparticle-functionalized capillary was more than 97.8%, whereas that by the monolayer antibody-immobilized tube was 30.5%. In addition, the method quantitation limit obtained by using the nanoparticle-coated capillary was ten times lower than that by the monolayer capillary. Therefore, the capillary coated by PS/IgG nanoparticles is more suitable for immunoaffinity in-tube SPME compared with the commonly used monolayer antibody-immobilized capillary.

  2. New Sorbents for Removing Arsenic From Water

    Science.gov (United States)

    McConchie, D. M.; Genc-Fuhrman, H.; Clark, M. W.; Caldicott, W.; Davies-McConchie, F. G.

    2004-12-01

    Elevated concentrations of arsenic in the drinking water used in many countries, including some of the poorest developing countries, and recognition that consuming this water can have serious consequences for human health, have led to increased investigations of ways to obtain safe water supplies. Finding new groundwater resources is a possible solution but this is a costly strategy that has no guarantee of success, particularly in areas where water is already a scarce commodity. The alternative is to treat water that is already available, but existing technologies are usually too expensive, too difficult to operate and maintain, or not completely effective when used in less developed countries or remote areas. There is therefore, an urgent need to find a simple and effective but inexpensive sorbent for arsenic that can be used to treat large volumes of water under less than ideal conditions. In this paper we present the results of field and laboratory trials that used a new, highly cost-effective, sorbent to remove arsenic from contaminated water. BauxsolT is the name given to the cocktail of minerals prepared by treating caustic bauxite refinery residues with Mg and Ca to produce a substance with a reaction pH of about 8.5, a high acid neutralizing capacity and an excellent ability to trap trace metals, metalloids and some other ionic species. The trapped ions are tightly bound by processes that include; precipitation of low solubility neoformational minerals, isomorphous substitution, solid-state diffusion, and adsorption; it is also an excellent flocculant. Although ordinary BauxsolT has an excellent ability to bind arsenate, and to a lesser extent arsenite, this ability can be further increased for particular water types by using activated BauxsolT or BauxsolT combined with small amounts of other reagents. Field trials conducted at the Gilt Edge Mine, South Dakota, showed that the addition of BauxsolT to highly sulfidic waste rock reduced the arsenic

  3. Steam reactivation of spent CaO-based sorbent for multiple CO2 capture cycles.

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J

    2007-02-15

    This study examines steam reactivation of sorbent to improve the reversibility of multiple CaO-CO2 capture cycles. Experiments to obtain spent sorbent were performed in a tube furnace, and reactivation was achieved using steam in a pressurized reactor. Sorbent activity for CO2 capture was then tested in a thermogravimetric analyzer (TGA), in multi-cycle carbonation tests. After reactivation the sorbent had even better characteristics for CO2 capture than that of the natural sorbent. The average carbonation degree over 10 cycles for the reactivated sorbent approached 70%, significantly higher than for the original sorbent (35-40%). This means that the same sorbent may achieve effective CO2 capture over a large number of cycles, in the absence of other phenomena such as attrition. Partially sulfated sorbents may also be reactivated, but hydration itself is also hindered by sulfation.

  4. Evaluation of Sorbent Injection for Mercury Control

    Energy Technology Data Exchange (ETDEWEB)

    Sharon Sjostrom

    2006-04-30

    The power industry in the U.S. is faced with meeting new regulations to reduce the emissions of mercury compounds from coal-fired plants. These regulations are directed at the existing fleet of nearly 1,100 boilers. These plants are relatively old with an average age of over 40 years. Although most of these units are capable of operating for many additional years, there is a desire to minimize large capital expenditures because of the reduced (and unknown) remaining life of the plant to amortize the project. Injecting a sorbent such as powdered activated carbon into the flue gas represents one of the simplest and most mature approaches to controlling mercury emissions from coal-fired boilers. This is the final site report for tests conducted at DTE Energy's Monroe Power Plant, one of five sites evaluated in this DOE/NETL program. The overall objective of the test program was to evaluate the capabilities of activated carbon injection at five plants: Sunflower Electric's Holcomb Station Unit 1, AmerenUE's Meramec Station Unit 2, Missouri Basin Power Project's Laramie River Station Unit 3, Detroit Edison's Monroe Power Plant Unit 4, and AEP's Conesville Station Unit 6. These plants have configurations that together represent 78% of the existing coal-fired generation plants. The goals for the program established by DOE/NETL were to reduce the uncontrolled mercury emissions by 50 to 70% at a cost 25 to 50% lower than the target established by DOE of $60,000/lb mercury removed. The results from Monroe indicate that using DARCO{reg_sign} Hg would result in higher mercury removal (80%) at a sorbent cost of $18,000/lb mercury, or 70% lower than the benchmark. These results demonstrate that the goals established by DOE/NETL were exceeded during this test program. The increase in mercury removal over baseline conditions is defined for this program as a comparison in the outlet emissions measured using the Ontario Hydro method during the baseline

  5. Novel approach to high-throughput determination of endocrine disruptors using recycled diatomaceous earth as a green sorbent phase for thin-film solid-phase microextraction combined with 96-well plate system.

    Science.gov (United States)

    Kirschner, Nicolas; Dias, Adriana Neves; Budziak, Dilma; da Silveira, Cristian Berto; Merib, Josias; Carasek, Eduardo

    2017-12-15

    A sustainable approach to TF-SPME is presented using recycled diatomaceous earth, obtained from a beer purification process, as a green sorbent phase for the determination of bisphenol A (BPA), benzophenone (BzP), triclocarban (TCC), 4-methylbenzylidene camphor (4-MBC) and 2-ethylhexyl-p-methoxycinnamate (EHMC) in environmental water samples. TF-SPME was combined with a 96-well plate system allowing for high-throughput analysis due to the simultaneous extraction/desorption up to 96 samples. The proposed sorbent phase exhibited good stability in organic solvents, as well as satisfactory analytical performance. The optimized method consisted of 240 min of extraction at pH 6 with the addition of NaCl (15% w/v). A mixture of MeOH:ACN (50:50 v/v) was used for the desorption the analytes, using a time of 30 min. Limits of detection varied from 1 μg L -1 for BzP and TCC to 8 μg L -1 for the other analytes, and R 2 ranged from 0.9926 for 4-MBC to 0.9988 for BPA. This novel and straightforward approach offers an environmentally-friendly and very promising alternative for routine analysis. . The total sample preparation time per sample was approximately 2.8 min, which is a significant advantage when a large number of analytical run is required. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Aminosilane-Functionalized Hollow Fiber Sorbents for Post-Combustion CO 2 Capture

    KAUST Repository

    Li, Fuyue Stephanie

    2013-07-03

    Increasing carbon dioxide emissions are generally believed to contribute to global warming. Developing new materials for capturing CO2 emitted from coal-fired plants can potentially mitigate the effect of these CO 2 emissions. In this study, we developed and optimized porous hollow fiber sorbents with both improved sorption capacities and rapid sorption kinetics by functionalizing aminosilane (N-(2-aminoethyl)-3- aminoisobutyldimethylmethoxysilane) to cellulose acetate hollow fibers as a "proof of concept". A lumen-side barrier layer was also developed in the aminosilane-functionalized cellulose acetate fiber sorbent to allow for facile heat exchange without significant mass transfer with the bore-side heat transfer fluid. The functionalized cellulose acetate fiber sorbents were characterized by pressure decay sorption measurements, multicomponent column chromatography, FT-IR, elemental analysis, and scanning electron microscopy. The carbon dioxide sorption capacity at 1 atm is 0.73 mmol/g by using the pressure decay apparatus. Multicomponent column chromatography measurements showed that aminosilane functionalized cellulose acetate fiber sorbent has a CO2 sorption capacity of 0.23 mmol/g at CO2 partial pressure 0.1 atm and 35 C in simulated flue gas. While this capacity is low, our proof of concept positions the technology to move forward to higher capacity with work that is underway. The presence of silicon and nitrogen elements in the elemental analysis confirmed the success of grafting along with FT-IR spectra which showed the absorbance peak (∼810 cm-1) for Si-C stretching. A cross-linked Neoprene material was used to form the lumen-side barrier layer. Preliminary data showed the required reduction in gas permeance to eliminate mixing between shell side and bore side fluid flows. Specifically the permeance was reduced from 10 000 GPUs for the neat fibers to 6.6 ± 0.1 and 3.3 ± 0.3 GPUs for the coated fibers. The selected lumen layer formation materials

  7. Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kazemi, Elahe; Haji Shabani, Ali Mohammad [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Dadfarnia, Shayessteh, E-mail: sdadfarnia@yazd.ac.ir [Department of Chemistry, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Abbasi, Amir [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of); Rashidian Vaziri, Mohammad Reza [Laser and Optics Research School, 14155-1339, Tehran (Iran, Islamic Republic of); Behjat, Abbas [Department of Physics, Yazd University, Safaieh, 89195-741, Yazd (Iran, Islamic Republic of)

    2016-01-28

    dispersive micro solid phase extraction is developed for the separation and preconcentration of trace amounts of fluoxetine before its determination by mode-mismatched thermal lens spectroscopy. - Highlights: • Development of a novel mixed hemimicelles dispersive micro solid phase extraction. • Utilization of IL coated magnetic graphene as efficient sorbent for SPME of fluoxetine. • Application of homemade mode-mismatched TLS for quantification of the fluoxetine. • Developed method showed the merits of very low LOD, rapidity and environmentally friendly.

  8. Development of a novel mixed hemimicelles dispersive micro solid phase extraction using 1-hexadecyl-3-methylimidazolium bromide coated magnetic graphene for the separation and preconcentration of fluoxetine in different matrices before its determination by fiber optic linear array spectrophotometry and mode-mismatched thermal lens spectroscopy

    International Nuclear Information System (INIS)

    Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Amir; Rashidian Vaziri, Mohammad Reza; Behjat, Abbas

    2016-01-01

    phase extraction is developed for the separation and preconcentration of trace amounts of fluoxetine before its determination by mode-mismatched thermal lens spectroscopy. - Highlights: • Development of a novel mixed hemimicelles dispersive micro solid phase extraction. • Utilization of IL coated magnetic graphene as efficient sorbent for SPME of fluoxetine. • Application of homemade mode-mismatched TLS for quantification of the fluoxetine. • Developed method showed the merits of very low LOD, rapidity and environmentally friendly.

  9. The preparation of sorbents from black coals

    Energy Technology Data Exchange (ETDEWEB)

    Rojak, A.; Roubicek, V.; Kaloc, M.; Lacny, Z. [Univ. of Mining and Metallurgy, Ostrava (Czechoslovakia)

    1994-12-31

    In this research project, different types of activated carbons were studied. The activated carbons were used as sorbents for phenol-ammonia waste water treatment. The basic parameters of coal, including specific surfaces, are shown in a table. The coals underwent carbonization under temperatures ranging from 500 C to 1,000 C. After cooling, the char was treated to achieve fineness ranging from 1.5 to 3.0 mm and was activated by a water stream. The active carbon was then used for biological-sorptional cleaning of waste water on model equipment. Results led to the following conclusions: (1) The sorption-biological refining process for phenol-ammonia waste waters from coking plants was suitable; (2) An activated coke has to be used as an input filter to acquire the highest efficiency during this biological process; and (3) During the sorption-biological refining of phenol-ammonia waters, phenol content was reduced significantly (90%), and chemical oxygen consumption was reduced (10%) in comparison with the unrefined phenol-ammonia water.

  10. Tributyl phosphate removal from reprocessing off-gas streams using a selected sorbent

    International Nuclear Information System (INIS)

    Parker, G.B.

    1980-01-01

    Laboratory experiments used small laboratory-scale columns packed with selected sorbent materials to remove tributyl phosphate (TBP) and iodine at conditions approaching those in actual reprocessing off-gas streams. The sorbent materials for TBP removal were placed upstream of iodine sorbent materials to protect the iodine sorbent from the deleterious effects of TBP. Methyl iodide in an airstream containing 30% TBP in normal paraffin hydrocarbons (NPH) and water vapor was metered to two packed columns of sorbents simultaneously (in parallel). One column contained a segment of 8-in. x 14-in. mesh alumina sorbent for TBP removal, the other did not. The measure of the effectiveness of TBP sorbent materials for TBP removal was determined by comparing the iodine retention of the iodine sorbent materials in the two parallel columns. Results from an 18 wt % Ag substituted mordenite iodine sorbent indicated that the iodine retention capacity of the sorbent was reduced 60% by the TBP and that the column containing iodine sorbent material protected by the alumina TBP sorbent retained 30 times more iodine than the column without TBP sorbent. TBP concentration was up to 500 mg/m 3 . Similar experiments using a 7 wt % Ag impregnated silica gel indicated that the TBP vapor had little effect on the iodine retention of the silica gel material. The stoichiometric maximum amount of iodine was retained by the silica gel material. Further experiments were conducted assessing the effects of NO 2 on iodine retention of this 7 wt % Ag sorbent. After the two columns were loaded with iodine in the presence of TBP (in NPH), one column was subjected to 2 vol % NO 2 in air. From visual comparison of the two columns, it appeared that the NO 2 regenerated the silica gel iodine sorbent and that iodine was washed off the silica gel iodine sorbent leaving the sorbent in the original state

  11. Spill sorbents: A comparison of water and oil sorbency

    International Nuclear Information System (INIS)

    Higgins, J.

    1993-01-01

    Sorbents for oil spills come in three general classes: organic, such as peat moss, sawdust, and paper fibre; inorganic, such as clay, vermiculite, and diatomaceous earth; and synthetic, including a variety of materials made from polymers such as polyethylene and polypropylene. The water and oil sorptive properties of various sorbents are listed and their characteristics are described. In spill remediation, most synthetic adsorbents are oleophilic with some degree of hydrophobic properties to prevent them from taking up water as they clean up the oil. In some situations, such as maintenance spills where aqueous liquids are also encountered, universal sorbents which have both oleophilic and hydrophilic properties are used. Sorbents are sold in a variety of product configurations, including powders, beads, rolls, ropes, and booms. Melt blown polypropylene is widely used since it is inexpensive, easy to apply, a good insulator, relatively inert, non-hazardous, and available in a wide variety of configurations. Its approximate oil sorbency is 20-30 times its own weight while its water sorbency is 0.0-0.1 times its own weight. In the Canadian market, sorbent products are available from importers, packagers, and manufacturers. The market is dominated by a few large companies that provide a range of high- and low-tech products in addition to ancillary products such as drums and skimmers. 2 tabs

  12. Dual layer hollow fiber sorbents: Concept, fabrication and characterization

    KAUST Repository

    Bhandari, Dhaval

    2013-02-01

    Hollow fiber sorbents are pseudo-monolithic separations materials created with fiber spinning technology using a polymer \\'binder\\', impregnated with high loadings of sorbent \\'fillers\\' [1]. To increase purified gas recovery during the sorption step and to ensure consistent sorption capacity over repeated cycles, a dense, thin polymer barrier layer on the fiber sorbents is needed to allow only thermal interactions between the sorbate loaded layer and the thermal regeneration fluid. This paper considers materials and methods to create delamination-free dual layer fiber sorbents, with a porous core and a barrier sheath layer formed using a simultaneous co-extrusion process. Low permeability polymers were screened for sheath layer creation, with the core layer comprising cellulose acetate polymer as binder and zeolite NaY as sorbent fillers. Appropriate core and sheath layer dope compositions were determined by the cloud-point method and rheology measurements. The morphology of the as-spun fibers was characterized in detail by SEM, EDX and gas permeation analysis. A simplified qualitative model is described to explain the observed fiber morphology. The effects of core, sheath spin dope and bore fluid compositions, spinning process parameters such as air-gap height, spin dope and coagulation bath temperatures, and elongation draw ratio are examined in detail. © 2012 Elsevier B.V. All rights reserved.

  13. Ecologically pure sorbents for power system of Myanmar

    Science.gov (United States)

    Nikitina, I. S.; Moryganova, Y. A.; Maung, Ko Ko; Arefeva, E. A.

    2017-11-01

    Currently, one of the most important problems of the thermal power plant, and many industrial enterprises in different countries is a wastewater treatment for oil products. When choosing the good sorbents is necessary to consider not only the properties and efficiency of the recommended materials, but also the cost, the possibility of environmentally friendly disposal of used sorbents and the possibility of using secondary resources. The purpose of this paper is to study the possibility of using agricultural waste in Myanmar as the sorbents in wastewater treatment containing oil products. The results of experiments have confirmed that rice hulls, and coconut fiber can be effectively used as the sorbents in wastewater treatment containing oil products at concentrations up to 10 mg/l. According to comparative analysis with the conventional sorbent-activated birch carbon (BAC-A) in the Russian power industry has shown that coconut fiber has very good sorption capacity and it is available to use as the raw materials for industries, which does not require to regenerate after using it and can be directly recycled in the factory.

  14. Cheap carbon sorbents produced from lignite by catalytic pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Kuznetsov, B.N.; Schchipko, M.L. [Inst. of Chemistry of Natural Organic Materials, Akademgorodok, Krasnoyarsk (Russian Federation)

    1995-12-01

    Some data are presented describing the new technology of carbon sorbent production from powdered lignite in the installation with fluidized bed of catalyst. It was shown the different types of char products with extended pore structure and high sorption ability can be produced from cheap and accessible lignite of Kansk-Achinsk coal pit in pilot installation with fluidized bed of Al-Cu-Cr oxide catalyst or catalytically active slag materials. In comparison with the conventional technologies of pyrolysis the catalytic pyrolysis allows to increase by 3-5 times the process productivity and to decrease significantly the formation of harmful compounds. The latter is accomplished by complete oxidation of gaseous pyrolysis products in the presence of catalysts and by avoiding the formation of pyrolysis tars - the source of cancerogenic compounds. The technology of cheap powdered sorbent production from lignites makes possible to obtain from lignite during the time of pyrolysis only a few seconds char products with porosity up to 0.6 cm{sup 3} /g, and specific surface area more than 400 m{sup 3} /g. Some methods of powdered chars molding into carbon materials with the different shape were proved for producing of firmness sorbents. Cheap carbon sorbents obtained by thermocatalytic pyrolysis can be successfully used in purification of different industrial pollutants as one-time sorbent or as adsorbents of long-term application with periodic regeneration.

  15. Sorbent application on the base of chitosan for radionuclides separation

    International Nuclear Information System (INIS)

    Pivarciova, L.

    2016-01-01

    Radioactive waste contains enormous amounts of radionuclides, which pollute the environment and can cause serious chemical and radiological toxicity threats to lower and higher living organism. Alternative process for the removal of heavy metal ions and radionuclides is sorption, which utilizes various certain natural materials of biological origin. Amino-polysaccharide-based sorbents e.g. chitosan represent suitable materials for binding of metal oxo-anion species because of numerous functional groups -OH and -NH 2 because of their suitable H-bond donor and acceptor sites. The sorbents on the base chitosan prepared through chemical modification were used for removal and separation certain radionuclides from aqueous media. The aim of this work was the study of physicochemical properties of prepared sorbents. The specific surface of sorbents was characterized with BET methods. Point of zero charge was identified with potentiometric titration. The size of particles and shape of sorbents were determined by scanning electron microscope. The sorption experiments for selected radionuclides were conducted under static and dynamic conditions. The effect of various parameters on the sorption 99m Tc, 60 Co and the effect of pH on the separation of radionuclide mixture in the solution were studied. (author)

  16. Development of a novel graphene/polyaniline electrodeposited coating for on-line in-tube solid phase microextraction of aldehydes in human exhaled breath condensate.

    Science.gov (United States)

    Li, Yu; Xu, Hui

    2015-05-22

    In this work, we introduced a novel graphene/polyaniline (G/PANI) electrodeposited coating for on-line in-tube solid phase microextraction (IT-SPME) for the first time. The G/PANI coating was prepared on the internal surface of stainless steel tube by a facile in-situ electrodeposition method. The morphology and formation of the composite coating were confirmed by scanning electronic microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Some important experimental parameters that could affect the extraction and separation such as the coating thickness, internal diameter of tube, sampling flow rate as well as sample volume were optimized. The extraction performance of the IT-SPME coating was evaluated systematically. The coating exhibited enhanced mechanical stability, long lifespan, large specific surface area and good biocompatibility compared with polyaniline coating. The on-line IT-SPME method showed higher enrichment efficiency, faster analysis speed and higher automation level than off-line manual mode. Six aldehydes were determined simultaneously with low limits of detection of 0.02-0.04nmolL(-1) and good linearity (R(2)≥0.9920). The method has been applied successfully for the determination of aldehydes in human exhaled breath condensates with good recovery (70-120%) and satisfied reproducibility (relative standard deviation: 1.1-11.9%). This on-line IT-SPME method provides a promising approach for the determination of trace aldehydes with approving sensitivity in human exhaled breath condensates. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. SPME-based air sampling method for inhalation exposure assessment studies: case study on perchlorethylene exposure in dry cleaning.

    Science.gov (United States)

    Zare Sakhvidi, Mohammad Javad; Bahrami, Abdul Rahman; Ghiasvand, Alireza; Mahjub, Hossein; Tuduri, Ludovic

    2013-06-01

    Exposure to perchlorethylene, especially for dry cleaning workers and for people living near dry cleaning shops, could lead to several diseases and disorders. This study examines the value of solid-phase microextraction (SPME) for sampling perchlorethylene in the atmosphere of dry cleaning shops. Carboxen/polydimethylsiloxane (CAR/PDMS) in 0.5-cm retracted mode was selected. There were no significant differences between sampling rates at different temperatures (range of 20 to 30 °C) and air velocities (2 to 50 cm/s). On the opposite, relative humidity (RH) had a significant effect on sampling rates. Method reproducibility was realized in the laboratory and field conditions and was 6.2 % and 7 to 11 %, respectively. Repeatability was also determined as 8.9 %. Comparison of the results according to the American Industrial Hygiene Association exposure assessment strategy showed the SPME sampler yields more conservative results in comparison with traditional standard method.

  18. Analysis of Volatile Markers for Virgin Olive Oil Aroma Defects by SPME-GC/FID: Possible Sources of Incorrect Data.

    Science.gov (United States)

    Oliver-Pozo, Celia; Aparicio-Ruiz, Ramón; Romero, Inmaculada; García-González, Diego L

    2015-12-09

    The need to explain virgin olive oil (VOO) aroma descriptors by means of volatiles has raised interest in applying analytical techniques for trapping and quantitating volatiles. Static headspace sampling with solid phase microextraction (SPME) as trapping material is one of the most applied solutions for analyzing volatiles. The use of an internal standard and the determination of the response factors of the main volatiles seem to guarantee the correct determination of volatile concentrations in VOOs by SPME-GC/FID. This paper, however, shows that the competition phenomena between volatiles in their adsorption to the SPME fiber, inherent in static headspace sampling, may affect the quantitation. These phenomena are more noticeable in the particular case of highly odorant matrices, such as rancid and vinegary VOOs with high intensity of defect. The competition phenomena can modify the measurement sensitivity, which can be observed in volatile quantitation as well as in the recording of internal standard areas in different matrices. This paper analyzes the bias of the peak areas and concentrations of those volatiles that are markers for each sensory defect of VOOs (rancid, vinegary, musty, and fusty) when the intensity and complexity of aroma are increased. Of the 17 volatile markers studied in this work, 10 presented some anomalies in the quantitation in highly odorant matrices due the competition phenomena. However, quantitation was not affected in the concentration ranges at which each volatile marker is typically found in the defective oils they were characteristic of, validating their use as markers.

  19. Essential oil from Rhaponticum acaule L. roots: Comparative study using HS-SPME/GC/GC–MS and hydrodistillation techniques

    Directory of Open Access Journals (Sweden)

    Batoul Benyelles

    2014-12-01

    Full Text Available The composition of essential oil extracted from Rhaponticum acaule L. roots growing wild in Algeria was studied by hydrodistillation (HD and by Head-Space Solid Phase Micro-Extraction (HS-SPME. Quantitative but not qualitative differences have been found in the chemical composition of both analysed samples depending on the extraction method. However, the oil obtained from R. acaule roots shows that aliphatic alcohols were found to be the major class (69.2%, followed by the terpenes (5.5%, alkenes (5.2% and alkynes (4.0%. In both cases the analysis were carried out using Gas Chromatography (GC and Gas Chromatography–Mass Spectrometry (GC–MS. Our study shows that HS-SPME extraction could be considered as an alternative technique for the isolation of volatiles from plant. 25 components were identified in oil vs. 39 in the HS-SPME. However the oil composition of roots was mainly represented by a variety of aliphatic hydrocarbons (alcohols, aldehydes and ketones and terpenes which are known for their antimicrobial activities.

  20. Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis

    Directory of Open Access Journals (Sweden)

    Kazuki Saito

    2013-04-01

    Full Text Available Plants produce various volatile organic compounds (VOCs, which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS. We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions.

  1. Characterization of calcium carbonate sorbent particle in furnace environment

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Kang Soo [Aerosol and Particle Technology Laboratory, Department of Mechanical Engineering, KAIST 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of); Jung, Jae Hee [Environment Sensor System Research Center, KIST 39-1 Hawolgok-dong, Seongbuk-gu, Seoul, 136-791 (Korea, Republic of); Keel, Sang In; Yun, Jin Han; Min, Tai Jin [Environmental Systems Research Division, KIMM 104 Sinseongno, Yuseong-gu, Daejeon, 305-343 (Korea, Republic of); Kim, Sang Soo, E-mail: sskim@kaist.ac.kr [Aerosol and Particle Technology Laboratory, Department of Mechanical Engineering, KAIST 291 Daehak-ro, Yuseong-gu, Daejeon, 305-701 (Korea, Republic of)

    2012-07-01

    The oxy-fuel combustion system is a promising technology to control CO{sub 2} and NO{sub X} emissions. Furthermore, sulfation reaction mechanism under CO{sub 2}-rich atmospheric condition in a furnace may lead to in-furnace desulfurization. In the present study, we evaluated characteristics of calcium carbonate (CaCO{sub 3}) sorbent particles under different atmospheric conditions. To examine the physical/chemical characteristics of CaCO{sub 3}, which is used as a sorbent particle for in-furnace desulfurization in the oxy-fuel combustion system, they were injected into high temperature drop tube furnace (DTF). Experiments were conducted at varying temperatures, residence times, and atmospheric conditions in a reactor. To evaluate the aerosolizing characteristics of the CaCO{sub 3} sorbent particle, changes in the size distribution and total particle concentration between the DTF inlet and outlet were measured. Structural changes (e.g., porosity, grain size, and morphology) of the calcined sorbent particles were estimated by BET/BJH, XRD, and SEM analyses. It was shown that sorbent particles rapidly calcined and sintered in the air atmosphere, whereas calcination was delayed in the CO{sub 2} atmosphere due to the higher CO{sub 2} partial pressure. Instead, the sintering effect was dominant in the CO{sub 2} atmosphere early in the reaction. Based on the SEM images, it was shown that the reactions of sorbent particles could be explained as a grain-subgrain structure model in both the air and CO{sub 2} atmospheres.

  2. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    Zhen Ding

    2014-01-01

    Full Text Available The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME coupled to chromatography-mass spectrometry (GC-MS, including geosmin (GSM and 2-methylisoborneol (2-MIB, as well as dimethyl trisulfide (DMTS, β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA, the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5. The limits of detection (LOD are all below 1.3 ng L−1, and the relative standard deviation (%RSD is between 4.4% and 9.9% (n = 7 and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

  3. Study of flavour compounds from orange juices by HS-SPME and GC-MS

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Covaciu, F.; Feher, I.; Magdas, A.; David, L.; Moldovan, Z.

    2013-11-01

    The flavour of the orange juices, which gives the taste and odour of the product, is an important criterion about the products quality for consumers. A fresh single strength and two commercial orange juices (obtained from concentrate) flavour profile were studied using a selective and sensitive gas chromatography - mass spectrometry (GC-MS) analytical system, after a solvent free, single step preconcentration and extraction technique, the headspace solid phase microextraction (HP-SPME). In the studied orange juices 55 flavour compounds were detected and classified as belonging to the esters, alcohols, ketones, monoterpenes and sesquiterpenes chemical families. The fresh single strength orange juice was characterized by high amount of esters, monoterpenes and sesquiterpenes. Limonene and valencene were the most abundant flavours in this fresh natural orange juice. Alcohols and ketones were found in higher concentration in the commercial orange juices made from concentrate, than in the single strength products. Nevertheless, in commercial juices the most abundant flavour was limonene and α-terpineol. The results highlight clear differences between fresh singles strength orange juice and juice from concentrate. The orange juices reconstructed from concentrate, made in Romania, present low quantity of flavour compounds, suggesting the absence or a low rearomatization process, but extraneous components were not detected.

  4. Volatile emerging contaminants in melon fruits, analysed by HS-SPME-GC-MS.

    Science.gov (United States)

    Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

    2018-03-01

    The aim of this research was to develop and validate a headspace-solid phase micro-extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for the determination of volatile emerging contaminants in fruit. The method showed good precision (RSD ≤ 14%) and satisfactory recoveries (99.1-101.7%) and LOD and LOQ values ranging between 0.011-0.033 μg kg -1 and 0.037-0.098 μg kg -1 , respectively. The method was applied to investigate the content of volatile emerging contaminants in two varieties of melon fruit (Cucumis melo L.) cultivated adjoining high-risk areas. Glycol ethers, BHT, BHA and BTEX (benzene, toluene, ethylbenzene and xylene) were determined in melon fruit pulps for the first time, with different sensitivities depending on sample and variety. Although the amount of the volatile contaminants in the melon samples were in the order of µg kg -1 , the safety of vegetable crops cultivated near risk areas should be more widely considered. The results showed that this accurate and reproducible method can be useful for routine safety control of fruits and vegetables.

  5. Fingerprint of volatiles from plant extracts based on SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Ezequias P. Siqueira

    Full Text Available The Laboratory of Chemistry of Natural Products has an ex situ collection of extracts from organisms of the biodiversity aiming at bioprospecting. Nowadays the collection has about 4000 extracts from 1000 different species. Extracts are used to identify new bioactive compounds that could be useful for developing new drugs against neglected diseases like leishmaniosis, Chagas disease, malaria and tuberculosis. After biologic assays, the bioactive extracts need to be prepared in larger quantity to allow isolation and characterization of the bioactive component. At this time, it is important to not only confirm the bioactivity of new extract but also check if its composition is similar to the old one. It was evaluated the ability of Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry analysis (SPME-GC-MS. It was used the AMDIS (Automatic Mass Spectral Deconvolution and Identification System software as tools to collect and to compare the chromatographic profiles of each extract (fingerprint. Forty six samples were analyzed, it was possible to infer from the composition of each sample and common compounds. Nine groups of samples, collected at different time, were analyzed and seasonal modifications between then could be elucidated. The results showed that this methodology can be used to monitor the composition of extracts, allowing to monitor chemical changes that may occur during storage periods and to investigate the occurrence of a determined component in different extracts.

  6. ANALYTICAL APPROACH OF THE VOLATILE FRACTION OF Solanum quitoense BY HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    EDUARDO CORPAS IGUARÁN

    2017-07-01

    Full Text Available The species of lulo fruit (Solanum quitoense, predominant in Colombia, is a promising fruit for both national and international market due to its flavor and nutritional characteristics, which generated the interest to know the volatile composition of its pulp. After adjusting, the chromatographic conditions necessary to analyze volatile fraction of this fruit, the effect of the temperature and time of adsorption was measured through the headspace - solid phase microextraction (HS-SPME and gas chromatography - mass spectrometry (GC-MS, on the area of volatile compounds of S. quitoense, by applying the experimental design of a factor. The descriptive analysis suggested that the adsorption at 60°C and 30 minutes promoted optimal recovery of volatiles as well as internal standard (1-Octanol, with recovery of 99,66% at 60ºC, while the non-parametric test Kruskal-Wallis showed statistical differences in the effect of time (P= 0,018, but not of the temperature adsorption (P= 0,058 upon the volatiles compounds area. A predominance of esters (48,98%, aldehydes (18,37%, and alcohols (14,29% was observed and also were found compounds of greatest area such as 3-hexen-1-ol acetate, acetic acid methyl ester, and acetic acid hexyl ester. These metabolites determine the characteristic aroma from lulo pulp and influence the consumer preference.

  7. 21 CFR 876.5600 - Sorbent regenerated dialysate delivery system for hemodialysis.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Sorbent regenerated dialysate delivery system for hemodialysis. 876.5600 Section 876.5600 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND....5600 Sorbent regenerated dialysate delivery system for hemodialysis. (a) Identification. A sorbent...

  8. Regeneration of FGD dry-sorbent materials. Phase I. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Kapsalopoulou, A.J.; Sargent, D.H.; Rissman, E.F.

    1982-05-01

    Sodium-based sorbent injection directly into the flue gas duct of a coal-burning power plant has been investigated since 1975 by GFETC (using laboratory and pilot plant apparatus) as an SO/sub 2/ control technology. Regeneration of sorbent from spent sorbent material is highly desirable to reduce the sorbent cost, and to alleviate the leaching and potential pollution problems of soluble sodium compounds when disposing of spent sorbent materials in landfills. The work reported herein was initiated to develop a continuous, aqueous-based process for regeneration of sodium carbonate-type sorbents from spent sodium-base sorbent/flyash materials. Specific project objectives are to: (1) retain process simplicity and to avoid difficult process conditions; (2) maximize recovery of sodium from spent sorbents; (3) minimize process costs and energy requirements; (4) maximize reactivity of the regenerated sodium bicarbonate sorbent; and (5) produce process waste materials that may be disposed of in an environmental acceptable manner. The sorbent regeneration process which has been developed during the laboratory investigation (Phase I) of this project may be divided into three parts: (1) leaching of the spent sodium-based sorbent; (2) conversion of the leachate to a NaCl brine; and (3) production of NaHCO/sub 3/ (regenerated sorbent) using commercially-proven Solvay (ammonia-soda) process technology. Significant results from the laboratory study are as given.

  9. High Temperature Flue Gas Desulfurization In Moving Beds With Regenerable Copper Based Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Cengiz, P.A.; Ho, K.K.; Abbasian, J.; Lau, F.S.

    2002-09-20

    The objective of this study was to develop new and improved regenerable copper based sorbent for high temperature flue gas desulfurization in a moving bed application. The targeted areas of sorbent improvement included higher effective capacity, strength and long-term durability for improved process control and economic utilization of the sorbent.

  10. THE PERFORMANCE OF NATURAL SORBENTS IN THE SULFUR DIOXIDE ADSORPTION

    Directory of Open Access Journals (Sweden)

    Т. L. Rakyts’ka

    2015-02-01

    Full Text Available The performance of natural sorbents with different mineralogical makeup (zeolites, layered aluminosilicates, basalt tuffs, and dispersed silicas in the adsorption-desorption of sulfur dioxide at its contents in the gas-air mixture of 150 and 200 mg/m3 and at the temperature of 20 °C has been studied. The S02 adsorption has been found to be predominately the physical one. The adsorption capacity values obtained experimentally for the sorbents have been compared with the data presented in the literature.

  11. Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

    Directory of Open Access Journals (Sweden)

    R.V. Smotraiev

    2016-05-01

    Full Text Available The actual problem of water supply in the world and in Ukraine, in particular, is a high level of pollution in water resources and an insufficient level of drinking water purification. With industrial wastewater, a significant amount of pollutants falls into water bodies, including suspended particles, sulfates, iron compounds, heavy metals, etc. Aim: The aim of this work is to determine the impact of aluminum and manganese ions additives on surface and sorption properties of zirconium oxyhydroxide based sorbents during their production process. Materials and Methods: The sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were prepared by sol-gel method during the hydrolysis of metal chlorides (zirconium oxychloride ZrOCl2, aluminum chloride AlCl3 and manganese chloride MnCl2 with carbamide. Results: The surface and sorption properties of sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were investigated. X-ray amorphous structure and evolved hydroxyl-hydrate cover mainly characterize the obtained xerogels. The composite sorbents based on xerogels of zirconium oxyhydroxide doped with aluminum oxyhydroxide (aS = 537 m2/g and manganese oxyhydroxide (aS = 356 m2/g have more developed specific surface area than single-component xerogels of zirconium oxyhydroxide (aS = 236 m2/g and aluminum oxyhydroxide (aS = 327 m2/g. The sorbent based on the xerogel of zirconium and manganese oxyhydroxides have the maximum SO42--ions sorption capacity. It absorbs 1.5 times more SO42–-ions than the industrial anion exchanger AN-221. The sorbents based on xerogels of zirconium oxyhydroxide has the sorption capacity of Fe3+-ions that is 1.5…2 times greater than the capacity of the industrial cation exchanger KU-2-8. The Na+-ions absorption capacity is 1.47…1.56 mmol/g for each sorbent. Conclusions: Based on these data it can be concluded that the proposed method is effective for sorbents production based on

  12. A novel ionic liquid-modified organic-polymer monolith as the sorbent for in-tube solid-phase microextraction of acidic food additives.

    Science.gov (United States)

    Wang, Ting-Ting; Chen, Yi-Hui; Ma, Jun-Feng; Hu, Min-Jie; Li, Ying; Fang, Jiang-Hua; Gao, Hao-Qi

    2014-08-01

    A novel ionic liquid-modified organic-polymer monolithic capillary column was prepared and used for in-tube solid-phase microextraction (SPME) of acidic food additives. The primary amino group of 1-aminopropyl-3-methylimidazolium chloride was reacted with the epoxide group of glycidyl methacrylate. The as-prepared new monomer was then copolymerized in situ with acrylamide and N,N'-methylenebisacrylamide in the presence of polyethylene glycol (PEG)-8000 and PEG-10,000 as porogens. The extraction performance of the developed monolithic sorbent was evaluated for benzoic acid, 3-hydroxybenzoic acid, cinnamic acid, 2,4-dichlorophenoxyacetic acid, and 3-(trifluoromethyl)-cinnamic acid. Such a sorbent, bearing hydrophobic and anion-exchange groups, had high extraction efficiency towards the test compounds. The adsorption capacities for the analytes dissolved in water ranged from 0.18 to 1.74 μg cm(-1). Good linear calibration curves (R(2) > 0.99) were obtained, and the limits of detection (S/N = 3) for the analytes were found to be in the range 1.2-13.5 ng mL(-1). The recoveries of five acidic food additives spiked in Coca-Cola beverage samples ranged from 85.4 % to 98.3 %, with RSD less than 6.9 %. The excellent applicability of the ionic liquid (IL)-modified monolithic column was further tested by the determination of benzoic acid content in Sprite samples, further illustrating its good potential for analyzing food additives in complex samples.

  13. Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke.

    Science.gov (United States)

    Conde, Francisco J; Afonso, Ana M; González, Venerando; Ayala, Juan H

    2006-08-01

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L(-1), followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L(-1) and 2 L min(-1) for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-microm carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL(-1). 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R2 > or = 0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%).

  14. Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke

    Energy Technology Data Exchange (ETDEWEB)

    Conde, Francisco J.; Afonso, Ana M.; Gonzalez, Venerando; Ayala, Juan H. [University of La Laguna, Campus de Anchieta, Department of Analytical Chemistry, Nutrition and Food Science, La Laguna (Spain)

    2006-08-15

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L{sup -1}, followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L{sup -1} and 2 L min{sup -1} for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-{mu}m carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL{sup -1}. 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R {sup 2}{>=}0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%). (orig.)

  15. Mercury Information Clearinghouse. Quarterly 1: sorbent injection technologies for mercury control

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2004-07-01

    Sorbent injection technologies for mercury control in coal-fired power plants and, in particular, the injection of activated carbon sorbents are examined. The retrofit technology that has been demonstrated to have the widest application for the control of mercury in plants without flue gas desulphurization scrubbers is discussed. The report covers mercury control requirements, laboratory studies on factors that affect sorbent capacity, pilot scale tests of the capture performance of different coals, research on sorbent properties, and full scale demonstration of sorbent control technologies. 34 refs., 3 figs., 4 tabs.

  16. Evaluation of inorganic sorbent treatment for LWR coolant process streams

    Energy Technology Data Exchange (ETDEWEB)

    Roddy, J.W.

    1984-03-01

    This report presents results of a survey of the literature and of experience at selected nuclear installations to provide information on the feasibility of replacing organic ion exchangers with inorganic sorbents at light-water-cooled nuclear power plants. Radioactive contents of the various streams in boiling water reactors and pressurized water reactors were examined. In addition, the methods and performances of current methods used for controlling water quality at these plants were evaluated. The study also includes a brief review of the physical and chemical properties of selected inorganic sorbents. Some attributes of inorganic sorbents would be useful in processing light water reactor (LWR) streams. The inorganic resins are highly resistant to damage from ionizing radiation, and their exchange capacities are generally equivalent to those of organic ion exchangers. However, they are more limited in application, and there are problems with physical integrity, especially in acidic solutions. Research is also needed in the areas of selectivity and anion removal before inorganic sorbents can be considered as replacements for the synthetic organic resins presently used in LWRs. 11 figures, 14 tables.

  17. New Composite Sorbents for Caesium and Strontium Ions Sorption

    Directory of Open Access Journals (Sweden)

    Mykola Kartel

    2017-06-01

    Full Text Available Composite lignocellulose-inorganic sorbents derived from plant residues of agriculture and food industry, modified with ferrocyanides of d-metals and hydrated antimony pentoxide were prepared. Caesium and strontium ions removal from water was tested by radiotracer method. Sorption of heavy metal ions, methylene blue, gelatin, vitamin B12 was also studied.

  18. Novel composite sorbent AAm/MA hydrogels containing starch and ...

    Indian Academy of Sciences (India)

    A novel polymer/clay composite sorbent based on acrylamide/maleic acid, starch and clay such as kaolin was synthesized with free radical solution polymerization by using ammonium persulfate/,,','-tetramethylethylenediamine as redox initiating pair in the presence of poly(ethylene glycol)diacrylate as a crosslinker.

  19. Core-in-shell sorbent for hot coal gas desulfurization

    Science.gov (United States)

    Wheelock, Thomas D.; Akiti, Jr., Tetteh T.

    2004-02-10

    A core-in-shell sorbent is described herein. The core is reactive to the compounds of interest, and is preferably calcium-based, such as limestone for hot gas desulfurization. The shell is a porous protective layer, preferably inert, which allows the reactive core to remove the desired compounds while maintaining the desired physical characteristics to withstand the conditions of use.

  20. Comments on "Ceria-Zirconia High-Temperature Desulfurization Sorbents".

    Czech Academy of Sciences Publication Activity Database

    Hartman, Miloslav; Trnka, Otakar

    2006-01-01

    Roč. 45, č. 4 (2006), s. 1548-1549 ISSN 0888-5885 Institutional research plan: CEZ:AV0Z40720504 Keywords : hydrogen sulfide * desulfurization * cerium sorbent Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 1.518, year: 2006

  1. Sorption of Antimony from Organic Solutions on Inorganic Sorbents

    International Nuclear Information System (INIS)

    El-Dessouky, S.I.; Zakaria, N.; Alian, A.

    2000-01-01

    Sorption of 124 Sb(III) from its complexes in benzene, toluene, o-xylene and chloroform on an artificial inorganic exchanger (chabazite, a) and on bone charcoal (b.ch) was investigated using the static method. Complexes pf Sb(III) with these non-polar organic liquids were prepared by extraction of its chloride by each liquid from 12 M H 2 SO 4 . For the various liquids the order of the uptake in case of chabazite is o-xylene> toluene > benzene> chloroform and in case of b.ch the order is benzene> toluene > chloroform> o-xylene. This suggests different sorption mechanisms for the two studied sorbents, one of them (chabazite) being purely an inorganic sorbent. In general the uptake of Sb(III) from all solvents studied is much higher by b.ch than by chabazite. The uptake of Sb(III) from these non-aqueous solvents by b.ch is also much higher than its uptake by four previously studied sorbents: ashless filter paper cellulose, pyrolysis residue from domestic waste, bentonite elay from upper Egypt and fly ash from a thermal electricity station. The desorption of Sb(III) from the loaded sorbents by 1M HCI was also studied and found maximum within 30 minutes

  2. Evaluation of inorganic sorbent treatment for LWR coolant process streams

    International Nuclear Information System (INIS)

    Roddy, J.W.

    1984-03-01

    This report presents results of a survey of the literature and of experience at selected nuclear installations to provide information on the feasibility of replacing organic ion exchangers with inorganic sorbents at light-water-cooled nuclear power plants. Radioactive contents of the various streams in boiling water reactors and pressurized water reactors were examined. In addition, the methods and performances of current methods used for controlling water quality at these plants were evaluated. The study also includes a brief review of the physical and chemical properties of selected inorganic sorbents. Some attributes of inorganic sorbents would be useful in processing light water reactor (LWR) streams. The inorganic resins are highly resistant to damage from ionizing radiation, and their exchange capacities are generally equivalent to those of organic ion exchangers. However, they are more limited in application, and there are problems with physical integrity, especially in acidic solutions. Research is also needed in the areas of selectivity and anion removal before inorganic sorbents can be considered as replacements for the synthetic organic resins presently used in LWRs. 11 figures, 14 tables

  3. Natural sorbents for decontamination of objects of urban territories

    International Nuclear Information System (INIS)

    Movchan, N.; Fedorenko, Yu.; Zlobenko, B.; Spigoun, A.

    1996-01-01

    This paper gives an information about the use of film coverings, based on natural sorbents, in decontamination of buildings, contaminated after the Chernobyl accident. This method has incontrovertible advantages in the beginning period after the accident and can be used for cleaning considerable areas of urban territories

  4. Monolithic natural gas storage delivery system based on sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Hornbostel, Marc; Krishnan, Gopala N.; Sanjurjo, Angel

    2016-09-27

    The invention provides methods for producing a strong, light, sorbent-based storage/dispenser system for gases and fuels. The system comprises a porous monolithic material with an adherent strong impervious skin that is capable of storing a gas under pressure in a safe and usable manner.

  5. A selective sorbent for removing bacterial endotoxins from blood

    Science.gov (United States)

    Morozov, A. S.; Kopitsyna, M. N.; Bessonov, I. V.; Karelina, N. V.; Nuzhdina, A. V.; Sarkisov, I. Yu.; Pavlova, L. A.; Tsyurupa, M. P.; Blinnikova, Z. K.; Davankov, V. A.

    2016-12-01

    Synthetic ligands carrying a positive charge and capable of selective binding of bacterial endotoxins are covalently immobilized on surfaces of domestic hemosorbent Styrosorb-514 based on hypercrosslinked polystyrene. It is shown that the resulting sorbent aimed at treating sepsis exceeds imported specific hemosorbent in Toraymyxin™ columns in removing lipopolysaccharides, and can be used in domestically-produced Desepta columns.

  6. Sorbent preparation/modification/additives. Final report, September 1, 1992--November 30, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Prudich, M.E.; Venkataramakrishnan, R. [Ohio Univ., Athens, OH (United States)

    1994-02-01

    Sorbent preparation techniques used today have generally been adapted from techniques traditionally used by the lime industry. Traditional dry hydration and slaking processes have been optimized to produce materials intended for use in the building industry. These preparation techniques should be examined with an eye to optimization of properties important to the SO{sub 2} capture process. The study of calcium-based sorbents for sulfur dioxide capture is complicated by two factors: (1) little is known about the chemical mechanisms by which the standard sorbent preparation and enhancement techniques work, and (2) a sorbent preparation technique that produces a calcium-based sorbent that enjoys enhanced calcium utilization in one regime of operation [flame zone (>2400 F), in-furnace (1600--2400 F), economizer (800--1100 F), after air preheater (<350 F)] may not produce a sorbent that enjoys enhanced calcium utilization in the other reaction zones. Again, an in-depth understanding of the mechanism of sorbent enhancement is necessary if a systematic approach to sorbent development is to be used. As a long-term goal, an experimental program is being carried out for the purpose of (1) defining the effects of slaking conditions on the properties of calcium-based sorbents, (2) determining how the parent limestone properties of calcium-based sorbents, and (3) elucidating the mechanism(s) relating to the activity of various dry sorbent additives. An appendix contains a one-dimensional duct injection model with modifications to handle the sodium additives.

  7. Sorbent-Based Gas Phase Air Cleaning for VOCs in CommercialBuildings

    Energy Technology Data Exchange (ETDEWEB)

    Fisk, William J.

    2006-05-01

    This paper provides a review of current knowledge about the suitability of sorbent-based air cleaning for removing volatile organic compounds (VOCs) from the air in commercial buildings as needed to enable reductions in ventilation rates and associated energy savings. The fundamental principles of sorbent air cleaning are introduced, criteria are suggested for sorbent systems that can counteract indoor VOC concentration increases from reduced ventilation, major findings from research on sorbent performance for this application are summarized, novel sorbent technologies are described, and related priority research needs are identified. Major conclusions include: sorbent systems can remove a broad range of VOCs with moderate to high efficiency, sorbent technologies perform effectively when challenged with VOCs at the low concentrations present indoors, and there is a large uncertainty about the lifetime and associated costs of sorbent air cleaning systems when used in commercial buildings for indoor VOC control. Suggested priority research includes: experiments to determine sorbent system VOC removal efficiencies and lifetimes considering the broad range and low concentration of VOCs indoors; evaluations of in-situ regeneration of sorbents; and an updated analysis of the cost of sorbent air cleaning relative to the cost of ventilation.

  8. Solid sorbents for removal of carbon dioxide from gas streams at low temperatures

    Science.gov (United States)

    Sirwardane, Ranjani V.

    2005-06-21

    New low-cost CO.sub.2 sorbents are provided that can be used in large-scale gas-solid processes. A new method is provided for making these sorbents that involves treating substrates with an amine and/or an ether so that the amine and/or ether comprise at least 50 wt. percent of the sorbent. The sorbent acts by capturing compounds contained in gaseous fluids via chemisorption and/or physisorption between the unit layers of the substrate's lattice where the polar amine liquids and solids and/or polar ether liquids and solids are located. The method eliminates the need for high surface area supports and polymeric materials for the preparation of CO.sub.2 capture systems, and provides sorbents with absorption capabilities that are independent of the sorbents' surface areas. The sorbents can be regenerated by heating at temperatures in excess of 35.degree. C.

  9. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry

    Science.gov (United States)

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-01

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r2 = 0.998) in the range of 3.0-85.0 μg L-1 with a detection limit of 0.7 μg L-1 for preconcentration of 25.0 mL of the sample and the relative standard deviation (n = 6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

  10. On-site monitoring of biogenic emissions from Eucalyptus dunnii leaves using membrane extraction with sorbent interface combined with a portable gas chromatograph system.

    Science.gov (United States)

    Liu, Xinyu; Pawliszyn, Richard; Wang, Limei; Pawliszyn, Janusz

    2004-01-01

    Membrane extraction with sorbent interface, combined with a portable gas chromatograph system (MESI-Portable GC) for continuous on-line monitoring of biogenic volatile organic compounds (BVOCs) emissions (from leaves of Eucalytus dunnii in a greenhouse), is presented herein. A sampling chamber was designed to facilitate the extraction and identification of the BVOCs emitted by the Eucalytus dunnii leaves. Preliminary experiments, including; enrichment times, microtrap temperatures, stripping gas flow rates, and desorption temperatures were investigated to optimize experimental parameters. The main components of BVOCs released by the Eucalytus dunnii leaves were identified by comparing the retention times of peaks with those of authentic standard solutions. They were then confirmed with solid phase microextraction coupled with gas chromatography and mass spectrometry (SPME-GC-MS). BVOC emission profiles of [small alpha]-pinene, eucalyptol, and [gamma]-terpinene emitted by intact and damaged Eucalytus dunnii leaves were obtained. The findings suggest that the MESI-Portable GC system is a simple and useful tool for field monitoring changes in plant emissions as a function of time.

  11. Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

    Science.gov (United States)

    Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

    2015-08-05

    A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Lime-Based Sorbents for High-Temperature CO2 Capture—A Review of Sorbent Modification Methods

    Directory of Open Access Journals (Sweden)

    Edward J. Anthony

    2010-08-01

    Full Text Available This paper presents a review of the research on CO2 capture by lime-based looping cycles undertaken at CanmetENERGY’s (Ottawa, Canada research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO2 capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC reactor which contains a carbonator—a unit for CO2 capture, and a calciner—a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO2 carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use.

  13. Lime-Based Sorbents for High-Temperature CO2 Capture—A Review of Sorbent Modification Methods

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J.

    2010-01-01

    This paper presents a review of the research on CO2 capture by lime-based looping cycles undertaken at CanmetENERGY’s (Ottawa, Canada) research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO2 capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC) reactor which contains a carbonator—a unit for CO2 capture, and a calciner—a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO2 carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use. PMID:20948952

  14. Lime-based sorbents for high-temperature CO2 capture--a review of sorbent modification methods.

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J

    2010-08-01

    This paper presents a review of the research on CO(2) capture by lime-based looping cycles undertaken at CanmetENERGY's (Ottawa, Canada) research laboratories. This is a new and very promising technology that may help in mitigation of global warming and climate change caused primarily by the use of fossil fuels. The intensity of the anticipated changes urgently requires solutions such as more cost-effective technologies for CO(2) capture. This new technology is based on the use of lime-based sorbents in a dual fluidized bed combustion (FBC) reactor which contains a carbonator-a unit for CO(2) capture, and a calciner-a unit for CaO regeneration. However, even though natural materials are cheap and abundant and very good candidates as solid CO(2) carriers, their performance in a practical system still shows significant limitations. These limitations include rapid loss of activity during the capture cycles, which is a result of sintering, attrition, and consequent elutriation from FBC reactors. Therefore, research on sorbent performance is critical and this paper reviews some of the promising ways to overcome these shortcomings. It is shown that reactivation by steam/water, thermal pre-treatment, and doping simultaneously with sorbent reforming and pelletization are promising potential solutions to reduce the loss of activity of these sorbents over multiple cycles of use.

  15. EVALUATION OF FGD DRY INJECTION SORBENTS AND ADDITIVES - VOLUME 2 - PILOT PLANT EVALUATION OF HIGH REACTIVITY SORBENTS

    Science.gov (United States)

    The report describes a mini-pilot test program to investigate potential new sorbents and processes for dry SO2 removal. Initial tests showed that the 85 cu m/h pilot plant could be used successfully to evaluate both spray dryer and dry injection processes using traditional calciu...

  16. Low temperature SO{sub 2} removal with solid sorbents in a circulating fluidized bed absorber. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Lee, S.K.; Keener, T.C.

    1994-10-10

    A novel flue gas desulfurization technology has been developed at the University of Cincinnati incorporating a circulating fluidized bed absorber (CFBA) reactor with dry sorbent. The main features of CFBA are high sorbent/gas mixing ratios, excellent heat and mass transfer characteristics, and the ability to recycle partially utilized sorbent. Subsequently, higher SO{sub 2} removal efficiencies with higher overall sorbent utilization can be realized compared with other dry sorbent injection scrubber systems.

  17. Carbon Dioxide Capture from Flue Gas Using Dry Regenerable Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Thomas Nelson; David Green; Paul Box; Raghubir Gupta; Gennar Henningsen

    2007-06-30

    Regenerable sorbents based on sodium carbonate (Na{sub 2}CO{sub 3}) can be used to separate carbon dioxide (CO{sub 2}) from coal-fired power plant flue gas. Upon thermal regeneration and condensation of water vapor, CO{sub 2} is released in a concentrated form that is suitable for reuse or sequestration. During the research project described in this report, the technical feasibility and economic viability of a thermal-swing CO{sub 2} separation process based on dry, regenerable, carbonate sorbents was confirmed. This process was designated as RTI's Dry Carbonate Process. RTI tested the Dry Carbonate Process through various research phases including thermogravimetric analysis (TGA); bench-scale fixed-bed, bench-scale fluidized-bed, bench-scale co-current downflow reactor testing; pilot-scale entrained-bed testing; and bench-scale demonstration testing with actual coal-fired flue gas. All phases of testing showed the feasibility of the process to capture greater than 90% of the CO{sub 2} present in coal-fired flue gas. Attrition-resistant sorbents were developed, and these sorbents were found to retain their CO{sub 2} removal activity through multiple cycles of adsorption and regeneration. The sodium carbonate-based sorbents developed by RTI react with CO{sub 2} and water vapor at temperatures below 80 C to form sodium bicarbonate (NaHCO3) and/or Wegscheider's salt. This reaction is reversed at temperatures greater than 120 C to release an equimolar mixture of CO{sub 2} and water vapor. After condensation of the water, a pure CO{sub 2} stream can be obtained. TGA testing showed that the Na{sub 2}CO3 sorbents react irreversibly with sulfur dioxide (SO{sub 2}) and hydrogen chloride (HCl) (at the operating conditions for this process). Trace levels of these contaminants are expected to be present in desulfurized flue gas. The sorbents did not collect detectable quantities of mercury (Hg). A process was designed for the Na{sub 2}CO{sub 3}-based sorbent that

  18. Comparison of Spot and Time Weighted Averaging (TWA Sampling with SPME-GC/MS Methods for Trihalomethane (THM Analysis

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

    Full Text Available Water samples were collected and analyzed for conductivity, pH, temperature and trihalomethanes (THMs during the fall of 2014 at two monitored municipal drinking water source ponds. Both spot (or grab and time weighted average (TWA sampling methods were assessed over the same two day sampling time period. For spot sampling, replicate samples were taken at each site and analyzed within 12 h of sampling by both Headspace (HS- and direct (DI- solid phase microextraction (SPME sampling/extraction methods followed by Gas Chromatography/Mass Spectrometry (GC/MS. For TWA, a two day passive on-site TWA sampling was carried out at the same sampling points in the ponds. All SPME sampling methods undertaken used a 65-µm PDMS/DVB SPME fiber, which was found optimal for THM sampling. Sampling conditions were optimized in the laboratory using calibration standards of chloroform, bromoform, bromodichloromethane, dibromochloromethane, 1,2-dibromoethane and 1,2-dichloroethane, prepared in aqueous solutions from analytical grade samples. Calibration curves for all methods with R2 values ranging from 0.985–0.998 (N = 5 over the quantitation linear range of 3–800 ppb were achieved. The different sampling methods were compared for quantification of the water samples, and results showed that DI- and TWA- sampling methods gave better data and analytical metrics. Addition of 10% wt./vol. of (NH42SO4 salt to the sampling vial was found to aid extraction of THMs by increasing GC peaks areas by about 10%, which resulted in lower detection limits for all techniques studied. However, for on-site TWA analysis of THMs in natural waters, the calibration standard(s ionic strength conditions, must be carefully matched to natural water conditions to properly quantitate THM concentrations. The data obtained from the TWA method may better reflect actual natural water conditions.

  19. HS-SPME-GC×GC-qMS volatile metabolite profiling of Chrysolina herbacea frass and Mentha spp. leaves.

    Science.gov (United States)

    Cordero, Chiara; Zebelo, Simon Atsbaha; Gnavi, Giorgio; Griglione, Alessandra; Bicchi, Carlo; Maffei, Massimo E; Rubiolo, Patrizia

    2012-02-01

    Headspace solid-phase microextraction (HS-SPME) comprehensive two-dimensional (2D) gas chromatography combined with quadrupole-mass spectrometry (GC×GC-qMS) with dedicated comparative data elaboration was applied to separate chemical patterns arising from the interaction between some Mentha species and the herbivore Chrysolina herbacea, also known as the mint bug. Upon feeding on different Mentha species (Mentha spicata L., Mentha × piperita L. and Mentha longifolia L.), C. herbacea produced frass (faeces) which were characterized by a typical volatile fraction. HS-SPME GC×GC-qMS analysis of the complex volatile fraction of both mint leaf and C. herbacea frass was submitted to advanced fingerprinting analysis of 2D chromatographic data. 1,8-Cineole, found in the leaves of all the Mentha species examined, was oxidized, and C. herbacea frass yielded high rates of several hydroxy-1,8-cineoles, including 2α-hydroxy-, 3α-hydroxy-, 3β-hydroxy- and 9-hydroxy-1,8-cineole. Upon insect feeding, several unknown oxidized monoterpenes, a p-menthane diol and three unknown phenylpropanoids were also detected in the frass volatiles. In M. longifolia, the occurrence of the monoterpene piperitenone oxide was found to be toxic and associated with insect death. The results of this work show that high throughput techniques such as HS-SPME and GC×GC-qMS fingerprint analysis are ideal tools to analyze complex volatile matrices, and provide a sensitive method for the direct comparison and chemical visualization of plant and insect emitted volatile components.

  20. Enhancement of phosphorus sorption onto light expanded clay aggregates by means of aluminum and iron oxide coatings.

    Science.gov (United States)

    Yaghi, Nader; Hartikainen, Helinä

    2013-11-01

    Phosphorus (P) loading from non-point or point sources increases the eutrophication risk of natural waters. The functioning of constructed wetlands (CWs) used as natural water treatment systems can be improved by means of additional materials adsorbing soluble P. In this study, light expanded clay aggregates (LECA) and LECA coated with aluminum (Al) oxide (Al-LECA) or iron (Fe) oxide (Fe-LECA) were tested for their efficiency as P sorbents in the pH range 3-8. The oxide coatings duplicated the actual sorption capacity calculated from the sorption isotherms at the P concentration in the equilibrium solution of 20 μg L(-1), assumed to be the allowable P level in purified water. In the oxide-coated LECAs the sorption was fast and followed both the first- and second-order Lagergren kinetic models, suggesting that the formation of a binuclear surface complex was feasible. In LECA, sorption was markedly slower and followed the first-order kinetic model, indicating that retention occurred through a monodentate attachment. These findings were in harmony with the degree of P saturation (DPS) of the sorbent surfaces at the highest P addition level (200 μg L(-1)), DPS being decisively higher for LECA than for the oxide-coated sorbents. Accordingly, at higher pH values the competition by hydroxyl ions diminished the sorption in LECA relatively more than that in the coated sorbents. In agreement with the acidity of Al(3+) being 100 times lower than that of Fe(3+), at elevated pH the sorption by Al-LECA proved to be less reversible than that by Fe-LECA. The results provide evidence that in CWs Al-coated sorbents are superior to Fe-coated ones that are also redox-sensitive and may lose their sorption properties in anoxic conditions. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. Graphene deposited onto aligned zinc oxide nanorods as an efficient coating for headspace solid-phase microextraction of gasoline fractions from oil samples.

    Science.gov (United States)

    Wen, Congying; Li, Mengmeng; Li, Wangbo; Li, Zizhou; Duan, Wei; Li, Yulong; Zhou, Jie; Li, Xiyou; Zeng, Jingbin

    2017-12-29

    The content of gasoline fraction in oil samples is not only an important indicator of oil quality, but also an indispensable fundamental data for oil refining and processing. Before its determination, efficient preconcentration and separation of gasoline fractions from complicated matrices is essential. In this work, a thin layer of graphene (G) was deposited onto oriented ZnO nanorods (ZNRs) as a SPME coating. By this approach, the surface area of G was greatly enhanced by the aligned ZNRs, and the surface polarity of ZNRs was changed from polar to less polar, which were both beneficial for the extraction of gasoline fractions. In addition, the ZNRs were well protected by the mechanically and chemically stable G, making the coating highly durable for use. With headspace SPME (HS-SPME) mode, the G/ZNRs coating can effectively extract gasoline fractions from various oil samples, whose extraction efficiency achieved 1.5-5.4 and 2.1-8.2 times higher than those of a G and commercial 7-μm PDMS coating respectively. Coupled with GC-FID, the developed method is sensitive, simple, cost effective and easily accessible for the analysis of gasoline fractions. Moreover, the method is also feasible for the detection of gasoline markers in simulated oil-polluted water, which provides an option for the monitoring of oil spill accident. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Synthetic sorbents for removal of sulfur dioxide in fluidized-bed coal combustors. [25 refs

    Energy Technology Data Exchange (ETDEWEB)

    Snyder, R.B.; Wilson, W.I.; Johnson, I.; Jonke, A.A.

    1977-06-01

    Synthetic sorbents have been investigated for use in place of limestone for SO/sub 2/ emission control in fluidized-bed coal combustors. Sorbents prepared by impregnation of porous alumina with alkali metal or alkaline earth oxides were studied. The most promising sorbent was found to be calcium oxide in alumina. However, the SO/sub 2/ reactivity of this synthetic sorbent was less than that for a moderately reactive limestone. Hence, a greater quantity of synthetic sorbent would be needed to meet SO/sub 2/ emission standards. The attrition resistance of this synthetic sorbent was found to be greater than that of natural stones; therefore, a larger number of cycles of use would be expected. It is estimated that the use of this synthetic sorbent would reduce the amount of waste sorbent to about one-sixth the amount expected using a moderately reactive once-through limestone. The cost of using this synthetic sorbent is estimated to be about three and a half times the cost expected using once-through limestone. This cost is considered to be too large in view of the expected modest decrease in environmental impact. The synthetic sorbents developed in this study are therefore not considered viable alternatives for limestone in fluidized-bed coal combustors.

  3. Method for removing metal ions from solution with titanate sorbents

    Science.gov (United States)

    Lundquist, Susan H.; White, Lloyd R.

    1999-01-01

    A method for removing metal ions from solution comprises the steps of providing titanate particles by spray-drying a solution or slurry comprising sorbent titanates having a particle size up to 20 micrometers, optionally in the presence of polymer free of cellulose functionality as binder, said sorbent being active towards heavy metals from Periodic Table (CAS version) Groups IA, IIA, IB, IIB, IIIB, and VIII, to provide monodisperse, substantially spherical particles in a yield of at least 70 percent of theoretical yield and having a particle size distribution in the range of 1 to 500 micrometers. The particles can be used free flowing in columns or beds, or entrapped in a nonwoven, fibrous web or matrix or a cast porous membrane, to selectively remove metal ions from aqueous or organic liquid.

  4. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir Gupta; Alejandro Lopez-Ortiz

    2001-01-01

    Four grades of sodium bicarbonate and two grades of trona were characterized in terms of particle size distribution, surface area, pore size distribution, and attrition. Surface area and pore size distribution determinations were conducted after calcination of the materials. The sorbent materials were subjected to thermogravimetric testing to determine comparative rates and extent of calcination (in inert gas) and sorption (in a simulated coal combustion flue gas mixture). Selected materials were exposed to five calcination/sorption cycles and showed no decrease in either sorption capacity or sorption rate. Process simulations were conducted involving different heat recovery schemes. The process is thermodynamically feasible. The sodium-based materials appear to have suitable physical properties for use as regenerable sorbents and, based on thermogravimetric testing, are likely to have sorption and calcination rates that are rapid enough to be of interest in full-scale carbon sequestration processes.

  5. Simultaneous removal of As, Cd, Cr, Cu, Ni and Zn from stormwater using high-efficiency industrial sorbents: Effect of pH, contact time and humic acid

    DEFF Research Database (Denmark)

    Genc-Fuhrman, Hülya; Mikkelsen, Peter Steen; Ledin, Anna

    2016-01-01

    The effect of contact time, solution pH, and the presence of humic acid (HA) on the combined removal of As, Cd, Cr, Cu, Ni and Zn is investigated in batch tests using alumina, granulated activated carbon (GAC), and bauxsol coated sand (BCS) as sorbents. It is found that the equilibrium time for Cd...... their removal. The presence of both 20 and 100 mg/L HA suppressed the heavy metal removal except for Cr, and the suppression was higher at the higher HA concentration. Geochemical simulations suggest that this is due to the formation of dissolved HA-metal complexes preventing effective metal sorption...

  6. Amine enriched solid sorbents for carbon dioxide capture

    Science.gov (United States)

    Gray, McMahan L.; Soong, Yee; Champagne, Kenneth J.

    2003-04-15

    A new method for making low-cost CO.sub.2 sorbents that can be used in large-scale gas-solid processes. The new method entails treating a solid substrate with acid or base and simultaneous or subsequent treatment with a substituted amine salt. The method eliminates the need for organic solvents and polymeric materials for the preparation of CO.sub.2 capture systems.

  7. Durable zinc ferrite sorbent pellets for hot coal gas desulfurization

    Science.gov (United States)

    Jha, Mahesh C.; Blandon, Antonio E.; Hepworth, Malcolm T.

    1988-01-01

    Durable, porous sulfur sorbents useful in removing hydrogen sulfide from hot coal gas are prepared by water pelletizing a mixture of fine zinc oxide and fine iron oxide with inorganic and organic binders and small amounts of activators such as sodium carbonate and molybdenite; the pellets are dried and then indurated at a high temperature, e.g., 1800.degree. C., for a time sufficient to produce crush-resistant pellets.

  8. Retention of 131I volatilized from aqueous solutions by sorbents

    International Nuclear Information System (INIS)

    Deuber, H.

    1985-02-01

    By far the largest proportion of the I-131 that was volatilized from alkaline aqueous solutions was in a form whose retention by various sorbents was lower than that of I 2 , but higher than that of CH 3 I. This form is called 'HOI' although no direct identification exists. With all the fresh impregnated activated carbons investigated, the retention of 'HOI' was higher than 99% at a residence time of 0.1 s. The influence of purging was insignificant. (orig.) [de

  9. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    International Nuclear Information System (INIS)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO(sub 2) as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbents being investigated in this project are primarily alkali carbonates, and particularly sodium carbonate and potassium carbonate, which are converted to bicarbonates, through reaction with carbon dioxide and water vapor. Bicarbonates are regenerated to carbonates when heated, producing a nearly pure CO(sub 2) stream after condensation of water vapor. This quarter, electrobalance tests conducted at LSU indicated that exposure of sorbent to water vapor prior to contact with carbonation gas does not significantly increase the reaction rate. Calcined fine mesh trona has a greater initial carbonation rate than calcined sodium bicarbonate, but appears to be more susceptible to loss of reactivity under severe calcination conditions. The Davison attrition indices for Grade 5 sodium bicarbonate, commercial grade sodium carbonate and extra fine granular potassium carbonate were, as tested, outside of the range suitable for entrained bed reactor testing. Fluidized bed testing at RTI indicated that in the initial stages of reaction potassium carbonate removed 35% of the carbon dioxide in simulated flue gas, and is reactive at higher temperatures than sodium carbonate. Removals declined to 6% when 54% of the capacity of the sorbent was exhausted. Carbonation data from electrobalance testing was correlated using a shrinking core reaction model. The activation energy of the reaction of sodium carbonate with carbon dioxide and water vapor was determined from nonisothermal thermogravimetry

  10. Partitioning of the pesticide trifluralin between dissolved organic matter and water using automated SPME-GC/MS

    KAUST Repository

    Caupos, Emilie

    2014-10-04

    Solid-phase microextraction (SPME) was used to determine the equilibrium association constant for a pesticide, trifluralin (TFR), with dissolved organic matter (DOM). After optimization of the SPME method for the analysis of TFR, partition coefficients (K DOM) with three different sources of DOM were determined in buffered solutions at pH 7. Commercial humic acids and DOM fractions isolated from two surface waters were used. The values of log K DOMvaried from 4.3 to 5.8, depending on the nature of the organic material. A good correlation was established between log K DOMand DOM properties (as measured with the H/O atomic ratio and UV absorbance), in agreement with literature data. This is consistent with the effect of polarity and aromaticity for governing DOM-pollutant associations, regardless of the origin of DOM. This association phenomenon is relevant to better understand the behavior of pesticides in the environment since it controls part of pesticide leaching and fate in aquatic systems.

  11. Development of an SPME-GC-MS/MS method for the determination of pesticides in rainwater: Laboratory and field experiments

    International Nuclear Information System (INIS)

    Sauret-Szczepanski, Nathalie; Mirabel, Philippe; Wortham, Henri

    2006-01-01

    A solid-phase microextraction - coupled to a gas chromatography - ion trap tandem mass spectrometry (SPME-GC-MS/MS) method was developed for the quantitative determination in rainwater of 8 pesticides amongst the most used in France and 3 triazines metabolites. The main factors affecting the SPME process were studied. Using a 3 mL sample, the method developed showed good linearity for concentrations ranging from 0.05 to 50 μg L -1 with correlation coefficients between 0.997 and 0.9999 and relative standard deviations (% RSD) below 14%. The study of matrix effects showed that rainwater was too diluted to have any significant influence on the extraction efficiency. To validate the method, a field campaign was carried out on the rain events, which occurred in Strasbourg during a one-year period. The rain concentrations showed patterns of high pesticide concentrations during spring months, which were correlated to the spraying periods of most of these substances. - Solid-phase microextraction efficiency of pesticides in rainwater was optimized

  12. Characterisation of the volatile profile of coconut water from five varieties using an optimised HS-SPME-GC analysis.

    Science.gov (United States)

    Prades, Alexia; Assa, Rebecca Rachel Ablan; Dornier, Manuel; Pain, Jean-Pierre; Boulanger, Renaud

    2012-09-01

    Coconut (Cocos nucifera L.) water is a refreshing tropical drink whose international market has recently been growing. However, little is yet known about its physicochemical composition, particularly its aroma. This study set out to characterise the volatile profile of water from five coconut varieties. Aroma compounds were characterised by headspace solid phase microextraction gas chromatography (HS-SPME-GC) analysis. An experimental design was established to optimise SPME conditions, leading to an equilibration time of 10 min followed by an extraction time of 60 min at 50 °C. Accordingly, immature coconut water from WAT (West African Tall), PB121 (MYD × WAT Hybrid), MYD (Malayan Yellow Dwarf), EGD (Equatorial Guinea Green Dwarf) and THD (Thailand Aromatic Green Dwarf) palms was analysed and described. Ketones were mainly present in the Tall and Hybrid varieties, whereas aldehydes were most abundant in the Dwarf palms. Tall coconut water was characterised by a high lactone content. THD exhibited a high ethyl octanoate level. The cluster analysis of the volatile fraction from the five coconut cultivars was found to be related to their genetic classification. The volatile compounds of immature coconut water from five varieties were characterised for the first time. Volatile profile analysis could be a useful tool for the selection of Dwarf coconut varieties, which are mainly consumed as a beverage. Copyright © 2012 Society of Chemical Industry.

  13. Development of an SPME-GC-MS/MS method for the determination of pesticides in rainwater: Laboratory and field experiments

    Energy Technology Data Exchange (ETDEWEB)

    Sauret-Szczepanski, Nathalie [Equipe de Physico-chimie de l' Atmosphere, Centre de Geochimie de la Surface (UMR 7517) 1, rue Blessig, 67084 Strasbourg Cedex (France)]. E-mail: nathalie.sauret-szczepanski@alcan.com; Mirabel, Philippe [Equipe de Physico-chimie de l' Atmosphere, Centre de Geochimie de la Surface (UMR 7517) 1, rue Blessig, 67084 Strasbourg Cedex (France); Wortham, Henri [Universite de Provence, Laboratoire Chimie et Environnement, Case 29, 3 Place Victor Hugo, 13331 Marseille Cedex (France)]. E-mail: wortham@up.univ-mrs.fr

    2006-01-15

    A solid-phase microextraction - coupled to a gas chromatography - ion trap tandem mass spectrometry (SPME-GC-MS/MS) method was developed for the quantitative determination in rainwater of 8 pesticides amongst the most used in France and 3 triazines metabolites. The main factors affecting the SPME process were studied. Using a 3 mL sample, the method developed showed good linearity for concentrations ranging from 0.05 to 50 {mu}g L{sup -1} with correlation coefficients between 0.997 and 0.9999 and relative standard deviations (% RSD) below 14%. The study of matrix effects showed that rainwater was too diluted to have any significant influence on the extraction efficiency. To validate the method, a field campaign was carried out on the rain events, which occurred in Strasbourg during a one-year period. The rain concentrations showed patterns of high pesticide concentrations during spring months, which were correlated to the spraying periods of most of these substances. - Solid-phase microextraction efficiency of pesticides in rainwater was optimized.

  14. Cadmium(II)-based metal-organic nanotubes as solid-phase microextraction coating for ultratrace-level analysis of polychlorinated biphenyls in seawater samples.

    Science.gov (United States)

    Sheng, Wan-Ru; Chen, Yue; Wang, Shan-Shan; Wang, Xiao-Li; Wang, Ming-Lin; Zhao, Ru-Song

    2016-11-01

    In this study, stable cadmium(II)-based metal-organic nanotubes (Cd-MONTs) were prepared and used as a coating material for solid-phase microextraction (SPME) of polychlorinated biphenyls (PCBs) from environmental water samples. The as-prepared Cd-MONT SPME coating material was characterized by thermal gravimetric analysis, scanning electron microscopy, and X-ray diffraction. The synthesized Cd-MONTs exhibited high thermal stability (385 °C) and excellent extraction performance toward PCBs. The important conditions were optimized systematically by the response surface method. Under the optimal conditions, the new fiber achieved high enrichment factors (938-3417), low limits of detection (1.80-8.73 pg L -1 ), and wide linearity (10-5000 pg L -1 ). The method developed was used in ultratrace-level analysis of PCBs in seawater samples, with satisfactory results for each sample.

  15. Ionic liquids: solvents and sorbents in sample preparation.

    Science.gov (United States)

    Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

    2018-01-01

    The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; Alejandro Lopez-Ortiz; Douglas P. Harrison; Ya Liang

    2001-07-01

    Sodium based sorbents including sodium carbonate may be used to capture carbon dioxide from flue gas. A relatively concentrated carbon dioxide stream may be recoverable for sequestration when the sorbent is regenerated. Electrobalance tests indicated that sodium carbonate monohydrate was formed in a mixture of helium and water vapor at temperatures below 65 C. Additional compounds may also form, but this could not be confirmed. In the presence of carbon dioxide and water vapor, both the initial reaction rate of sodium carbonate with carbon dioxide and water and the sorbent capacity decreased with increasing temperature, consistent with the results from the previous quarter. Increasing the carbon dioxide concentration at constant temperature and water vapor concentration produced a measurable increase in rate, as did increasing the water vapor concentration at constant carbon dioxide concentration and temperature. Runs conducted with a flatter TGA pan resulted in a higher initial reaction rate, presumably due to improved gas-solid contact, but after a short time, there was no significant difference in the rates measured with the different pans. Analyses of kinetic data suggest that the surface of the sodium carbonate particles may be much hotter than the bulk gas due to the highly exothermic reaction with carbon dioxide and water, and that the rate of heat removal from the particle may control the reaction rate. A material and energy balance was developed for a cyclic carbonation/calcination process which captures about 26 percent of the carbon dioxide present in flue gas available at 250 C.

  17. Oil sorbents with high sorption capacity, oil/water selectivity and reusability for oil spill cleanup.

    Science.gov (United States)

    Wu, Daxiong; Fang, Linlin; Qin, Yanmin; Wu, Wenjuan; Mao, Changming; Zhu, Haitao

    2014-07-15

    A sorbent for oil spill cleanup was prepared through a novel strategy by treating polyurethane sponges with silica sol and gasoline successively. The oil sorption capacity, oil/water selectivity, reusability and sorption mechanism of prepared sorbent were studied. The results showed that the prepared sorbent exhibited high sorption capacity and excellent oil/water selectivity. 1g of the prepared sorbent could adsorb more than 100 g of motor oil, while it only picks up less than 0.1 g of water from an oil-water interface under both static and dynamic conditions. More than 70% of the sorption capacity remained after 15 successive sorption-squeezing cycles, which suggests an extraordinary high reusability. The prepared sorbent is a better alternative of the commercial polypropylene sorbent which are being used nowadays. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Biomass-Derived Porous Carbonaceous Aerogel as Sorbent for Oil-Spill Remediation.

    Science.gov (United States)

    Wang, Zhuqing; Jin, Pengxiang; Wang, Min; Wu, Genhua; Dong, Chen; Wu, Aiguo

    2016-12-07

    We prepared a cost-effective, environmentally friendly carbonaceuous oil sorbent with a lotus effect structure using a simple one-pot hydrothermal reaction and a mild modification process. The carbonaceous oil sorbent can rapidly, efficiently, and continuously collect oil in situ from a water surface. This sorbent was unlike traditional sorbents because it was not dependent on the weight and volume of the sorption material. The sorbent was also successfully used to separate and collect crude oil from the water surface and can collect organic solvents underwater. This novel oil sorbent and oil-collection device can be used in case of emergency for organic solvent leakages, as well as leakages in tankers and offshore drilling platforms.

  19. Dual layer hollow fiber sorbents for trace H2S removal from gas streams

    KAUST Repository

    Bhandari, Dhaval A.

    2013-05-01

    Hollow fiber sorbents are pseudo monolithic materials with potential use in various adsorption based applications. Dual layer hollow fiber sorbents have the potential to allow thermal regeneration without direct contact of the regeneration fluid with the sorbent particles. This paper considers the application of dual layer hollow fiber sorbents for a case involving trace amounts of H2S removal from a simulated gas stream and offers a comparison with single layer hollow fiber sorbents. The effect of spin dope composition and core layer zeolite loading on the gas flux, H2S transient sorption capacity and pore structure are also studied. This work can be used as a guide to develop and optimize dual layer hollow fiber sorbent properties beyond the specific example considered here. © 2013 Elsevier Ltd.

  20. New ZnO-Based Regenerable Sulfur Sorbents for Fluid-Bed/Transport Reactor Applications

    Energy Technology Data Exchange (ETDEWEB)

    Slimane, R.B.; Lau, F.S.; Abbasian, J.; Ho, K.H.

    2002-09-19

    The overall objective of the ongoing sorbent development work at GTI is the advancement to the demonstration stage of a promising ZnO-TiO2 sulfur sorbent that has been developed under DCCA/ICCI and DOE/NETL sponsorship. This regenerable sorbent has been shown to possess an exceptional combination of excellent chemical reactivity, high effective capacity for sulfur absorption, high resistance to attrition, and regenerability at temperatures lower than required by typical zinc titanates.

  1. Advanced Utility Mercury-Sorbent Field-Testing Program

    Energy Technology Data Exchange (ETDEWEB)

    Ronald Landreth

    2007-12-31

    This report summarizes the work conducted from September 1, 2003 through December 31, 2007 on the project entitled Advanced Utility Mercury-Sorbent Field-Testing Program. The project covers the testing at the Detroit Edison St. Clair Plant and the Duke Power Cliffside and Buck Stations. The St. Clair Plant used a blend of subbituminous and bituminous coal and controlled the particulate emissions by means of a cold-side ESP. The Duke Power Stations used bituminous coals and controlled their particulate emissions by means of hot-side ESPs. The testing at the Detroit Edison St. Clair Plant demonstrated that mercury sorbents could be used to achieve high mercury removal rates with low injection rates at facilities that burn subbituminous coal. A mercury removal rate of 94% was achieved at an injection rate of 3 lb/MMacf over the thirty day long-term test. Prior to this test, it was believed that the mercury in flue gas of this type would be the most difficult to capture. This is not the case. The testing at the two Duke Power Stations proved that carbon- based mercury sorbents can be used to control the mercury emissions from boilers with hot-side ESPs. It was known that plain PACs did not have any mercury capacity at elevated temperatures but that brominated B-PAC did. The mercury removal rate varies with the operation but it appears that mercury removal rates equal to or greater than 50% are achievable in facilities equipped with hot-side ESPs. As part of the program, both sorbent injection equipment and sorbent production equipment was acquired and operated. This equipment performed very well during this program. In addition, mercury instruments were acquired for this program. These instruments worked well in the flue gas at the St. Clair Plant but not as well in the flue gas at the Duke Power Stations. It is believed that the difference in the amount of oxidized mercury, more at Duke Power, was the difference in instrument performance. Much of the equipment was

  2. Attrition resistant catalysts and sorbents based on heavy metal poisoned FCC catalysts

    Science.gov (United States)

    Gangwal, Santosh; Jothimurugesan, Kandaswamy

    1999-01-01

    A heavy metal poisoned, spent FCC catalyst is treated by chemically impregnating the poisoned catalyst with a new catalytic metal or metal salt to provide an attrition resistant catalyst or sorbent for a different catalytic or absorption processes, such as catalysts for Fischer-Tropsh Synthesis, and sorbents for removal of sulfur gasses from fuel gases and flue-gases. The heavy metal contaminated FCC catalyst is directly used as a support for preparing catalysts having new catalytic properties and sorbents having new sorbent properties, without removing or "passivating" the heavy metals on the spent FCC catalyst as an intermediate step.

  3. Assessment of hydrophobic organic contaminant availability in sediments after sorbent amendment and its complete removal.

    Science.gov (United States)

    Wu, Yanwen; Cho, Yeo-Myoung; Luthy, Richard G; Kim, Kibeum; Jung, Jihyeun; Gala, William R; Choi, Yongju

    2017-12-01

    Sorbents amended to sediments in situ for sequestration of hydrophobic organic contaminants (HOCs) may be swept away from the treated sites due to hydrodynamic forces applied to the sediment surface. The purpose of this study is to examine the possibility of recovery of HOC availability in sorbent-amended sediment after complete removal of the sorbent. Sediment contact with an easily separable model sorbent Tenax beads for 28 days in a slurry phase resulted in 74-98% reduction in polycyclic aromatic hydrocarbon and polychlorinated biphenyl availability compared to the untreated controls. HOC availability in the sorbent-treated sediment slightly increased by sorbent removal and after one month of mixing in a slurry phase because the slowly-desorbing HOC fraction was released and repartitioned back to the sediment, partially replenishing the rapidly-desorbing HOC fraction. However, HOC availability did not further increase during an extended mixing period of 12 months suggesting that the repartitioning process was not an infinite source. HOC availability after the 12-month post-treatment mixing for the sorbent-treated sediment was 53-97% lower than that of the untreated sediment because of the combined effect of HOC mass removal from sediment (with the sorbent) and incomplete recovery of available HOC fraction in the sorbent-treated sediment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Sulphation of CaO-Based Sorbent Modified in CO2 Looping Cycles

    Science.gov (United States)

    Manovic, Vasilije; Anthony, Edward J.; Loncarevic, Davor

    CaO-based looping cycles for CO2 capture at high temperatures are based on cyclical carbonation of CaO and regeneration of CaCO3. The main limitation of natural sorbents is the loss of carrying capacity with increasing numbers of reaction cycles, resulting in spent sorbent ballast. Use of spent sorbent from CO2 looping cycles for SO2 capture is a possible solution investigated in this study. Three limestones were investigated: Kelly Rock (Canada), La Blanca (Spain) and Katowice (Poland). Carbonation/calcination cycles were performed in a tube furnace with original limestones and samples thermally pretreated for different times (i.e., sintered). The spent sorbent samples were sulphated in a thermogravimetric analyzer. Changes in the resulting pore structure were then investigated using mercury porosimetry. Final conversions of both spent and pretreated sorbents after longer sulphation times were comparable or higher than those observed for the original sorbents. Maximum sulphation levels strongly depend on sorbent porosity and pore surface area. The shrinkage of sorbent particles during calcination/cycling resulted in a loss of sorbent porosity (≤48%), which corresponds to maximum sulphation levels ˜55% for spent Kelly Rock and Katowice. However, this is ˜10% higher than for the original samples. By contrast, La Blanca limestone had more pronounced particle shrinkage during pretreatment and cycling, leading to lower porosity, Katowice samples final conversions are determined by the total pore volume available for the bulky CaSO4 product.

  5. IMMOBILIZATION OF MICROALGAE ON THE SURFACE OF NEW CROSS-LINKED POLYETHYLENIMINE-BASED SORBENTS.

    Science.gov (United States)

    Vasilieva, Svetlana; Shibzukhova, Karina; Morozov, Alexey; Solovchenko, Alexei; Bessonov, Ivan; Kopitsyna, Maria; Lukyanov, Alexander; Chekanov, Konstantin; Lobakova, Elena

    2018-04-11

    We report on the use of the polyethylenimine-based (PEI) sorbents for immobilization and harvesting of microalgae (MA) cells. Specific materials assessed were porous solid polymers from highly-branched PEI synthesized by cross-linking with epichlorohydrin (ECH) or diethylene glycol diglycidyl ether (DGDE). We estimated the effect of PEI/cross-linker ratio on the MA attachment and biocompatibility of the sorbents with the MA cells. A decrease in the cross-linker percentage resulted in the enhancement of the immobilization efficiency but impaired the cell viability as was manifested by inhibition of the photosynthetic activity of the MA cells. The rate of Chlorella vulgaris cell attachment to the sorbents with ECH was faster as compared to that of the PEI-DGDE-based polymers. The cells immobilized on the PEI-ECH sorbents showed a more profound decline in their viability (assessed via photosynthetic activity). The sorbents with 60% of DGDE were characterized by high immobilization efficiency. These sorbents supported a prolonged cultivation of the immobilized MA without impairing their viability and metabolic activity. We conclude that the sorbents with a lower percentage of DGDE (<30%) and sorbents with ECH are suitable for harvesting of the MA cells intended for immediate downstream processing, potentially without the cell desorption. To the best of our knowledge, this is the first report on successful application of PEI-based sorbents in microalgal biotechnology. Copyright © 2018 Elsevier B.V. All rights reserved.

  6. Dispersive solid-phase extraction using polyaniline-modified zeolite NaY as a new sorbent for multiresidue analysis of pesticides in food and environmental samples.

    Science.gov (United States)

    Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

    2017-03-01

    The applicability of polyaniline (PANI)-modified zeolite NaY as a sorbent for multi-class pesticides extraction was investigated. The sorbent had a sorption capacity of 833mgkg -1 sorbent and preconcentration factor of 42 in the mixture of twenty pesticides. The PANI-coated zeolite NaY was successfully created via oxidative polymerization of aniline onto the surface of the zeolite. The sorbent was applied for dispersive solid phase extraction (DSPE) of commonly used pesticides belonging to five different chemical groups, involving carbamate, organophosphate, sulfonylurea, pyrethroid and neonicotinoid. The coupling of DSPE and HPLC-PDA resulted in an efficient method for multiresidue analysis of pesticides. The proposed method gave LODs and LOQs in the ranges of 0.001-1.00mgL -1 and 0.005-2.50mgL -1 , respectively. The method was applied for determination of pesticide residues in environmental and food samples including drinking water, pond waters, soils, honey, cabbages, cucumbers, tomatoes and strawberries which were collected in Khon Kaen Province, Thailand. Recoveries of the target pesticides were in the range of 64-128% with RSDs less than 12% using matrix matched calibration for all sample matrices. Eight pesticides were found in fruit and vegetable samples at concentrations of 0.003-0.033mgkg -1 whereas a few compounds in contaminated pond waters have concentrations of 0.046-0.092mgL -1 . The occurrence of high concentration of up to 1.26mgkg -1 in the soil samples is noteworthy. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO{sub 2} as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, or ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO{sub 2} stream after condensation of water vapor. This quarter, five cycle thermogravimetric tests were conducted at the Louisiana State University (LSU) with sodium bicarbonate Grade 3 (SBC{number_sign}3) which showed that carbonation activity declined slightly over 5 cycles following severe calcination conditions of 200 C in pure CO{sub 2}. Three different sets of calcination conditions were tested. Initial carbonation activity (as measured by extent of reaction in the first 25 minutes) was greatest subsequent to calcination at 120 C in He, slightly less subsequent to calcination in 80% CO{sub 2}/20% H{sub 2}O, and lowest subsequent to calcination in pure CO{sub 2} at 200 C. Differences in the extent of reaction after 150 minutes of carbonation, subsequent to calcination under the same conditions followed the same trend but were less significant. The differences between fractional carbonation under the three calcination conditions declined with increasing cycles. A preliminary fixed bed reactor test was also conducted at LSU. Following calcination, the sorbent removed approximately 19% of the CO{sub 2} in the simulated flue gas. CO{sub 2} evolved during subsequent calcination was consistent with an extent of carbonation of approximately 49%. Following successful testing of SBC{number_sign}3 sorbent at RTI reported in the last quarter, a two cycle fluidized bed reactor test was conducted with trona as the sorbent precursor, which was calcined to sodium carbonate. In the first

  8. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    International Nuclear Information System (INIS)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; William J. McMichael; Douglas P. Harrison; Ya Liang

    2002-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO(sub 2) as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, or ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO(sub 2) stream after condensation of water vapor. This quarter, five cycle thermogravimetric tests were conducted at the Louisiana State University (LSU) with sodium bicarbonate Grade 3 (SBC(number s ign)3) which showed that carbonation activity declined slightly over 5 cycles following severe calcination conditions of 200 C in pure CO(sub 2). Three different sets of calcination conditions were tested. Initial carbonation activity (as measured by extent of reaction in the first 25 minutes) was greatest subsequent to calcination at 120 C in He, slightly less subsequent to calcination in 80% CO(sub 2)/20% H(sub 2)O, and lowest subsequent to calcination in pure CO(sub 2) at 200 C. Differences in the extent of reaction after 150 minutes of carbonation, subsequent to calcination under the same conditions followed the same trend but were less significant. The differences between fractional carbonation under the three calcination conditions declined with increasing cycles. A preliminary fixed bed reactor test was also conducted at LSU. Following calcination, the sorbent removed approximately 19% of the CO(sub 2) in the simulated flue gas. CO(sub 2) evolved during subsequent calcination was consistent with an extent of carbonation of approximately 49%. Following successful testing of SBC(number s ign)3 sorbent at RTI reported in the last quarter, a two cycle fluidized bed reactor test was conducted with trona as the sorbent precursor, which was calcined to sodium carbonate. In the first carbonation cycle, CO

  9. Influence of fibre coating in headspace solid-phase microextraction-gas chromatographic analysis of aromatic and medicinal plants.

    Science.gov (United States)

    Bicchi, C; Drigo, S; Rubiolo, P

    2000-09-15

    Solid-phase microextraction (SPME) is a solvent-free technique, which is well established in headspace analysis since it is sensitive, because of the concentration factor achieved by the fibres, and selective, because of different coating materials which can be used. The performance of eight commercially available SPME fibres was compared to evaluate the recoveries of some characteristic components with different polarities and structures present in the headspace of four aromatic and medicinal plants: rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.), thyme (Thymus vulgaris L.) and valerian (Valeriana officinalis L.). The relative concentration capacity of each fibre on the same components of each plant was also determined by comparing their abundance with that obtained by classical static-headspace GC. The partition coefficient, K1, between the headspace gaseous phase and SPME polymeric coating, and the relative concentration factors, of some of the characteristic components of the plant investigated dissolved in dibutyl phtalate, were also determined, under rigorously standardised analysis conditions. The results showed that the most effective fibres were those consisting of two components, i.e., a liquid phase (polydimethylsiloxane) and a porous solid (carboxen or divinylbenzene, or both).

  10. Preparation of silica-magnetite nanoparticle mixed hemimicelle sorbents for extraction of several typical phenolic compounds from environmental water samples.

    Science.gov (United States)

    Zhao, Xiaoli; Shi, Yali; Wang, Thanh; Cai, Yaqi; Jiang, Guibin

    2008-04-25

    A novel type of superparamagnetic silica-coated (Fe3O4/SiO2 core/shell) magnetite nanoparticle modified by surfactants has been successfully synthesized and was applied as an effective sorbent material for the pre-concentration of several typical phenolic compounds (bisphenol A (BPA), 4-tert-octylphenol (4-OP) and 4-n-nonylphenol (4-NP)) from environmental water samples. Compared with pure magnetic particles, a thin and dense silica layer would protect the iron oxide core from leaching out in acidic conditions. In order to enhance their adsorptive tendency towards organic compounds, cetylpyridinium chloride (CPC) or cetyltrimethylammonium bromide (CTAB) were added, which adsorbed on the surface of the Fe3O4/SiO2 nanoparticles (Fe3O4/SiO2 NPs) and formed mixed hemimicelles. Main factors affecting the adsolubilization of analytes were optimized and comparative study on the use of CPC and CTAB-coated Fe3O4/SiO2 NPs mixed hemimicelles-based SPE was also carried out. CPC-coated Fe3O4/SiO2 NPs system was selected due to lower elution volume required and more effective adsorption of the target compounds. Under selected conditions, concentration factor of 1600 was achieved by using this method to extract 800 mL of different environmental water samples. The detection limits obtained for BPA, 4-OP and 4-NP with HPLC-FLD were 7, 14, and 20 ng/L, respectively.

  11. Comparative DNA isolation behaviours of silica and polymer based sorbents in batch fashion: monodisperse silica microspheres with bimodal pore size distribution as a new sorbent for DNA isolation.

    Science.gov (United States)

    Günal, Gülçin; Kip, Çiğdem; Eda Öğüt, S; İlhan, Hasan; Kibar, Güneş; Tuncel, Ali

    2018-02-01

    Monodisperse silica microspheres with bimodal pore-size distribution were proposed as a high performance sorbent for DNA isolation in batch fashion under equilibrium conditions. The proposed sorbent including both macroporous and mesoporous compartments was synthesized 5.1 μm in-size, by a "staged shape templated hydrolysis and condensation method". Hydrophilic polymer based sorbents were also obtained in the form of monodisperse-macroporous microspheres ca 5.5 μm in size, with different functionalities, by a developed "multi-stage microsuspension copolymerization" technique. The batch DNA isolation performance of proposed material was comparatively investigated using polymer based sorbents with similar morphologies. Among all sorbents tried, the best DNA isolation performance was achieved with the monodisperse silica microspheres with bimodal pore size distribution. The collocation of interconnected mesoporous and macroporous compartments within the monodisperse silica microspheres provided a high surface area and reduced the intraparticular mass transfer resistance and made easier both the adsorption and desorption of DNA. Among the polymer based sorbents, higher DNA isolation yields were achieved with the monodisperse-macroporous polymer microspheres carrying trimethoxysilyl and quaternary ammonium functionalities. However, batch DNA isolation performances of polymer based sorbents were significantly lower with respect to the silica microspheres.

  12. Magnetic materials as sorbents for metal/metalloid preconcentration and/or separation. A review.

    Science.gov (United States)

    Giakisikli, Georgia; Anthemidis, Aristidis N

    2013-07-30

    The use of magnetic materials in solid phase extraction has received considerable attention in recent years taking into account many advantages arising from the inherent characteristics of magnetic particles. Magnetic solid phase extraction (MSPE) methodology overcomes problems such as column packing and phase separation, which can be easily performed by applying an external magnetic field. The use of magnetic particles in automatic systems is growing over the last few years making the on-line operation of MSPE a promising technique in the frame of green chemistry. This article aims to provide all recent progress in the research of novel magnetic materials as sorbents for metal preconcentration and determination coupled with different detection systems as well as their implementation in sequential injection and microfluidic systems. In addition, a description of preparation, characterization as well as applications of various types of magnetic materials, either with organic or inorganic coating of the magnetic core, is presented. Concluding remarks and future trends are also commented. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Chapter 4. Cross-linked polymers of ethynyl-piperidol as sorbents for removing endogenous toxins from biological fluids. 4.1. Sorbents for endogenous toxins and increasing their hemo compatibility and selectivity

    International Nuclear Information System (INIS)

    Khalikov, D.Kh.

    2012-01-01

    Sorbents for endogenous toxins, including different types of activated carbons were considered. Different methods of creation of hemo compatible sorbents based on various classes of ion exchangers were considered as well.

  14. Sol-gel-based SPME fiber as a reliable sampling technique for studying biogenic volatile organic compounds released from Clostridium tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2017-11-01

    A novel and efficient headspace solid-phase microextraction (HS-SPME) method, followed by gas chromatography mass spectrometry (GC-MS), was developed to study volatile organic compounds (VOCs) emerging from microorganisms. Two homemade SPME fibers, a semi-polar poly (dimethylsiloxane) (PDMS) fiber, and a polar polyethylene glycol (PEG) fiber, along with two commercial fibers (PDMS and PDMS/DVB) were used to collect VOCs emerging from Clostridium tetani which was cultured in different media. The adsorbed VOCs were desorbed and identified, in vitro, using GC-MS. The adsorption efficiency was improved by optimizing the time duration of adsorption and desorption. About 50 components were identified by the proposed method. The main detected compounds appeared to be sulfur containing compounds such as butanethioic acid S-methyl ester, dimethyl trisulfide, and dimethyl tetrasulfide. These volatile sulfur containing compounds are derived from amino acids containing the sulfur element, which probably coexist in the mentioned bacterium or are added to the culture media. The developed HS-SPME-GC-MS method allowed the determination of the chemical fingerprint of Clostridium tetani volatile constituents, and thus provides a new, simple, and reliable tool for studying the growth of microorganisms. Graphical abstract Investigation of biogenic VOCs released from Clostridium tetani using SPME-GC-MS.

  15. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    Science.gov (United States)

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  16. Multivariate statistical analysis of hemlock (Tsuga) volatiles by SPME/GC/MS: insights into the phytochemistry of the hemlock woolly adelgid (Adelges tsugae Annand)

    Science.gov (United States)

    Anthony Lagalante; Frank Calvosa; Michael Mirzabeigi; Vikram Iyengar; Michael Montgomery; Kathleen Shields

    2007-01-01

    A previously developed single-needle, SPME/GC/MS technique was used to measure the terpenoid content of T. canadensis growing in a hemlock forest at Lake Scranton, PA (Lagalante and Montgomery 2003). The volatile terpenoid composition was measured over a 1-year period from June 2003 to May 2004 to follow the annual cycle of foliage development from...

  17. KINETICS OF Mn-BASED SORBENTS FOR HOT COAL GAS DESULFURIZATION

    Energy Technology Data Exchange (ETDEWEB)

    J.J. BERNS; K.A. SADECKI; M.T. HEPWORTH

    1997-09-15

    Mixed manganese oxide sorbents have been investigated for high-temperature removal of hydrogen sulfide (the primary sulfur bearing compound) from hot coal gases. The sorbents were screened by thermodynamic equilibrium considerations for sulfidation. Preliminary experimental work using thermogravimetric analysis (TGA) indicated titania to be a superior substrate than alumina. Four formulations showing superior reactivity in a TGA were then tested in an ambient pressure fixed-bed reactor to determine steady state H 2 S concentrations, breakthrough times and effectiveness of the sorbent when subjected to cyclic sulfidation and regeneration testing. Eight tests were conducted with each test consisting of five cycles of sulfidation and regeneration. Sulfidation occurred at 600 o C using a simulated coal gas at an empty-bed space velocity of approximately 12,000 per hour. Manganese-based sorbents with molar ratios > 1:1 Mn:Substrate were effective in reducing the H 2 S concentration in simulated coal gases to less than 100 ppmv over five cycles. Actual breakthrough time for formulation C6-2-1100 was as high as 73% of breakthrough time based on wt% Mn in sorbent at 600 o C. Regeneration tests determined that loaded pellets can be essentially completely regenerated in an air/steam mixture at 750 o C with minimal sulfate formation. The leading formulation (designated C6-2) from the fixed-bed tests was then further tested under varying sorbent induration temperature, sulfidation temperature and superficial gas velocity. Four tests were conducted with each test consisting of four cycles of sulfidation and regeneration. Results showed that the induration temperature of the sorbent and the reaction temperature greatly affected the H 2 S removal capacity of the sorbent while the superficial gas velocity between 1090 and 1635 cm/min had minimal affect on the sorbent's breakthrough capacity. Testing showed that the sorbent's strength was a strong function of the sorbent

  18. Caracterización de los compuestos del aroma en rones colombianos por HS-SPME-GC-MS-O

    Directory of Open Access Journals (Sweden)

    Jazmín Osorio Monsalve

    2016-11-01

    Full Text Available Se identificaron por primera vez 46 compuestos volátiles olfativamente activos con actividad aromática significativa presentes en rones comerciales de Colombia. Lo anterior, mediante microextracción en fase sólida en modo espacio de cabeza (HS-SPME, acoplada a cromatografía de gases con detectores de espectrometría de masas y olfatometría (GC-MS-O. Dentro de los compuestos identificados se encuentran ésteres, compuestos aromáticos, alcoholes, acetales, lactonas y furfural. De esos 46 compuestos, nueve están presentes en todos los rones estudiados y algunos otros son característicos solo de la marca.

  19. A continuous hemofiltration system using sorbents for hemofiltrate regeneration.

    Science.gov (United States)

    Murisasco, A; Baz, M; Boobes, Y; Bertocchio, P; el Mehdi, M; Durand, C; Reynier, J P; Ragon, A

    1986-01-01

    Plasma ultrafiltrate obtained by glomerular filtration undergoes tubular modification which leads to the elimination of toxic substances, excess water and electrolytes, and consequently maintains homeostasis. Using normal urine and the substances it contains as a reference, we have developed a wearable device capable of replacing both the renal excretion function and maintaining fluid and electrolyte equilibrium in uremics within acceptable biological limits. Our device includes a hemofilter allowing continuous plasma ultrafiltration and sorbents obtained from a Redy sorbent cartridge to treat 85% of the ultrafiltrate, whereas 15% of this UF is rejected untreated. After calculating the quantity of ultrafiltrate (about 13 l) containing an amount of waste products of metabolism equivalent to 24-h urine elimination, we determined in vitro the amount of sorbent required to eliminate these waste products from the ultrafiltrate (e.g., 20 g of urea/day) and we have evaluated the quantities of other substances which must be replaced using a tailored diet. This extra-corporeal detoxification process was used in a uremic patient who had been on traditional hemodialysis for the past two years. The continuous treatment permitted maintenance of fluid and electrolyte equilibrium at the desired level and allowed rapid improvement of patient clinical status: elimination uf nausea, vomiting, diarrhea and edema, which had previously reappeared during the interdialytic periods, as well as a rapid decrease in heart size as ascites disappeared. In addition, the patient regained sexual drive and the ability to have an erection. In conclusion, traditional hemodialysis and hemofiltration techniques allow intermittent elimination of products retained by the body and reestablish nearly normal fluid and electrolyte balance.(ABSTRACT TRUNCATED AT 250 WORDS)

  20. Measurement of mercury species in human blood using triple spike isotope dilution with SPME-GC-ICP-DRC-MS.

    Science.gov (United States)

    Sommer, Yuliya L; Verdon, Carl P; Fresquez, Mark R; Ward, Cynthia D; Wood, Elliott B; Pan, Yi; Caldwell, Kathleen L; Jones, Robert L

    2014-08-01

    The measurement of different mercury compounds in human blood can provide valuable information about the type of mercury exposure. To this end, our laboratory developed a biomonitoring method for the quantification of inorganic (iHg), methyl (MeHg), and ethyl (EtHg) mercury in whole blood using a triple-spike isotope dilution (TSID) quantification method employing capillary gas chromatography (GC) and inductively coupled dynamic reaction cell mass spectrometry (ICP-DRC-MS). We used a robotic CombiPAL(®) sample handling station featuring twin fiber-based solid-phase microextraction (SPME) injector heads. The use of two SPME fibers significantly reduces sample analysis cycle times making this method very suitable for high sample throughput, which is a requirement for large public health biomonitoring studies. Our sample preparation procedure involved solubilization of blood samples with tetramethylammonium hydroxide (TMAH) followed by the derivatization with sodium tetra(n-propyl)borate (NaBPr(4)) to promote volatility of mercury species. We thoroughly investigated mercury species stability in the blood matrix during the course of sample treatment and analysis. The method accuracy for quantifying iHg, MeHg, and EtHg was validated using NIST standard reference materials (SRM 955c level 3) and the Centre de Toxicologie du Québec (CTQ) proficiency testing (PT) samples. The limit of detection (LOD) for iHg, MeHg, and EtHg in human blood was determined to be 0.27, 0.12, and 0.16 μg/L, respectively.

  1. An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

    Science.gov (United States)

    Du, Xin; Ren, YongLin; Beckett, Stephen J

    2016-01-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

  2. Durable zinc oxide-containing sorbents for coal gas desulfurization

    Science.gov (United States)

    Siriwardane, Ranjani V.

    1996-01-01

    Durable zinc-oxide containing sorbent pellets for removing hydrogen sulfide from a gas stream at an elevated temperature are made up to contain titania as a diluent, high-surface-area silica gel, and a binder. These materials are mixed, moistened, and formed into pellets, which are then dried and calcined. The resulting pellets undergo repeated cycles of sulfidation and regeneration without loss of reactivity and without mechanical degradation. Regeneration of the pellets is carried out by contacting the bed with an oxidizing gas mixture.

  3. The use of clays as sorbents and catalysts

    International Nuclear Information System (INIS)

    McCabe, R.W.

    1998-01-01

    The paper attempts to show the structural, physical and chemical properties of clay minerals relate to their laboratory, industrial and environmental uses as sorbents and catalysts. A brief review of the formulae and structures of clays and their relationship to their chemical and physical properties follows. Clay minerals are also useful in environmental protection as they can adsorb crude oils from spills and they are used, sometimes mixed into concrete, as containment barriers for radionuclides caesium 137 and strontium 90. Clay soils can also act as natural barriers to the migration of radionuclides in the environment

  4. Microwave synthesis of nanostructured oxide sorbents doped with lanthanides

    Energy Technology Data Exchange (ETDEWEB)

    Mitrofanov, Andrey A., E-mail: mitrofanov-a@icloud.com; Silyavka, Elena S.; Shilovskikh, Vladimir V.; Kolonitckii, Petr D.; Sukhodolov, Nikolai G.; Selyutin, Artem A., E-mail: selutin@inbox.ru [Saint Petersburg State University, 7/9, Universitetskaya nab., St. Petersburg, 199034 (Russian Federation)

    2016-06-17

    A number of nanostructured mesoporous oxide systems based on aluminum oxide, doped with lanthanide ions have been obtained in this study. Structure and morphology of oxides obtained have been examined by X-ray diffraction analysis, thermogravimetric analysis, scanning electron microscopy. The surface area of the samples was determined by the BET method. The dependence of the adsorption of insulin on synthesized oxides from the concentration was investigated. The containing of insulin in solutions after adsorption was determined by the Bradford method. The isotherms of adsorption of insulin on resulting oxide sorbents were plotted, the dependence capacity of the sorption of insulin from the lanthanide dopant was determined.

  5. Stability of Tritium and Iodine Sorbents in TPOG Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Jordan, Jacob A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jubin, Robert Thomas [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    US regulations could require the removal of both iodine and tritium from the off-gas stream of a used nuclear fuel (UNF) reprocessing facility. Advanced tritium pretreatment is a pretreatment step that uses high concentrations of NOR2R in a gas stream to volatilize tritium and iodine from UNF prior to traditional dissolution. The gaseous effluent from this process would then require abatement to remove tritium and iodine, but high levels of NOR2R could have a detrimental effect on the ability of various solid sorbents to remove the volatile radionuclides. For tritium and iodine, the sorbents of interest are 3Å molecular sieve (3AMS) for tritium and reduced silver mordenite (AgP0 PZ), silver-functionalized silica-aerogel (AgAerogel), and silver-nitrate-impregnated alumina (AgA) for iodine. Prior research has demonstrated that exposure to high concentrations of NOR2R can reduce the iodine loading capacity of AgP0 PZ by > 90% when exposed for 1 week. Research in Japan has demonstrated that AgA is more robust to NOR2R exposure than AgZ. The testing described here was intended to assess the effects of high concentrations of NOR2R on the iodine capture capacity of AgA and the water adsorption capacity of 3AMS. To determine the effect of extended exposure of the sorbents to NOR2R, both 3AMS and AgA were aged in a 75% NOR2R environment prior to loading. The 3AMS samples were aged for 1, 4, and 5.5 weeks at 40°C. They were then loaded with water in a 10°C dew point stream (corresponding to a water concentration of ~12,000 ppmv) at 40°C. There was no significant change in the water adsorption capacity of the 3AMS upon exposure to 75% NOR2R. The AgA samples were aged for 1, 2, and 4 weeks at 150°C and were loaded with 50 ppmv IR2R at 150°C. The results show that the iodine capture capacity of AgA is reduced by exposure to high concentrations of NOR2R. The iodine capacity reductions were 16%, 36%, and 76% for 1, 2, and 4 week exposures, respectively

  6. Spherical silica particles decorated with graphene oxide nanosheets as a new sorbent in inorganic trace analysis

    International Nuclear Information System (INIS)

    Sitko, Rafal; Zawisza, Beata; Talik, Ewa; Janik, Paulina; Osoba, Grzegorz; Feist, Barbara; Malicka, Ewa

    2014-01-01

    Highlights: • Graphene oxide (GO) covalently bonded to the spherical silica. • Very stable sorbent for SPE of metal ions. • Excellent contact with solution due to the softness and flexibility of GO nanosheets. • Several adsorption–elution cycles without any loss of adsorptive properties. • High adsorption capacity due to the wrinkled structure of GO nanosheets. - Abstract: Graphene oxide (GO) is a novel material with excellent adsorptive properties. However, the very small particles of GO can cause serious problems is solid-phase extraction (SPE) such as the high pressure in SPE system and the adsorbent loss through pores of frit. These problems can be overcome by covalently binding GO nanosheets to a support. In this paper, GO was covalently bonded to spherical silica by coupling the amino groups of spherical aminosilica and the carboxyl groups of GO (GO@SiO 2 ). The successful immobilization of GO nanosheets on the aminosilica was confirmed by scanning electron microscopy and X-ray photoelectron spectroscopy. The spherical particle covered by GO with crumpled silk wave-like carbon sheets are an ideal sorbent for SPE of metal ions. The wrinkled structure of the coating results in large surface area and a high extractive capacity. The adsorption bath experiment shows that Cu(II) and Pb(II) can be quantitatively adsorbed at pH 5.5 with maximum adsorption capacity of 6.0 and 13.6 mg g −1 , respectively. Such features of GO nanosheets as softness and flexibility allow achieving excellent contact with analyzed solution in flow-rate conditions. In consequence, the metal ions can be quantitatively preconcentrated from high volume of aqueous samples with excellent flow-rate. SPE column is very stable and several adsorption–elution cycles can be performed without any loss of adsorptive properties. The GO@SiO 2 was used for analysis of various water samples by flame atomic absorption spectrometry with excellent enrichment factors (200–250) and detection

  7. Spherical silica particles decorated with graphene oxide nanosheets as a new sorbent in inorganic trace analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sitko, Rafal, E-mail: rafal.sitko@us.edu.pl [University of Silesia, Institute of Chemistry, ul. Szkolna 9, 40-006 Katowice (Poland); Zawisza, Beata [University of Silesia, Institute of Chemistry, ul. Szkolna 9, 40-006 Katowice (Poland); Talik, Ewa [University of Silesia, Institute of Physics, ul. Uniwersytecka 4, 40-007 Katowice (Poland); Janik, Paulina; Osoba, Grzegorz; Feist, Barbara; Malicka, Ewa [University of Silesia, Institute of Chemistry, ul. Szkolna 9, 40-006 Katowice (Poland)

    2014-06-27

    Highlights: • Graphene oxide (GO) covalently bonded to the spherical silica. • Very stable sorbent for SPE of metal ions. • Excellent contact with solution due to the softness and flexibility of GO nanosheets. • Several adsorption–elution cycles without any loss of adsorptive properties. • High adsorption capacity due to the wrinkled structure of GO nanosheets. - Abstract: Graphene oxide (GO) is a novel material with excellent adsorptive properties. However, the very small particles of GO can cause serious problems is solid-phase extraction (SPE) such as the high pressure in SPE system and the adsorbent loss through pores of frit. These problems can be overcome by covalently binding GO nanosheets to a support. In this paper, GO was covalently bonded to spherical silica by coupling the amino groups of spherical aminosilica and the carboxyl groups of GO (GO@SiO{sub 2}). The successful immobilization of GO nanosheets on the aminosilica was confirmed by scanning electron microscopy and X-ray photoelectron spectroscopy. The spherical particle covered by GO with crumpled silk wave-like carbon sheets are an ideal sorbent for SPE of metal ions. The wrinkled structure of the coating results in large surface area and a high extractive capacity. The adsorption bath experiment shows that Cu(II) and Pb(II) can be quantitatively adsorbed at pH 5.5 with maximum adsorption capacity of 6.0 and 13.6 mg g{sup −1}, respectively. Such features of GO nanosheets as softness and flexibility allow achieving excellent contact with analyzed solution in flow-rate conditions. In consequence, the metal ions can be quantitatively preconcentrated from high volume of aqueous samples with excellent flow-rate. SPE column is very stable and several adsorption–elution cycles can be performed without any loss of adsorptive properties. The GO@SiO{sub 2} was used for analysis of various water samples by flame atomic absorption spectrometry with excellent enrichment factors (200–250) and

  8. New ZnO-based regenerable sulfur sorbents for fluid-bed/transport reactor applications

    Energy Technology Data Exchange (ETDEWEB)

    Slimane, R.B.; Williams, B.E. [Inst. of Gas Technology, Des Plaines, IL (United States)

    2002-11-13

    A new sorbent synthesis technique has been developed at GTI, based on sol-gel processing of inorganic and organic precursors, for the preparation of ZnO-based regenerable sulfur sorbents with unique properties that could not be attained with 'conventional' sorbent preparation methods such as coprecipitation or solid-oxide mixing followed by extrusion, granulation, or spray drying. Unlike these techniques, which require very high calcination temperatures to impart physical strength to sorbents, sol-gel processing offers the unique capability of producing sintering at exceptionally low temperatures. As a result, materials with high surface areas, small pore sizes, and very high resistance to attrition can be synthesized. Sorbents prepared with this new technique demonstrated attrition indices that are well below the stringent requirement of the transport reactor of about 4% and effective capacity for sulfur absorption exceeding 8 g of S 1100 g of sorbent. In addition, these sorbents demonstrated regenerability at temperatures that are lower than those required by typical zinc titanates. On the basis of chemical analysis, physical characterization, attrition resistance determination, and evaluation of chemical reactivity and regenerability, the exceptional characteristics of this new class of zinc-based sorbents are demonstrated in this paper.

  9. Application of inorganic sorbents for waste waters purification in paper production

    International Nuclear Information System (INIS)

    Present work is devoted to application of inorganic sorbents for waste waters purification in paper production. Therefore as sorbents for waste waters purification of paper production inorganic materials (hydroxides of different elements, bentonite, chalk) are tested. The optimal conditions of sorption are defined.

  10. Adsorption of H2O and CO2 on supported amine sorbents

    NARCIS (Netherlands)

    Veneman, Rens; Frigka, Natalia; Zhao, Wenying; Li, Zhenshan; Kersten, Sascha R.A.; Brilman, Derk Willem Frederik

    2015-01-01

    In this work the adsorption of H2O and CO2 on Lewatit VP OC 1065 was studied in view of the potential application of this sorbent in post combustion CO2 capture. Both CO2 and H2O were found to adsorb on the amine active sites present on the pore surface of the sorbent material. However, where the

  11. Development of miniaturized sorbent membrane funnel-based spray platform for biological analysis.

    Science.gov (United States)

    Yeung, Hoi Sze; Chen, Xiangfeng; Li, Wan; Wang, Ze; Wong, Y L Elaine; Chan, T-W Dominic

    2015-03-17

    In this work, a miniaturized solid-phase extraction (SPE) platform, called sorbent membrane funnel, which permits in situ cleanup prior to membrane funnel-based spray analysis was developed. The fabrication of funnel and the mounting of SPE sorbent were simple and straightforward by a homemade punching system. Using different sorbents, the SPE sorbent funnel has been successfully applied in spray analysis of drug molecules spiked in human plasma, trypsin digested solution of bovine serum albumin in the presence of high concentration of chaotropic reagents, and phosphopeptides in the tryptic digested solution of casein. The results demonstrated that SPE sorbent attached membrane funnels can be a useful tool in common metabolomic and proteomic applications.

  12. Cobalt oxide nanoparticles as a novel high-efficiency fiber coating for solid phase microextraction of benzene, toluene, ethylbenzene and xylene from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Gholivand, Mohammad Bagher, E-mail: MB.Gholivand@yahoo.com [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Shamsipur, Mojtaba; Shamizadeh, Mohammad [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Moradian, Rostam; Astinchap, Bandar [Physics Department, Faculty of Science, Razi University, Kermanshah (Iran, Islamic Republic of); Nano Technology Research Laboratory, Razi University, Kermanshah (Iran, Islamic Republic of)

    2014-04-01

    Highlights: • Co{sub 3}O{sub 4} nanoparticles were introduced as a novel SPME fiber coating. • The fiber was evaluated for the extraction of BTEX in combination with GC–MS. • The fiber showed extraction efficiencies better than a PDMS fiber toward BTEX. • The fiber was successfully applied to the determination of BTEX in real samples. - Abstract: In this work cobalt oxide nanoparticles were introduced for preparation of a novel solid phase microextraction (SPME) fiber coating. Chemical bath deposition (CBD) technique was used in order for synthesis and immobilization of the Co{sub 3}O{sub 4} nanomaterials on a Pt wire for fabrication of SPME fiber. The prepared cobalt oxide coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The fiber was evaluated for the extraction of benzene, toluene, ethylbenzene and xylene (BTEX) in combination with GC–MS. A simplex optimization method was used to optimize the factors affecting the extraction efficiency. Under optimized conditions, the proposed fiber showed extraction efficiencies comparable to those of a commercial polydimethylsiloxane (PDMS) fiber toward the BTEX compounds. The repeatability of the fiber and its reproducibility, expressed as relative standard deviation (RSD), were lower than about 11%. No significant change was observed in the extraction efficiency of the new SPME fiber after over 50 extractions. The fiber was successfully applied to the determination of BTEX compounds in real samples. The proposed nanostructure cobalt oxide fiber is a promising alternative to the commercial fibers as it is robust, inexpensive and easily prepared.

  13. Facile synthesis of new nano sorbent for magnetic solid-phase extraction by self assembling of bis-(2,4,4-trimethyl pentyl)-dithiophosphinic acid on Fe3O4-Ag core-shell nanoparticles: Characterization and application

    International Nuclear Information System (INIS)

    Tahmasebi, Elham; Yamini, Yadollah

    2012-01-01

    Graphical abstract: Self assembling of bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid on Fe 3 O 4 -Ag core-shell nanoparticles and application of it for solid phase extraction of PAHs. Highlights: ► A novel sorbent for magnetic solid-phase extraction of PAHs was introduced. ► Silver was coated on Fe 3 O 4 nanoparticles (MNPs) by reduction of AgNO 3 with NaBH 4 . ► Bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid self-assembled on silver coated MNPs. ► Size, morphology, composition and properties of the nanoparticles were characterized. ► Extraction efficiency of the sorbent was investigated by extraction of five PAHs. - Abstract: A novel sorbent for magnetic solid-phase extraction by self-assembling of organosulfur compound, (bis-(2,4,4-trimethylpentyl)-dithiophosphinic acid), onto the silver-coated Fe 3 O 4 nanoparticles was introduced. Due to the formation of covalent bond of S-Ag, the new coating on the silver surface was very stable and showed high thermal stability (up to 320 °C). The size, morphology, composition, and properties of the prepared nanoparticles have also been characterized and determined using scanning electron microscopy (SEM), energy-dispersive X-ray analyzer (EDX), dynamic light scattering (DLS), Fourier transform-infrared (FT-IR) spectroscopy, and thermal gravimetric analysis (TGA). Extraction efficiency of the new sorbent was investigated by extraction of five polycyclic aromatic hydrocarbons (PAHs) as model compounds. The optimum extraction conditions for PAHs were obtained as of extraction time, 20 min; 50 mg sorbent from 100 mL of the sample solution, and elution with 100 μL of 1-propanol under fierce vortex for 2 min. Under the optimal conditions, the calibration curves were obtained in the range of 0.05–100 μg L −1 (R 2 > 0.9980) and the LODs (S/N = 3) were obtained in the range of 0.02–0.10 μg L −1 . Relative standard deviations (RSDs) for intra- and inter-day precision were 2.6–4.2% and 3.6–8

  14. Zinc oxide/polypyrrole nanocomposite as a novel solid phase microextraction coating for extraction of aliphatic hydrocarbons from water and soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Amanzadeh, Hatam; Yamini, Yadollah [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175 Tehran (Iran, Islamic Republic of); Moradi, Morteza [Department of Semiconductors, Materials and Energy Research Center, Karaj (Iran, Islamic Republic of)

    2015-07-16

    Highlights: • ZnO/polypyrrole (ZNO/PPY) nanocomposite coating was fabricated on stainless steel. • Nanocomposite coating morphology was evaluated using scanning electron microscopy. • It was applied for HS-SPME of aliphatic hydrocarbons in water and soil samples. • Separation and determination of the hydrocarbons were performed by GC-FID. • The method is suitable for routine analysis of n-alkanes in various environmental samples. - Abstract: In this work, ZnO/PPy nanocomposite coating was fabricated on stainless steel and evaluated as a novel headspace solid phase microextraction (HS-SPME) fiber coating for extraction of ultra-trace amounts of environmental pollutants; namely, aliphatic hydrocarbons in water and soil samples. The ZnO/PPy nanocomposite were prepared by a two-step process including the electrochemical deposition of PPy on the surface of stainless steel in the first step, and the synthesis of ZnO nanorods by hydrothermal process in the pores of PPy matrix in the second step. Porous structure together with ZnO nanorods with the average diameter of 70 nm were observed on the surface by using scanning electron microscopy (SEM). The effective parameters on HS-SPME of hydrocarbons (i.e., extraction temperature, extraction time, desorption temperature, desorption time, salt concentration, and stirring rate) were investigated and optimized by one-variable-at-a-time method. Under optimized conditions (extraction temperature, 65 ± 1 °C; extraction time, 15 min; desorption temperature, 250 °C; desorption time, 3 min; salt concentration, 10% w/v; and stirring rate, 1200 rpm), the limits of detection (LODs) were found in the range of 0.08–0.5 μg L{sup −1}, whereas the repeatability and fiber-to-fiber reproducibility were in the range 5.4–7.6% and 8.6–10.4%, respectively. Also, the accuracies obtained for the spiked n-alkanes were in the range of 85–108%; indicating the absence of matrix effects in the proposed HS-SPME method. The results

  15. Hard coatings

    International Nuclear Information System (INIS)

    Dan, J.P.; Boving, H.J.; Hintermann, H.E.

    1993-01-01

    Hard, wear resistant and low friction coatings are presently produced on a world-wide basis, by different processes such as electrochemical or electroless methods, spray technologies, thermochemical, CVD and PVD. Some of the most advanced processes, especially those dedicated to thin film depositions, basically belong to CVD or PVD technologies, and will be looked at in more detail. The hard coatings mainly consist of oxides, nitrides, carbides, borides or carbon. Over the years, many processes have been developed which are variations and/or combinations of the basic CVD and PVD methods. The main difference between these two families of deposition techniques is that the CVD is an elevated temperature process (≥ 700 C), while the PVD on the contrary, is rather a low temperature process (≤ 500 C); this of course influences the choice of substrates and properties of the coating/substrate systems. Fundamental aspects of the vapor phase deposition techniques and some of their influences on coating properties will be discussed, as well as the very important interactions between deposit and substrate: diffusions, internal stress, etc. Advantages and limitations of CVD and PVD respectively will briefly be reviewed and examples of applications of the layers will be given. Parallel to the development and permanent updating of surface modification technologies, an effort was made to create novel characterisation methods. A close look will be given to the coating adherence control by means of the scratch test, at the coating hardness measurement by means of nanoindentation, at the coating wear resistance by means of a pin-on-disc tribometer, and at the surface quality evaluation by Atomic Force Microscopy (AFM). Finally, main important trends will be highlighted. (orig.)

  16. Methods and sorbents for utilizing a hot-side electrostatic precipitator for removal of mercury from combustion gases

    Science.gov (United States)

    Nelson, Sidney [Hudson, OH

    2011-02-15

    Methods are provided for reducing emission of mercury from a gas stream by treating the gas with carbonaceous mercury sorbent particles to reduce the mercury content of the gas; collecting the carbonaceous mercury sorbent particles on collection plates of a hot-side ESP; periodically rapping the collection plates to release a substantial portion of the collected carbonaceous mercury sorbent particles into hoppers; and periodically emptying the hoppers, wherein such rapping and emptying are done at rates such that less than 70% of mercury adsorbed onto the mercury sorbent desorbs from the collected mercury sorbent into the gas stream.

  17. Protective Coatings

    Science.gov (United States)

    1980-01-01

    General Magnaplate Corporation's pharmaceutical machine is used in the industry for high speed pressing of pills and capsules. Machine is automatic system for molding glycerine suppositories. These machines are typical of many types of drug production and packaging equipment whose metal parts are treated with space spinoff coatings that promote general machine efficiency and contribute to compliance with stringent federal sanitation codes for pharmaceutical manufacture. Collectively known as "synergistic" coatings, these dry lubricants are bonded to a variety of metals to form an extremely hard slippery surface with long lasting self lubrication. The coatings offer multiple advantages; they cannot chip, peel or be rubbed off. They protect machine parts from corrosion and wear longer, lowering maintenance cost and reduce undesired heat caused by power-robbing friction.

  18. Sorption of Aromatic Compounds with Copolymer Sorbent Materials Containing β-Cyclodextrin

    Directory of Open Access Journals (Sweden)

    Lee D. Wilson

    2011-08-01

    Full Text Available Urethane copolymer sorbent materials that incorporate β-cyclodextrin (CD have been prepared and their sorption properties with chlorinated aromatic compounds (i.e., pentachlorophenol, 2,4-dichlorophenol and 2,4-dichlorophenoxy acetic acid have been evaluated. The sorption properties of granular activated carbon (GAC were similarly compared in aqueous solution at variable pH conditions. The sorbents displayed variable BET surface areas as follows: MDI-X copolymers (< 101 m2/g, CDI-X copolymers (< 101 m2/g, and granular activated carbon (GAC ~103 m2/g. The sorption capacities for the copolymers sorbents are listed in descending order, as follows: GAC > CDI-3 copolymer ≈ MDI-3 copolymer. The sorption capacity for the aromatic adsorbates with each sorbent are listed in descending order, as follows: 2,4-dichlorophenol > 2,4-dichlorophenoxy acetic acid > pentachlorophenol. In general, the differences in the sorption properties of the copolymer sorbents with the chlorinated organics were related to the following factors: (i surface area of the sorbent; (ii CD content and accessibility; and (iii and the chemical nature of the sorbent material.

  19. Evaluation of silk-floss fiber and dog fur as sorbent materials for the petroleum sector

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Lucas P. dos [Universidade Federal do Parana (PGMec/UFPR), Curitiba, PR (Brazil). Programa de Pos-Graduacao em Engenharia Mecanica; Dubiella, Juliana [Universidade Federal do Parana (DEMEC/UFPR), Curitiba, PR (Brazil). Dept. de Engenharia Mecanica. Programa Institucional de Bolsas de Iniciacao Cientifica; Perotta, Larissa [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Programa Interdisciplinar em Engenharia de Petroleo e Gas Natural; Satyanarayana, Kestur G. [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica; Flores-Sahagun, Thais Sydenstricker [Universidade Federal do Parana (DEMEC/UFPR), Curitiba, PR (Brazil). Dept. de Engenharia Mecanica

    2009-07-01

    In this study silk-floss and dog fur were tested as sorbent materials for oils and the results were compared with peat, a commercial sorbent. Sorption tests were carried out in dry and aqueous systems, with and without stirring for different periods of time (5-1440 min). Density, hydrophobicity, buoyancy and water uptake by the fibers of the impregnated sorbents have been determined. The use of silk-floss and dog fur was also tested in columns to purify water containing toluene, benzene, motor oil or sunflower oil. Breakthrough curves during 120 min were drawn for each material with the samples (oily water or water containing benzene or toluene) and were analyzed by ultraviolet spectroscopy. It was concluded that the silk-floss is the best sorbent material (65.3 g oil/g sorbent) followed by the dog fur (34.6 g oil/g sorbent) and peat (19.5 g oil/g sorbent), for sorption time of 1 h in dynamic condition. The efficiency of the pollutant removal from water with the use of adsorption columns was high for both materials although the use of dog fur was preferable because of the slight superiority in efficiency compared to silk-floss and also, due to the easier packing of the dog fur in the column. (author)

  20. Thermochemical Characterizations of Novel Vermiculite-LiCl Composite Sorbents for Low-Temperature Heat Storage

    Directory of Open Access Journals (Sweden)

    Yannan Zhang

    2016-10-01

    Full Text Available To store low-temperature heat below 100 °C, novel composite sorbents were developed by impregnating LiCl into expanded vermiculite (EVM in this study. Five kinds of composite sorbents were prepared using different salt concentrations, and the optimal sorbent for application was selected by comparing both the sorption characteristics and energy storage density. Textural properties of composite sorbents were obtained by extreme-resolution field emission scanning electron microscopy (ER-SEM and an automatic mercury porosimeter. After excluding two composite sorbents which would possibly exhibit solution leakage in practical thermal energy storage (TES system, thermochemical characterizations were implemented through simulative sorption experiments at 30 °C and 60% RH. Analyses of thermogravimetric analysis/differential scanning calorimetry (TGA/DSC curves indicate that water uptake of EVM/LiCl composite sorbents is divided into three parts: physical adsorption of EVM, chemical adsorption of LiCl crystal, and liquid–gas absorption of LiCl solution. Energy storage potential was evaluated by theoretical calculation based on TGA/DSC curves. Overall, EVMLiCl20 was selected as the optimal composite sorbent with water uptake of 1.41 g/g, mass energy storage density of 1.21 kWh/kg, and volume energy storage density of 171.61 kWh/m3.

  1. Development of the advanced coolside sorbent injection process for SO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Withum, J.A.; Maskew, J.T.; Rosenhoover, W.A. [Consol, Inc., Library, PA (United States)] [and others

    1995-11-01

    The goal of this work was to develop a low-capital-cost process capable of over 90% SO{sub 2} removal as an economically attractive option for compliance with the Clean Air Act. The Advanced Coolside Process uses a contactor to simultaneously remove fly ash and saturate the flue gas with water, followed by sorbent injection into the highly humid flue gas and collection of the sorbent by the existing particulate collector High sorbent utilization is achieved by sorbent recycle. The original performance targets of 90% SO{sub 2} removal and 60% sorbent utilization were exceeded in 1000 acfm pilot plant operations using commercial hydrated lime as the only sorbent. Process optimization simplified the process equipment, resulting in significant cost reduction. Recent accomplishments include completion of equipment testing and sorbent optimization, a waste management study, and a long-term performance test. An economic evaluation for the optimized process projects capital costs 55% to 60 % less than those of limestone forced oxidation wet FGD. The projected levelized control cost is 15% to 35% lower than wet FGD (25% lower for a 260 MWe plant burning a 2.5% sulfur coal), depending on plant size and coal sulfur content.

  2. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    Energy Technology Data Exchange (ETDEWEB)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; Douglas P. Harrison; Ya Liang

    2001-10-01

    The objective of this project is to develop a simple, inexpensive process to separate CO{sub 2} as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO{sub 2} stream after condensation of water vapor. Testing conducted previously confirmed that the reaction rate and achievable CO{sub 2} capacity of sodium carbonate decreased with increasing temperature, and that the global rate of reaction of sodium carbonate to sodium bicarbonate increased with an increase in both CO{sub 2} and H{sub 2}O concentrations. Energy balance calculations indicated that the rate of heat removal from the particle surface may determine the reaction rate for a particular particle system. This quarter, thermogravimetric analyses (TGA) were conducted which indicated that calcination of sodium bicarbonate at temperatures as high as 200 C did not cause a significant decrease in activity in subsequent carbonation testing. When sodium bicarbonate was subjected to a five cycle calcination/carbonation test, activity declined slightly over the first two cycles but was constant thereafter. TGA tests were also conducted with two other potential sorbents. Potassium carbonate was found to be less active than sodium carbonate, at conditions of interest in preliminary TGA tests. Sodium carbonate monohydrate showed negligible activity. Testing was also conducted in a 2-inch internal diameter quartz fluidized-bed reactor system. A five cycle test demonstrated that initial removals of 10 to 15 percent of the carbon dioxide in a simulated flue gas could be achieved. The carbonation reaction proceeded at temperatures as low as 41 C. Future work by TGA and in fixed

  3. CARBON DIOXIDE CAPTURE FROM FLUE GAS USING DRY REGENERABLE SORBENTS

    International Nuclear Information System (INIS)

    David A. Green; Brian S. Turk; Raghubir P. Gupta; Douglas P. Harrison; Ya Liang

    2001-01-01

    The objective of this project is to develop a simple, inexpensive process to separate CO(sub 2) as an essentially pure stream from a fossil fuel combustion system using a regenerable, sodium-based sorbent. The sorbent being used in this project is sodium carbonate which is converted to sodium bicarbonate, ''baking soda,'' through reaction with carbon dioxide and water vapor. Sodium bicarbonate is regenerated to sodium carbonate when heated, producing a nearly pure CO(sub 2) stream after condensation of water vapor. Testing conducted previously confirmed that the reaction rate and achievable CO(sub 2) capacity of sodium carbonate decreased with increasing temperature, and that the global rate of reaction of sodium carbonate to sodium bicarbonate increased with an increase in both CO(sub 2) and H(sub 2)O concentrations. Energy balance calculations indicated that the rate of heat removal from the particle surface may determine the reaction rate for a particular particle system. This quarter, thermogravimetric analyses (TGA) were conducted which indicated that calcination of sodium bicarbonate at temperatures as high as 200 C did not cause a significant decrease in activity in subsequent carbonation testing. When sodium bicarbonate was subjected to a five cycle calcination/carbonation test, activity declined slightly over the first two cycles but was constant thereafter. TGA tests were also conducted with two other potential sorbents. Potassium carbonate was found to be less active than sodium carbonate, at conditions of interest in preliminary TGA tests. Sodium carbonate monohydrate showed negligible activity. Testing was also conducted in a 2-inch internal diameter quartz fluidized-bed reactor system. A five cycle test demonstrated that initial removals of 10 to 15 percent of the carbon dioxide in a simulated flue gas could be achieved. The carbonation reaction proceeded at temperatures as low as 41 C. Future work by TGA and in fixed-bed, fluidized-bed, and transport

  4. Establishment of Exposure to Organophosphorus Warfare Agents by Means of SPME-GSMS Analysis of Bodily Fluids

    International Nuclear Information System (INIS)

    Saveleva, E. I.; Koryagina, N. L.; Radilov, A. S.; Khlebnikova, N. S.; Khrustaleva, V. S.; Feld, V. E.

    2007-01-01

    Reliable chemical analytical procedures for revealing an exposure to toxic chemicals, identifying the active substance, and assessing the degree of exposure are necessary as a component of medical and forensic activities in cases of the possible use of highly toxic chemicals in war conflicts and terrorism acts, as well as emergency situations in chemical industry, specifically at chemical weapons storage and destruction facilities. According to Chemical Weapons Convention, Part XI, Appendix 4, e-17, 'samples of importance in the investigation of alleged use include biomedical samples from human or animal sources (blood, urine, excreta, tissue etc.)'. Urinary metabolites, O-alkyl esters of methylphosphic acid, offer one of the simplest means of confirming an exposure to organophosphorus warfare agents (OPWA). Urine, unlike blood or tissues, does not require invasive collection demanding in terms of sterility. Excretion with urine is the major route of elimination of OPWA from an organism. According to published data, 90% of OPWA metabolites are excreted within 48-72 h after intoxication. We developed an SPME-GCMS procedure for the determination of O-alkyl esters methylphosphonic acid in urine, with the following detection limits,: isopropyl and isobutyl esters 5 ng/ml and pinacolyl ester 1 ng/ml. The procedure involves derivatization of the target compounds directly on the microfiber. The total analysis time is 1-1.5 h. In animal experiments in vivo we could establish the exposure to OPWA at a half-LD50 level within no less than 48 h after intoxication. In principle, OPWA metabolites could be detected in urine within two weeks after intoxication but at higher doses. Retrospective analysis of urinary metabolites in cases of the exposure to low doses of OPWA requires lower detection limits (0.1-1 ng/ml). Optimal objects for the retrospective analysis of OPWA in an organism are long-lived blood protein adducts. We developed a procedure for revealing an exposure to

  5. Inorganic sorbents for radiostrontium removal from waste solutions: selectivity and role of calixarenes

    International Nuclear Information System (INIS)

    Vijayan, S.; Belikov, K.; Drapailo, A.

    2011-01-01

    The challenge in the remediation of 90 Sr-contaminated waters arises from the need to achieve very high removal efficiencies to meet discharge targets from waste effluents containing relatively high concentrations of non-radioactive cations. Low-cost natural zeolites are not selective for strontium over other divalent cations, notably such ions as calcium; and produce low 90 Sr removal performance, and large volumes of spent sorbent waste. The synthesis and use of selective, synthetic inorganic sorbents could prove to be a feasible approach for high 90 Sr removal efficiencies, and much smaller volumes of secondary solid waste generation. The essential advantages of inorganic sorbents include their stability and resistance to radiation, and the potential for producing stable waste forms such as vitrified glass or ceramics for disposal. However, the cost of strontium-specific sorbents is prohibitive for large-scale applications at present. This paper is a review of the reported information on removal mechanisms and performance of Sr-specific inorganic sorbents. The analysis has revealed promising performance, efficiency and selectivity for strontium removal from solutions containing low and high concentrations of salts. The leading sorbents are crystalline silicotitanate and oxides of metals such as titanium. An initial assessment has also been made of the performance of calixarene-based macrocyclic compounds. These are known for their selectivity for strontium in solvent extraction processes. From the initial strontium removal results in bench-scale tests using different solid substrates, impregnated with calixarene derivatives, only sodium-mordenite impregnated with calyx[8]arene octamide gave an overall strontium removal efficiency in the range of 90 to 95% in the presence of 3.5 ppm calcium. There was no improvement observed for strontium-removal efficiency or selectivity over calcium in the calixarene-impregnated inorganic sorbent matrix. In several tests, the

  6. Metal-organic framework templated synthesis of porous inorganic materials as novel sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, Kathryn M. L.; Lin, Wenbin; Abney, Carter W.

    2017-03-21

    A novel metal-organic framework (MOF) templated process for the synthesis of highly porous inorganic sorbents for removing radionuclides, actinides, and heavy metals is disclosed. The highly porous nature of the MOFs leads to highly porous inorganic sorbents (such as oxides, phosphates, sulfides, etc) with accessible surface binding sites that are suitable for removing radionuclides from high level nuclear wastes, extracting uranium from acid mine drainage and seawater, and sequestering heavy metals from waste streams. In some cases, MOFs can be directly used for removing these metal ions as MOFs are converted to highly porous inorganic sorbents in situ.

  7. Aerosol Formation during the Combustion of Straw with Addition of Sorbents

    DEFF Research Database (Denmark)

    Zeuthen, Frederik Jacob; Jensen, Peter Arendt; Jensen, Jørgen P.

    2007-01-01

    The influence of six sorbents on aerosol formation during the combustion of straw in a 100 MW boiler on a Danish power plant has been studied in full-scale. The following sorbents were studied: ammonium sulfate, monocalcium phosphate, Bentonite, ICA5000, clay, and chalk. Bentonite and ICA5000......, calcium phosphate, Bentonite, ICA5000, and clay. The addition of chalk increased the aerosol mass concentration by 24%. Experiments in a laminar flow aerosol condenser with the six sorbents were carried out in the laboratory using a synthetic flue gas to avoid fluctuations in the alkali feeding...

  8. Efficient CO2 sorbents based on silica foam with ultra-large mesopores

    KAUST Repository

    Qi, Genggeng

    2012-01-01

    A series of high-capacity, amine impregnated sorbents based on a cost-effective silica foam with ultra-large mesopores is reported. The sorbents exhibit fast CO2 capture kinetics, high adsorption capacity (of up to 5.8 mmol g-1 under 1 atm of dry CO2), as well as good stability over multiple adsorption-desorption cycles. A simple theoretical analysis is provided relating the support structure to sorbent performance. © 2012 The Royal Society of Chemistry.

  9. Optimization of the coating procedure for a high-throughput 96-blade solid phase microextraction system coupled with LC-MS/MS for analysis of complex samples.

    Science.gov (United States)

    Mirnaghi, Fatemeh S; Chen, Yong; Sidisky, Leonard M; Pawliszyn, Janusz

    2011-08-01

    Biocompatible C18-polyacrylonitrile (PAN) coating was used as the extraction phase for an automated 96-blade solid phase microextraction (SPME) system with thin-film geometry. Three different methods of coating preparation (dipping, brush painting, and spraying) were evaluated; the spraying method was optimum in terms of its stability and reusability. The high-throughput sample preparation was achieved by using a robotic autosampler that enabled simultaneous preparation of 96 samples in 96-well-plate format. The increased volume of the extraction phase of the C18-PAN thin film coating resulted in significant enhancement in the extraction recovery when compared with that of the C18-PAN rod fibers. Various factors, such as reusability, reproducibility, pH stability, and reliability of the coating were evaluated. The results showed that the C18-PAN 96-blade SPME coating presented good extraction recovery, long-term reusability, good reproducibility, and biocompatibility. The limits of detection and quantitation were in the ranges of 0.1-0.3 and 0.5-1 ng/mL for all four analytes.

  10. Regenerable immobilized aminosilane sorbents for carbon dioxide capture applications

    Science.gov (United States)

    Gay, McMahan; Choi, Sunho; Jones, Christopher W

    2014-09-16

    A method for the separation of carbon dioxide from ambient air and flue gases is provided wherein a phase separating moiety with a second moiety are simultaneously coupled and bonded onto an inert substrate to create a mixture which is subsequently contacted with flue gases or ambient air. The phase-separating moiety is an amine whereas the second moiety is an aminosilane, or a Group 4 propoxide such as titanium (IV) propoxide (tetrapropyl orthotitanate, C.sub.12H.sub.28O.sub.4Ti). The second moiety makes the phase-separating moiety insoluble in the pores of the inert substrate. The new sorbents have a high carbon dioxide loading capacity and considerable stability over hundreds of cycles. The synthesis method is readily scalable for commercial and industrial production.

  11. Application of TIO2 as A sorbent for radioactive waste

    International Nuclear Information System (INIS)

    Zamroni, H.; Las, T.; Kamarz, H.

    1997-01-01

    The sorption properties of the neodymium has been studied by using TiO 2 sorbent. The experiment was carried out by batch methods to investigate the kinetic sorption, effect of pH and effect of NaNO 3 concentration in the solution. Neodymium uses for a model of trivalent actinide treated by TiO 2 which was known as materials having high thermal and radiation stabilities as well as potentially used for immobilization of waste with cement or vitrification. the results show that the optimum of kinetic sorption was obtained after one day experiment to reach the equilibrium in sorption on pH 4, and the increasing of NaNO 3 concentrations will increase the sorption of neodymium in solution (author)

  12. Modeling of IR spectra for nerve agent-sorbent binding

    Science.gov (United States)

    Papantonakis, M. R.; Roberts, C. A.; Shabaev, A.; Kim, Y.; McGill, R. A.; Kendziora, C. A.; Furstenberg, R.; Lambrakos, S. G.

    2017-08-01

    An inverse analysis of experimentally measured infrared absorption spectra for the custom sorbent SiFA4H, nerve agent precursor and simulant DMMP, and intermolecularly bonded structure SiFA4H+DMMP is presented. These structures and their associated infrared spectra provide general understanding of the process whereby an analyte chemical may be detected using infrared spectral analysis. The inverse analysis presented provides estimates of permittivity functions, which when combined with the Clausius-Mossotti relation, can predict molecular polarizabilities associated with SiFA4H-SiFA4H and SiFA4H-DMMP interactions. Molecular polarizabilities deduced from measured absorption coefficients are modeled using molecular dynamics simulations.

  13. Rapid sampling of BTEX in air by SPME in the city of Nice and at the Nice-Cote d'Azur airport; Echantillonnage rapide des BTEX dans l'air par SPME dans la ville de Nice et a l'aeroport Nice-Cote d'Azur

    Energy Technology Data Exchange (ETDEWEB)

    Tumbiolo, S.; Gal, J.F.; Maria, P.Ch. [Nice Univ. Sophia Antipolis, Lab. de Radiochimie, Sciences Analytique et Environnement, Faculte des Sciences, 06 (France); Laborde, P.; Teton, S. [Qualitair, Nice Leader, 06 - Nice (France)

    2006-04-15

    This article presents the results of a tentative application of Solid Phase Micro Extraction (SPME) to the analysis of BTEX (benzene, toluene, ethyl-benzene and xylenes) at the {mu}g/m{sup 3} level in indoor and outdoor air. The salient features of the method validation are reported. Sampling by QUALITAIR using Radiello passive samplers, was carried out from 2001 to 2004 in the city of Nice and its airport. Urban traffic impact was proved, but a link between BTX concentrations and the variations of airport activities was not clearly established. During the same period, several samplings were performed using SPME. Taking into account the short (30 minutes) sampling time, rapid changes of BTEX concentrations were evidenced, as for example the start of airplane engines. As field studies have shown, SPME technique appears as a method of choice for fast qualitative analysis and quantitative determination of Volatile Organic Compounds (VOC). The small dimensions of the SPME sampling system and the short sampling time let envisage its utilisation for the rapid diagnostic and the monitoring of indoor air quality. (author)

  14. Spherical silica particles decorated with graphene oxide nanosheets as a new sorbent in inorganic trace analysis.

    Science.gov (United States)

    Sitko, Rafal; Zawisza, Beata; Talik, Ewa; Janik, Paulina; Osoba, Grzegorz; Feist, Barbara; Malicka, Ewa

    2014-06-27

    Graphene oxide (GO) is a novel material with excellent adsorptive properties. However, the very small particles of GO can cause serious problems is solid-phase extraction (SPE) such as the high pressure in SPE system and the adsorbent loss through pores of frit. These problems can be overcome by covalently binding GO nanosheets to a support. In this paper, GO was covalently bonded to spherical silica by coupling the amino groups of spherical aminosilica and the carboxyl groups of GO (GO@SiO2). The successful immobilization of GO nanosheets on the aminosilica was confirmed by scanning electron microscopy and X-ray photoelectron spectroscopy. The spherical particle covered by GO with crumpled silk wave-like carbon sheets are an ideal sorbent for SPE of metal ions. The wrinkled structure of the coating results in large surface area and a high extractive capacity. The adsorption bath experiment shows that Cu(II) and Pb(II) can be quantitatively adsorbed at pH 5.5 with maximum adsorption capacity of 6.0 and 13.6 mg g(-1), respectively. Such features of GO nanosheets as softness and flexibility allow achieving excellent contact with analyzed solution in flow-rate conditions. In consequence, the metal ions can be quantitatively preconcentrated from high volume of aqueous samples with excellent flow-rate. SPE column is very stable and several adsorption-elution cycles can be performed without any loss of adsorptive properties. The GO@SiO2 was used for analysis of various water samples by flame atomic absorption spectrometry with excellent enrichment factors (200-250) and detection limits (0.084 and 0.27 ng mL(-1) for Cu(II) and Pb(II), respectively). Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Diagnostic value of enzyme linked immuno-sorbent assay for cytomegalovirus disease.

    Directory of Open Access Journals (Sweden)

    Priya K

    2002-07-01

    Full Text Available BACKGROUND: Since interpretation of results of enzyme linked immuno-sorbent assay (ELISA for diagnosis of Cytomegalovirus (CMV infection in India is difficult, its diagnostic value required evaluation. AIMS: To evaluate the diagnostic value of ELISA against polymerase chain reaction (PCR in CMV disease. SETTINGS AND DESIGN: Results of ELISA test for CMV antibodies in CMV-DNA PCR positive and negative patients and normal healthy blood donors were analysed. METHODS AND MATERIAL: Anti-CMV antibodies were assayed by ELISA on the sera of 26 CMV PCR positive and 21 PCR negative patients and 35 normal healthy blood donors. STATISTICAL ANALYSIS: Chi square and Fischer exact test were used for statistical analysis. RESULTS: Anti-CMV antibodies (IgG or IgG and IgM were present in 20 (76.9% of 26 PCR positive and 13 (61.9% of 21 PCR negative patients. ELISA was negative in six (23.1% of 26 PCR positive patients. Of the 28 paediatric patients, ELISA was positive in 14 (73.7% of 19 PCR positive and three (33.3% of nine PCR negative patients showing a statistically significant difference (Chi square test, P value 0.038. Among the 19 patients having complications after organ transplant, ELISA showed anti-CMV antibodies in six (85.7% of seven PCR positive and 11 (91.7% of 12 PCR negative patients showing no significant difference. CMV-DNA was not detected in the buffy coat of 35 sero-positive blood donors. CONCLUSION: ELISA has no diagnostic value in the detection of CMV activation although it may help in the differential diagnosis of CMV infection in the paediatric age group.

  16. Analysis of the volatiles in the headspace above the plasmodium and sporangia of the slime mould (Physarum polycephalum) by SPME-GCMS

    OpenAIRE

    Kateb, Huda al; Costello, Ben de Lacy

    2013-01-01

    Solid phase micro-extraction (SPME) coupled with Gas Chromatography Mass Spectrometry (GC-MS) was used to extract and analyse the volatiles in the headspace above the plasmodial and sporulating stages of the slime mould Physarum Polycephalum. In total 115 compounds were identified from across a broad range of chemical classes. Although more (87) volatile organic compounds (VOCs) were identified when using a higher incubation temperature of 75oC, a large number of compounds (79) were still ide...

  17. Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2018-02-06

    Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

  18. Hot coal gas desulfurization with manganese-based sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Hepworth, M.T.; Ben-Slimane, R.

    1994-10-01

    In this paper, the physical and chemical behavior of several sorbent formulations fabricated from a manganese-containing compound, alundum (Al{sub 2}O{sub 3}), and a binder are addressed. The thermodynamic feasibility of hydrogen sulfide (H{sub 2}S)-removal from hot-simulated coal-gases using these sorbents and their subsequent regeneration with air are established. A formulation, FORM4-A, which consists of MnCO{sub 3}, alundum, and bentonite exhibits the best combination of capacity and reactivity; whereas, FORM1-A, which consists of Mn-ore, alundum, and dextrin exhibits the best combination of strength and reactivity. One important finding is that the capacity of the pellets for sulfur pickup from a H{sub 2}/H{sub 2}S mixture (at 950{degrees}C) and the kinetics of reduction, sulfidation and regeneration (at 1000{degrees}C) improve with recycling without compromising the strength. The leading formulation, FORM4-A, was subjected to 20 consecutive cycles of sulfidation and regeneration at 900{degrees}C in a 2-inch fixed bed reactor. The sulfidation gas was a simulated Tampella U-gas with an increased hydrogen sulfide content of 3% by volume to accelerate the rate of breakthrough, arbitrarily taken as 500 ppmv. Consistent with thermo-gravimetric analysis (TGA) on individual pellets, the fixed bed tests show small improvement in capacity and kinetics with the sulfur-loading capacity being about 22% by weight of the original pellet, which corresponds to approximately 90% bed utilization.

  19. Development of a Microwave Regenerative Sorbent-Based Hydrogen Purifier

    Science.gov (United States)

    Wheeler, Richard R., Jr.; Dewberry, Ross H.; McCurry, Bryan D.; Abney, Morgan B.; Greenwood, Zachary W.

    2016-01-01

    This paper describes the design and fabrication of a Microwave Regenerative Sorbent-based Hydrogen Purifier (MRSHP). This unique microwave powered technology was developed for the purification of a hydrogen stream produced by the Plasma Pyrolysis Assembly (PPA). The PPA is a hydrogen recovery (from methane) post processor for NASA's Sabatier-based carbon dioxide reduction process. Embodied in the Carbon dioxide Reduction Assembly (CRA), currently aboard the International Space Station (ISS), the Sabatier reaction employs hydrogen to catalytically recover oxygen, in the form of water, from respiratory carbon dioxide produced by the crew. This same approach is base-lined for future service in the Air Revitalization system on extended missions into deep space where resupply is not practical. Accordingly, manned exploration to Mars may only become feasible with further closure of the air loop as afforded by the greater hydrogen recovery permitted by the PPA with subsequent hydrogen purification. By utilizing the well-known high sorbate loading capacity of molecular sieve 13x, coupled with microwave dielectric heating phenomenon, MRSHP technology is employed as a regenerative filter for a contaminated hydrogen gas stream. By design, freshly regenerated molecular sieve 13x contained in the MRSHP will remove contaminants from the effluent of a 1-CM scale PPA for several hours prior to breakthrough. By reversing flow and pulling a relative vacuum the MRSHP prototype then uses 2.45 GHz microwave power, applied through a novel coaxial antenna array, to rapidly heat the sorbent bed and drive off the contaminants in a short duration vacuum/thermal contaminant desorption step. Finally, following rapid cooling via room temperature cold plates, the MRSHP is again ready to serve as a hydrogen filter.

  20. Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

    Science.gov (United States)

    Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

    Energy Technology Data Exchange (ETDEWEB)

    Bravo, Manuel [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France); Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Lespes, Gaetane; Gautier, Martine Potin [Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Gregori, Ida de; Pinochet, Hugo [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France)

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 {mu}m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L{sup -1} in water and close to ng (Sn) kg{sup -1} in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. (orig.)

  2. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD).

    Science.gov (United States)

    Bravo, Manuel; Lespes, Gaëtane; De Gregori, Ida; Pinochet, Hugo; Gautier, Martine Potin

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mum PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L(-1) in water and close to ng (Sn) kg(-1) in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices.

  3. HS-SPME GC/MS characterization of volatiles in raw and dry-roasted almonds (Prunus dulcis).

    Science.gov (United States)

    Xiao, Lu; Lee, Jihyun; Zhang, Gong; Ebeler, Susan E; Wickramasinghe, Niramani; Seiber, James; Mitchell, Alyson E

    2014-05-15

    A robust HS-SPME and GC/MS method was developed for analyzing the composition of volatiles in raw and dry-roasted almonds. Almonds were analyzed directly as ground almonds extracted at room temperature. In total, 58 volatiles were identified in raw and roasted almonds. Straight chain aldehydes and alcohols demonstrated significant but minimal increases, while the levels of branch-chain aldehydes, alcohols, heterocyclic and sulfur containing compounds increased significantly (500-fold) in response to roasting (p<0.05). Benzaldehyde decreased from 2934.6±272.5 ng/g (raw almonds) to 315.8±70.0 ng/g (averaged across the roasting treatments evaluated i.e. 28, 33 and 38 min at 138 °C) after roasting. Pyrazines were detected in only the roasted almonds, with the exception of 2,5-dimethylpyrazine, which was also found in raw almonds. The concentration of most alcohols increased in the roasted samples with the exception of 2-methyl-1-propanol, 3-methyl-1-butanol and 2-phenylethyl alcohol, which decreased 68%, 80%, and 86%, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Analytic escrutineo for plaguicidas organofosforados in blood in forensic cases by means of SPME-GC/NPD

    International Nuclear Information System (INIS)

    Fernandez Quesada, K.; Saenz Ugalde, M. F.

    2003-01-01

    The plaguicidas organophosphorus represent one of the most important causes of intoxication in Costa Rica; 20% of the cases received in the Section of Toxicology of the Department of Forensic Sciences of the Organism of Judicial Investigation (OIJ) are related to these plaguicidas. At the present time, the employed techniques in this institution to carry out the organophosphorus analyses in blood, present important limitations in their analytic potential. As a consequence, it is necessary to look for new methodologies, with the purpose to obtain a great specificity, and to diminish the limits of detection. This would allow a more qualified service that assures the validity and reliability of the results. Besides, it is an ideal instrument for the correct administration of justice of the Judicial Authorities. In this final work of graduation, it develops a methodology for the scrutiny of pesticides organophosphorus, in which a sample of biological origin of forensic importance is used. This employs a technique of quick, simple and clean extraction, using a separation method of detection of high analytic sensibility. In the methodology's development, samples of total blood, and the microextraccion techniques in solid phase will be used (SPME), and detection with gas chromatography by a specific instrumental detector of match and nitrogen (GCINPD) [es

  5. [Difference of volatile constituents contained in female and male flowers of Trichosanthes kirilowii by HS-SPME-GC-MS].

    Science.gov (United States)

    Sun, Wen; Chao, Zhimao; Wang, Chun; Wu, Xiaoyi; Tan, Zhigao

    2012-06-01

    To compare and analyze volatile constituents from flowers of Trichosanthes kirilowii, in order to point out characteristic differences between female and male flowers. Blooming female and male flowers were collected in the same place. Volatile constituents were extracted from the flower by solid phase micro-extraction (SPME), then separated and analyzed by gas chromatography-mass-spectrometry (GC-MS). Fifty-two and forty-five chromatographic peaks were separated from the female and male flowers, respectively. Forty seven constituents were identified and their relative percentage compositions were determined with the peak area normalization method. Linalool, alpha-farnesene, benzene methanol, and (Z)-2-methylbutanal oxime were the main volatile constituents. The contents of linalool and alpha-farnesene in female flower were remarkably higher than those in male. In contrast, the content of benzene methanol in male flower was remarkably higher than that in female. In the first study on chemical constituents from flowers in genus Trichosanthes, 37 compounds are separated from T. kirilowii. Contents of linalool, alpha-farnesene and benzene methanol show the characteristic differences of volatile constituents contained in male and female flowers of T. kirilowii, which enriches the basic studies on dioecious plant.

  6. Analysis of volatile compounds in gluten-free bread crusts with an optimised and validated SPME-GC/QTOF methodology.

    Science.gov (United States)

    Pico, Joana; Antolín, Beatriz; Román, Laura; Gómez, Manuel; Bernal, José

    2018-04-01

    The aroma of bread crust, as one of the first characteristics perceived, is essential for bread acceptance. However, gluten-free bread crusts exhibit weak aroma. A SPME-GC/QTOF methodology was optimised with PCA and RSM and validated for the quantification of 44 volatile compounds in bread crust, extracting 0.75 g of crust at 60 °C for 51 min. LODs ranged between 3.60 and 1760 μg Kg -1 , all the R 2 were higher than 0.99 and %RSD for precision and %Er for accuracy were lower than 9% and 12%, respectively. A commercial wheat bread crust was quantified, and furfural was the most abundant compound. Bread crusts of wheat starch and of japonica rice, basmati rice and teff flours were also quantified. Teff flour and wheat starch crusts were very suitable for improving gluten-free bread crust aroma, due to their similar content in 2-acetyl-1-pyrroline and 4-hydroxy-2,5-dimethyl-3(2H)-furanone compared to wheat flour crust and also for their high content in pyrazines. Copyright © 2018 Elsevier Ltd. All rights reserved.

  7. Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products.

    Science.gov (United States)

    Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

    2017-12-01

    For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.

  8. Study of the factors affecting the performance of microextraction by packed sorbent (MEPS) using liquid scintillation counter and liquid chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Altun, Zeki [Karlstad University, Faculty of Technology and Science, SE-651 88 Karlstad (Sweden); Abdel-Rehim, Mohamed [Karlstad University, Faculty of Technology and Science, SE-651 88 Karlstad (Sweden); Clinical Pharmacology and DMPK, AstraZeneca R and D Soedertaelje, SE-151 85 Soedertaelje (Sweden)], E-mail: Mohamed.Abdel-Rehim@Astrazeneca.com

    2008-12-23

    Microextraction by packed sorbent (MEPS) is a new technique for sample preparation that can be connected on-line with LC or GC. In MEPS, approximately 1-2 mg of the solid packing material is inserted into a syringe (100-250 {mu}L) as a plug. Sample preparation takes place on the packed bed. The bed can be packed or coated to provide selective and suitable sampling conditions. The new method is very promising for extraction of drugs and metabolites from biological samples. In this paper, some factors affecting the performance of MEPS such as recovery, carry-over, leakage, washing volume and elution volume were studied using C18 and hydroxylated polystyrene-divinylbenzene copolymer (ENV+) as sorbents. Radioactively labelled bupivacaine in plasma samples was used as test analyte. For the extraction of this drug, using methanol/water 95:5 (v/v) (0.25% ammonium hydroxide) was used as elution solvent. The analyte response increased with increasing the elution volume and it was linear upp up to 100 {mu}L utilizing liquid scintillation counter. Further, for concentrating the sample, we found that MEPS may be used such that the sample can be drawn through the needle, up and down, several times. The analyte leakage increases as the volume washing increases, though higher washing volumes may also result in cleaner extracts. To eliminate analyte carry-over, the sorbents were washed first with 3 x 250 {mu}L elution solution and then with 3 x 250 {mu}L washing solution. In addition, the reproducibility measurements show relatively good relative standard deviation (RSD) % values concerning analyte recovery and analyte leakage. The present study provides an understanding of basic aspects when optimizing methods for MEPS. In this study, MEPS was used off-line with liquid scintillation counter and on-line with LC-MS/MS.

  9. Different CO2 absorbents-modified SBA-15 sorbent for highly selective CO2 capture

    Science.gov (United States)

    Liu, Xiuwu; Zhai, Xinru; Liu, Dongyang; Sun, Yan

    2017-05-01

    Different CO2 absorbents-modified SBA-15 materials are used as CO2 sorbent to improve the selectivity of CH4/CO2 separation. The SBA-15 sorbents modified by physical CO2 absorbents are very limited to increasing CO2 adsorption and present poor selectivity. However, the SBA-15 sorbents modified by chemical CO2 absorbents increase CO2 adsorption capacity obviously. The separation coefficients of CO2/CH4 increase in this case. The adsorption and regeneration properties of the SBA-15 sorbents modified by TEA, MDEA and DIPA have been compared. The SBA-15 modified by triethanolamine (TEA) presents better CO2/CH4 separation performance than the materials modified by other CO2 absorbents.

  10. Zinc-oxide-based sorbents and processes for preparing and using same

    Science.gov (United States)

    Gangwal, Santosh Kumar; Turk, Brian Scott; Gupta, Raghubir Prasael

    2010-03-23

    Zinc oxide-based sorbents, and processes for preparing and using them are provided. The sorbents are preferably used to remove one or more reduced sulfur species from gas streams. The sorbents comprise an active zinc component, optionally in combination with one or more promoter components and/or one or more substantially inert components. The active zinc component is a two phase material, consisting essentially of a zinc oxide (ZnO) phase and a zinc aluminate (ZnAl.sub.2O.sub.4) phase. Each of the two phases is characterized by a relatively small crystallite size of typically less than about 500 Angstroms. Preferably the sorbents are prepared by converting a precursor mixture, comprising a precipitated zinc oxide precursor and a precipitated aluminum oxide precursor, to the two-phase, active zinc oxide containing component.

  11. Mars CO2 Capture using Sorbent Fiber Materials for In-situ Resource Utilization (ISRU)

    Data.gov (United States)

    National Aeronautics and Space Administration — Determine the amount of Carbon Dioxide (CO2) that is adsorbed (in moles) under simulated Mars atmospheric conditions per unit mass of sorbent fiber material as a...

  12. Application of magnetic sorbent in the removal of cadmium from soils

    Directory of Open Access Journals (Sweden)

    Michal Lovás

    2006-12-01

    Full Text Available A contamination of soil by heavy metals is a common problem at many metalliferous mining sites. There are various treatment processes for the cleanup of soil contaminated with heavy metals. A method designed for the decontamination of soil polluted by Cd is described. The method utilizes a magnetic sorbent – sludges from the hydrometallurgic processing of nickel mineral, activated by milling. The influence of sorbent concentration, pH and microwave energy on the sorption capacity and content of Cd ions in a soil was studed. The effectiveness of Cd desorption from the soil was 75 %, the maximal sorption capacity of sorbent was 9,8 mg/g. The content of Cd in water is function of pH and the concentration of sorbent. The influence of microwave energy (90 W was negligible.

  13. High efficiency nanocomposite sorbents for CO2 capture based on amine-functionalized mesoporous capsules

    KAUST Repository

    Qi, Genggeng

    2011-01-01

    A novel high efficiency nanocomposite sorbent for CO2 capture has been developed based on oligomeric amine (polyethylenimine, PEI, and tetraethylenepentamine, TEPA) functionalized mesoporous silica capsules. The newly synthesized sorbents exhibit extraordinary capture capacity up to 7.9 mmol g-1 under simulated flue gas conditions (pre-humidified 10% CO 2). The CO2 capture kinetics were found to be fast and reached 90% of the total capacities within the first few minutes. The effects of the mesoporous capsule features such as particle size and shell thickness on CO2 capture capacity were investigated. Larger particle size, higher interior void volume and thinner mesoporous shell thickness all improved the CO2 capacity of the sorbents. PEI impregnated sorbents showed good reversibility and stability during cyclic adsorption-regeneration tests (50 cycles). © 2011 The Royal Society of Chemistry.

  14. Evaluation of Solid Sorbents as a Retrofit Technology for CO2 Capture

    Energy Technology Data Exchange (ETDEWEB)

    Sjostrom, Sharon [Ada-Es, Inc., Highlands Ranch, CO (United States)

    2016-06-02

    ADA completed a DOE-sponsored program titled Evaluation of Solid Sorbents as a Retrofit Technology for CO2 Capture under program DE-FE0004343. During this program, sorbents were analyzed for use in a post-combustion CO2 capture process. A supported amine sorbent was selected based upon superior performance to adsorb a greater amount of CO2 than the activated carbon sorbents tested. When the most ideal sorbent at the time was selected, it was characterized and used to create a preliminary techno-economic analysis (TEA). A preliminary 550 MW coal-fired power plant using Illinois #6 bituminous coal was designed with a solid sorbent CO2 capture system using the selected supported amine sorbent to both facilitate the TEA and to create the necessary framework to scale down the design to a 1 MWe equivalent slipstream pilot facility. The preliminary techno-economic analysis showed promising results and potential for improved performance for CO2 capture compared to conventional MEA systems. As a result, a 1 MWe equivalent solid sorbent system was designed, constructed, and then installed at a coal-fired power plant in Alabama. The pilot was designed to capture 90% of the CO2 from the incoming flue gas at 1 MWe net electrical generating equivalent. Testing was not possible at the design conditions due to changes in sorbent handling characteristics at post-regenerator temperatures that were not properly incorporated into the pilot design. Thus, severe pluggage occurred at nominally 60% of the design sorbent circulation rate with heated sorbent, although no handling issues were noted when the system was operated prior to bringing the regenerator to operating temperature. Testing within the constraints of the pilot plant resulted in 90% capture of the incoming CO2 at a flow rate equivalent of 0.2 to 0.25 MWe net electrical generating equivalent. The reduction in equivalent flow rate at 90% capture was

  15. Chitosan-ferrocyanide sorbent for Cs-137 removal from mineralized alkaline media

    Energy Technology Data Exchange (ETDEWEB)

    Egorin, Andrei [Far Eastern Federal Univ., Vladivostok (Russian Federation); Institute of Chemistry FEBRAS, Vladivostok (Russian Federation); Ozyorsk Technical Institute MEPHI, Ozersk (Russian Federation); Tokar, Eduard [Far Eastern Federal Univ., Vladivostok (Russian Federation); Zemskova, Larisa [Institute of Chemistry FEBRAS, Vladivostok (Russian Federation)

    2016-11-01

    An organomineral sorbent based on mixed nickel-potassium ferrocyanide and chitosan to be used in removal of Cs-137 radionuclide from highly mineralized media with high pH has been fabricated. The synthesized sorbent was applied to remove Cs-137 from model solutions under static and dynamic conditions. The effects of contact time, pH, and presence of sodium ions and complexing agents in the process of Cs-137 removal have been investigated. The sorbent is distinguished by increased stability to the impact of alkaline media containing complexing agents, whereas the sorbent capacity in solutions with pH 11 exceeds 1000 bed volumes with the Cs-137 removal efficiency higher than 95%.

  16. Purification of low level activity water by means of selective sorbents

    International Nuclear Information System (INIS)

    Berak, L.

    1978-01-01

    Results are stated of the investigations undertaken to study properties of selective sorbents used for purification of radioactive water. Main efforts were directed towards increase of sorption selectivity of sorbents with respect to radioactive isotopes of strontium and radium. Results of the investigations can find an application for therapeutics in the case of radionuclider penetration into the digestive system of man. Works were done for finding a sorbent capable to lower natural water activity when the water contains radium-226 and some type of wastes containing strontium-90 and also a sopbent for maximum reduction of activity of solutions with high salts content. Properties are given of sorbents on the base of alumosilicates in gel from, alcaline earth metals phosphates, hydrated oxides, barium sulphate, some natural organic compounds and ionites made of sulfated styrene copolymers. (I.T.) [ru

  17. Application of fibrous complexing sorbents for trace elements preconcentration and separation

    International Nuclear Information System (INIS)

    Zakhartchenko, E.A.; Myasoedova, G.V.

    2003-01-01

    This article demonstrates the application of the 'filled' fibrous sorbents for preconcentration and separation of platinum metals, as well as heavy metals and radionuclides. The POLYORGS complexing sorbents and ion-exchangers were used as fillers. Dynamic preconcentration conditions should be set for complete sorption of the elements: diameter and mass of the sorbent disk or the column as well as flow rate of the solution. These conditions depend on specific features of materials to be analysed and the requirements of the experimental task or detection method. Extensive alteration of features as well as perfect kinetic properties and high selectivity of the 'filled' sorbents confirm their applicability for trace elements preconcentration and separation in technology and analytical chemistry. (authors)

  18. Purification of liquid radioactive wastes of different salinity by sorbents of Termoksid type

    International Nuclear Information System (INIS)

    Komarevskij, V.M.; Stepanets, O.V.; Sharygin, L.M.

    2000-01-01

    Results of use of sorbents of Termoksid sort for purification of solutions of complex composition from radioactive impurities are presented. It is shown that for solution-imitators of liquid wastes of laundry and still bottoms of nuclear power plants containing considerable quantities of organic and inorganic impurities high coefficients of purification from Cs 137 (not less than 100) are observed when resources of sorbent are 400-500 of column volumes. It permits to reprocess great volumes of water effectively with low quantities of sorbents. Taking into account these results and high radiation resistance of sorbents of Termoksid sort conclusion are made about outlook of their industrial application in reprocessing of large volumes of liquid radioactive wastes [ru

  19. Sorption of short-lived radionuclides in a layer of sorbent with spherical granules

    International Nuclear Information System (INIS)

    Karlin, Yu.V.

    1993-01-01

    Sorption methods have found wide application in the purification of liquid radioactive wastes. The working element in sorption methods for this purpose is usually a sorption column with a fixed layer of sorbent. Continuous-action equipment with a moving layer of sorbent is very seldom used. When a fixed layer of sorbent is used its wear and prolonged mixing in the sorption column are reduced to a minimum, and maximum purification is achieved due to the advantages of the dynamic method of sorption over the static method. The time of protective action of the sorbent layer is determined by the time taken for the radionuclide to pass through the sorption column, and for the majority of radionuclides is determined by numerous parameters, including the type of sorbent and radionuclide, the rate of flow through the sorbent, the size of the sorbent granules, etc. The physical and chemical aspects of this process have been investigated in detail, and numerous methods for modeling it mathematically have been developed and have been used to develop methods of designing sorption column apparatus. The specific nature of the radionuclides as unstable materials enables the hypothetical case of a open-quotes perpetualclose quotes sorption filter to be represented. In fact, to achieve this it is only necessary to assume that the half-life of the radionuclide is so small that the rate of decay of the radionuclide in the sorption column (both in the sorbed state and in the aqueous phase of the sorption layer) is equal to the rate that it is fed into the column in the flow of liquid radioactive waste. In this case the sorption front of the radionuclide in the column wall remains fixed after a certain initial period. In this paper, a mathematical model of such a hypothetical filter for the case of spherical sorbent granules is considered

  20. Uranium extraction from sea water with a granulated titanium-containing sorbent

    International Nuclear Information System (INIS)

    Novikov, Yu.P.; Komarewsky, V.M.; Myasoedov, B.F.; Sharyigin, L.M.; Gonchar, V.F.; Malyich, T.G.

    1981-01-01

    A specially synthesized granulated titanium dioxide based sorbent of high mechanical strength was used for the extraction of uranium from sea water in a fluidized bed. The sorption process proceeds in an external diffusion kinetic area and depends only slightly on temperature. The kinetic behaviour of any sorbent during uranium extraction from natural sea water is assumed to be the same up to the moment of the process transition from the external to the internal kinetic area. (author)

  1. Silver nanoparticles embedded polymer sorbent for preconcentration of uranium from bio-aggressive aqueous media

    International Nuclear Information System (INIS)

    Das, Sadananda; Pandey, Ashok K.; Athawale, Anjali A.; Subramanian, M.; Seshagiri, T.K.; Khanna, Pawan K.; Manchanda, Vijay K.

    2011-01-01

    Adsorptive sorbent for bio-aggressive natural aqueous media like seawater was developed by one pot simultaneous synthesis of silver nanoparticles (Ag nps) and poly(ethylene glycol methacrylate phosphate) (PEGMP) by UV-initiator induced photo-polymerization. The photo-polymerization was carried out by irradiating N,N'-dimethylformamide (DMF) solution containing appropriate amounts of the functional monomer (ethylene glycol methacrylate phosphate), UV initiator (α,α'-dimethoxy-α-phenyl acetophenone), and Ag + ions with 365 nm UV light in a multilamps photoreactor. To increase mechanical strength, nano-composite sorbent (Ag-PEGMP) was also reinforced with thermally bonded non-woven poly(propylene) fibrous sheet. Transmission electron microscopy (TEM) of the nano-composite sorbent showed uniform distribution of spherical Ag nanoparticles with particles size ranging from 3 to 6 nm. The maximum amount of Ag 0 that could be anchored in the form of nanoparticles were 5 ± 1 and 10 ± 1 wt.% in self-supported PEGMP and poly(propylene) reinforced PEGMP matrices, respectively. Ag-PEGMP sorbent was found to be stable under ambient conditions for a period of six months. Ag-PEGMP composite sorbent did not exhibit growth at all after incubation with pre-grown Escherichia coli cells, and showed non-adherence of this bacteria to the composite. This indicated that composite sorbent has the bio-resistivity due to bacterial repulsion and bactericidal properties of Ag nanoparticles embedded in the PEGMP. Sorption of U(VI) in PEGMP and Ag-PEGMP nano-composite sorbents from well-stirred seawater was studied to explore the possibility of using it for uranium preconcentration from bio-aggressive aqueous streams. The nano-composite sorbent was used to preconcentrate U(VI) from a process aqueous waste stream.

  2. The Precious metals (Au, Ag, Pt, Pd, Rh) adsorption on the Silicon – organic sorbents

    OpenAIRE

    G Burmaa; S Alen; Yu Ganchimeg; I Sukhbaatar

    2014-01-01

    Sorption activity of two types of Silicon-organic sorbents for the previous metals has been studied. A polymer – poly (3- silsesquioxanilpropylthiocarbamate) - 3- silsesquioxanilpropylammonium which was obtained by the hydrolytic poly-condensation reaction and has been determined its physical, chemical characteristics and its sorption activity for the Ag(I), Au(III), Pt(IV), Pd(II), Rh(III). It has been found out that the sorbent shows high static sorption of Gold (III), Mercury (II) at acidi...

  3. Theoretical Predictions of the thermodynamic Properties of Solid Sorbents Capture CO2 Applications

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yuhua; Sorescu, Dan; Luebke David; Pennline, Henry

    2012-05-02

    We are establishing a theoretical procedure to identify most potential candidates of CO{sub 2} solid sorbents from a large solid material databank to meet the DOE programmatic goal for energy conversion; and to explore the optimal working conditions for the promising CO{sub 2} solid sorbents, especially from room to warm T ranges with optimal energy usage, used for both pre- and post-combustion capture technologies.

  4. Mixed and Doped Solid Sorbents for CO2 Capture Applications

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yuhua [National Energy Technology Lab. (NETL), Albany, OR (United States)

    2016-06-14

    The objectives of this presentation are to capture CO2 we need materials with optimal performance and low costs; establish a theoretical procedure to identify most potential candidates of CO2 solid sorbents from a large solid material databank; computational synthesis new materials to fit industrial needs; and explore the optimal working conditions for the promised CO2 solid sorbents, especially from room to warm T ranges with optimal energy usage.

  5. Determination of trace levels of parabens in real matrices by bar adsorptive microextraction using selective sorbent phases.

    Science.gov (United States)

    Almeida, C; Nogueira, J M F

    2014-06-27

    In the present work, the development of an analytical methodology which combines bar adsorptive microextraction with microliquid desorption followed by high performance liquid chromatography-diode array detection (BAμE-μLD/HPLC-DAD) is proposed for the determination of trace levels of four parabens (methyl, ethyl, propyl and buthyl paraben) in real matrices. By comparing six polymer (P1, P2, P3, P4, P5 and P6) and five activated carbon (AC1, AC2, AC3, AC4 and AC5) coatings through BAμE, AC2 exhibited much higher selectivity and efficiency from all the sorbent phases tested, even when compared with the commercial stir bar sorptive extraction with polydimethylsiloxane. Assays performed through BAμE(AC2, 1.7mg) on 25mL of ultrapure water samples spiked at the 8.0μg/L level, yielded recoveries ranging from 85.6±6.3% to 100.6±11.8%, under optimized experimental conditions. The analytical performance showed also convenient limits of detection (0.1μg/L) and quantification (0.3μg/L), as well as good linear dynamic ranges (0.5-28.0μg/L) with remarkable determination coefficients (r(2)>0.9982). Excellent repeatability was also achieved through intraday (RSDparabens, under optimized experimental conditions, showing that this analytical technology can be design to operate with lower volumes of sample and desorption solvent, thus increasing the sensitivity and effectiveness. The application of the proposed analytical approach using the standard addition methodology on tap, underground, estuarine, swimming pool and waste water samples, as well as on commercial cosmetic products and urine samples, revealed good sensitivity, absence of matrix effects and the occurrence of levels of some parabens. Moreover, the present methodology is easy to implement, reliable, sensitive, requiring low sample and minimized desorption solvent volume, having the possibility to tune the most selective sorbent coating, according to the target compounds involved. Copyright © 2014 Elsevier B

  6. Characterization of Modified and Polymer Coated Alumina Surfaces by Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available The prepared, modified, and coated alumina surfaces were characterized by infrared spectroscopy (FTIR to investigate the surface properties of the individual and double modified samples. FTIR helps in reporting the changes occurred in hydroxyl groups as well as the structure changes as a result of thermal treating, hydrothermal treating, silylation treating, alkali metal treating, coating, and bonding with polymer. FTIR spectroscopy represents the strength and abundance of surface acidic OH which determine the adsorption properties of polar and nonpolar sorbents. Generally, all treated samples exhibit decrease of OH groups compared with those of parent ones producing alumina surfaces of different adsorptive powers.

  7. Experimental evaluation of sorbents for sulfur control in a coal-fueled gas turbine slagging combustor

    International Nuclear Information System (INIS)

    Cowell, L.H.; Wen, C.S.; LeCren, R.T.

    1992-01-01

    This paper reports on a slagging combustor that has been used to evaluate three calcium-based sorbents for sulfur capture efficiency in order to assess their applicability for use in a oil-fueled gas turbine. Testing is competed in a bench-scale combustor with one-tenth the heat input needed for the full-scale gas turbine. The bench-scale rig is a two-stage combustor featuring a fuel-rich primary zone an a fuel-lean secondary zone. The combustor is operated at 6.5 bars with inlet air preheated to 600 K. Gas temperatures of 1840 K are generated in the primary zone and 1280 K in the secondary zone. Sorbents are either fed into the secondary zone or mixed with the coal-water mixture and fed into the primary zone. Dry powered sorbents are fed into the secondary zone by an auger into one of six secondary air inlet ports. The three sorbents tested in the secondary zone include dolomite, pressure-hydrated dolomitic lime, and hydrated lime. Sorbents have been tested while burning coal-water mixtures with coal sulfur loadings of 0.56 to 3.13 weight percent sulfur. Sorbents are injected into the secondary zone at varying flow rates such that the calcium/sulfur ratio varies from 0.5 to 10.0

  8. Sorption of uranium from carbonate-containing solutions by inorganic sorbents. IX. Kinetics of uranium sorption by fibers packed with finely divided sorbents

    International Nuclear Information System (INIS)

    Mikheeva, M.N.; Myasoedov, B.F.; Novikov, Yu.P.; Komarevskii, V.M.; Mezhirov, M.S.; Idiatulov, R.K.; Fedorova, A.N.

    1988-01-01

    We studied the kinetics at 20-65 degree C of uranium sorption from carbonate-containing seawaters at pH 7.85 ± 0.05 by polyacrylonitrile fibers to which was added, during preparation, 50-80% of Termoksid-5 titanium-containing sorbent ground to 1-3 μm. The sorption kinetics was described by an equation relating the theoretical uranium sorption rate constant to temperature and uranium concentration in the original solution. The constant was independent of the degree to which the fiber was packed with sorbent over the range studied

  9. Dopamine functionalized tannic-acid-templated mesoporous silica nanoparticles as a new sorbent for the efficient removal of Cu2+ from aqueous solution

    Science.gov (United States)

    Gao, Junkai; Lei, Hao; Han, Zhi; Shi, Qian; Chen, Yan; Jiang, Yanjun

    2017-03-01

    A simple, environmentally friendly and cost-effective nonsurfactant template method was used to synthesize tannic-acid-templated mesoporous silica nanoparticles (TMSNs), and then dopamine functionalized TMSNs (Dop-TMSNs) which was synthesized by a facile and biomimetic coating strategy, was developed as a new sorbent for the removal of Cu2+ from aqueous solution. The Dop-TMSNs were thoroughly characterized by SEM, TEM, BET, FT-IR and TGA, and the effects of contact time, initial pH, K+ and Na+ concentrations, co-existing polyvalent metal ions and adsorption-desorption cycle times on the sorption capacity of Dop-TMSNs were studied. It was demonstrated that the maximum adsorption capacity of Cu2+ by Dop-TMSNs was 58.7 mg/g at pH 5.5, and the sorption reached equilibrium within 180 min. Moreover, the K+ and Na+ concentrations had a very slight influence on the sorption process and the adsorption capacity of the Dop-TMSNs still remained 89.2% after recycling for four times. All the results indicated that the Dop-TMSNs could be utilized as an excellent sorbent for the sequestration of Cu2+.

  10. Modified surface based on magnetic nanocomposite of dithiooxamide/Fe{sub 3}O{sub 4} as a sorbent for preconcentration and determination of trace amounts of copper

    Energy Technology Data Exchange (ETDEWEB)

    Mirabi, Ali, E-mail: mirabi2012@yahoo.com [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Shokuhi Rad, Ali, E-mail: a.shokuhi@gmail.com [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Khodadad, Hadiseh [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

    2015-09-01

    Magnetic nanocomposites surface (MNCS) which has anionic surfactant sodium dodecyl sulfate (SDS) coating and has undergone dithiooxamide treatment as the sorbent could be an easy and useful method to extract and make a pre-concentrated in detecting the copper ions before they are determined via the flame atomic absorption spectrometry (FAAS). The influences of the experimental parameters such as the pH of the sample, the type and concentration of the eluent, dithiooxamide concentration and volume, amount of sorbent and the interactions of ions with respect to the copper ion detection have been studied. The calibration graph was linear in the range of 2–600 ng ml{sup −1} with detection limit of 0.2 ng ml{sup −1}. Relative standard deviation (RSD) for 6 replicate measurements was 1.8%. This method of detection has been applied to the determination of Cu ions at levels in real samples such as wheat flour, tomatoes, potatoes, red beans, oat, tap water, river water and sea water with satisfactory results. - Highlights: • Fe{sub 3}O{sub 4} nano-magnetic improved by SDS/dithiooxamide. • It can be used in both the pre-concentration function and detecting of Cu ions. • This modified surface shows high adsorptive characteristics. • This procedure is relatively simple, fast and imposes less test analysis expenses.

  11. Chlorophenol's ultra-trace analysis in environmental samples by chitosan-zinc oxide nanorod composite as a novel coating for solid phase micro-extraction combined with high performance liquid chromatography.

    Science.gov (United States)

    Alizadeh, Reza

    2016-01-01

    In this study, a simple, novel, and efficient preconcentration method has been developed for the determination of some chlorophenols (4-chlorophenol, 2,5-dichlorophenol, 2,3-dichlorophenol, and 2,4,6-trichlorophenol) using a direct solid phase microextraction (D-SPME) based on chitosan-ZnO nanorod composite combined with high performance liquid chromatography (HPLC). A one step-novel hydrothermal method was demonstrated on the fabrication of ZnO nanorods arrayed on the fused silica fiber in the chitosan hydrogel solution (CZNC) as a new coating of SPME fiber. The coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) instruments. The CZNC coating has combined the merits of both ZnO nanorods and chitosan hydrogel; it has several improvements such as increased extraction efficiency of chlorophenols and longer life time (over 80 cycles of D-SPME-HPLC operation). Experimental design method was used for optimization of extraction conditions and determination of four chlorophenols in water samples by SPME-HPLC-UV method. The calibration curves were linear from 5 to 1000 µg L(-1) for analytes, and the limits of detection were between 0.1 and 2 µg L(-1). Single fiber repeatability and fiber-to-fiber reproducibility were in the range of 5.8-10.2% and 8.8-14.5%, respectively. The spiked recoveries at 50 µg L(-1) for environmental water sample were in the range of 93-102%. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Development of a Catalyst/Sorbent for Methane Reforming

    Energy Technology Data Exchange (ETDEWEB)

    B.H. Shans; T.D. Wheelock; Justinus Satrio; Karl Albrecht; Tanya Harris Janine Keeley; Ben Silva; Aaron Shell; Molly Lohry; Zachary Beversdorf

    2008-12-31

    This project led to the further development of a combined catalyst and sorbent for improving the process technology required for converting CH{sub 4} and/or CO into H{sub 2} while simultaneously separating the CO{sub 2} byproduct all in a single step. The new material is in the form of core-in-shell pellets such that each pellet consists of a CaO core surrounded by an alumina-based shell capable of supporting a Ni catalyst. The Ni is capable of catalyzing the reactions of steam with CH{sub 4} or CO to produce H{sub 2} and CO{sub 2}, whereas the CaO is capable of absorbing the CO{sub 2} as it is produced. The absorption of CO{sub 2} eliminates the reaction inhibiting effects of CO{sub 2} and provides a means for recovering the CO{sub 2} in a useful form. The present work showed that the lifecycle performance of the sorbent can be improved either by incorporating a specific amount of MgO in the material or by calcining CaO derived from limestone at 1100 C for an extended period. It also showed how to prepare a strong shell material with a large surface area required for supporting an active Ni catalyst. The method combines graded particles of {alpha}-alumina with noncrystalline alumina having a large specific surface area together with a strength promoting additive followed by controlled calcination. Two different additives produced good results: 3 {micro}m limestone and lanthanum nitrate which were converted to their respective oxides upon calcination. The oxides partially reacted with the alumina to form aluminates which probably accounted for the strength enhancing properties of the additives. The use of lanthanum made it possible to calcine the shell material at a lower temperature, which was less detrimental to the surface area, but still capable of producing a strong shell. Core-in-shell pellets made with the improved shell materials and impregnated with a Ni catalyst were used for steam reforming CH{sub 4} at different temperatures and pressures. Under all

  13. PENJERAPAN GAS CO HASIL PEMBAKARAN SAMPAH MENGGUNAKAN SORBENT TERMODIFIKASI DALAM REAKTOR FIXED BED

    Directory of Open Access Journals (Sweden)

    Mariana Mariana

    2013-11-01

    Full Text Available ADSORPTION OF CO FROM WASTE COMBUSTION USING MODIFIED SORBENT IN A FIXED BED REACTOR. Gases produced by garbage burning consist of dangerous gases such as CO, SO2 and other gases. Technology for reducing dangerous gases from incinerator outlet can be done by using a dry or wet process. The dry process is more economical process because of simple process, easy maintenance and no liquid waste as product. However, the weakness of the dry process is low absorption conversion and low gas removal efficiency. One way to overcome these problems is to use sorbent which has high reactivity. An inexpensive sorbent that commonly used is Ca(OH2. The aim of this research was to increase the reactivity of Ca(OH2 sorbent by using diatomaceous earth and compost as a source of silica and biosorbent, respectively. Diatomaceous earth contains CaO, SiO2 and Al2O3 and compost contains bacteria as a biosorbent that can convert CO to CO2 and CH4. The reaction between SiO2 and Ca(OH2 would form calcium silicate hydrate (CaO.SiO2.2H2O that has a high porosity and reactivity. The results showed that the reactivity of Ca(OH2 sorbent increased by addition of diatomaceous earth and compost. The results also showed that the sorption of CO gas increases with increasing of height of sorbent bed and temperature. The highest CO gas sorption was obtained at temperature of 150oC and sorbent bed height of 6 cm using the modified sorbent with Ca(OH2/DE/compost ratio of 3:1:1. Gas hasil pembakaran sampah terdiri dari gas-gas yang berbahaya seperti CO, SO2 dan lain sebagainya. Teknologi penghilangan gas-gas tersebut dapat dilakukan dengan menggunakan proses kering maupun proses basah. Penghilangan dengan proses kering lebih ekonomis karena sederhana, mudah pemeliharaan dan tidak menghasilkan limbah cair. Namun demikian, kelemahan proses kering adalah konversi absorpsi rendah dan efisiensi penyisihan  gas relatif kecil. Salah satu cara mengatasi masalah tersebut di atas adalah dengan

  14. Development of Novel Sorbents for Uranium Extraction from Seawater

    International Nuclear Information System (INIS)

    Lin, Wenbin; Taylor-Pashow, Kathryn

    2014-01-01

    As the uranium resource in terrestrial ores is limited, it is difficult to ensure a long-term sustainable nuclear energy technology. The oceans contain approximately 4.5 billion tons of uranium, which is one thousand times the amount of uranium in terrestrial ores. Development of technologies to recover the uranium from seawater would greatly improve the uranium resource availability, sustaining the fuel supply for nuclear energy. Several methods have been previously evaluated including solvent extraction, ion exchange, flotation, biomass collection, and adsorption; however, none have been found to be suitable for reasons such as cost effectiveness, long term stability, and selectivity. Recent research has focused on the amidoxime functional group as a promising candidate for uranium sorption. Polymer beads and fibers have been functionalized with amidoxime functional groups, and uranium adsorption capacities as high as 1.5 g U/kg adsorbent have recently been reported with these types of materials. As uranium concentration in seawater is only ~3 ppb, great improvements to uranium collection systems must be made in order to make uranium extraction from seawater economically feasible. This proposed research intends to develop transformative technologies for economic uranium extraction from seawater. The Lin group will design advanced porous supports by taking advantage of recent breakthroughs in nanoscience and nanotechnology and incorporate high densities of well-designed chelators into such nanoporous supports to allow selective and efficient binding of uranyl ions from seawater. Several classes of nanoporous materials, including mesoporous silica nanoparticles (MSNs), mesoporous carbon nanoparticles (MCNs), meta-organic frameworks (MOFs), and covalent-organic frameworks (COFs), will be synthesized. Selective uranium-binding liagnds such as amidoxime will be incorporated into the nanoporous materials to afford a new generation of sorbent materials that will be

  15. Development of Novel Sorbents for Uranium Extraction from Seawater

    Energy Technology Data Exchange (ETDEWEB)

    Lin, Wenbin [Univ. of Chicago, IL (United States); Taylor-Pashow, Kathryn [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2014-01-08

    As the uranium resource in terrestrial ores is limited, it is difficult to ensure a long-term sustainable nuclear energy technology. The oceans contain approximately 4.5 billion tons of uranium, which is one thousand times the amount of uranium in terrestrial ores. Development of technologies to recover the uranium from seawater would greatly improve the uranium resource availability, sustaining the fuel supply for nuclear energy. Several methods have been previously evaluated including solvent extraction, ion exchange, flotation, biomass collection, and adsorption; however, none have been found to be suitable for reasons such as cost effectiveness, long term stability, and selectivity. Recent research has focused on the amidoxime functional group as a promising candidate for uranium sorption. Polymer beads and fibers have been functionalized with amidoxime functional groups, and uranium adsorption capacities as high as 1.5 g U/kg adsorbent have recently been reported with these types of materials. As uranium concentration in seawater is only ~3 ppb, great improvements to uranium collection systems must be made in order to make uranium extraction from seawater economically feasible. This proposed research intends to develop transformative technologies for economic uranium extraction from seawater. The Lin group will design advanced porous supports by taking advantage of recent breakthroughs in nanoscience and nanotechnology and incorporate high densities of well-designed chelators into such nanoporous supports to allow selective and efficient binding of uranyl ions from seawater. Several classes of nanoporous materials, including mesoporous silica nanoparticles (MSNs), mesoporous carbon nanoparticles (MCNs), meta-organic frameworks (MOFs), and covalent-organic frameworks (COFs), will be synthesized. Selective uranium-binding liagnds such as amidoxime will be incorporated into the nanoporous materials to afford a new generation of sorbent materials that will be

  16. DEVELOPMENT OF A CATALYST/SORBENT FOR METHANE REFORMING

    Energy Technology Data Exchange (ETDEWEB)

    B.H. Shanks; T.D. Wheelock; Justinus A. Satrio; Timothy Diehl; Brigitte Vollmer

    2004-09-27

    This work has led to the initial development of a very promising material that has the potential to greatly simplify hydrocarbon reforming for the production of hydrogen and to improve the overall efficiency and economics of the process. This material, which was derived from an advanced calcium-based sorbent, was composed of core-in-shell pellets such that each pellet consisted of a CaO core and an alumina-based shell. By incorporating a nickel catalyst in the shell, a combined catalyst and sorbent was prepared to facilitate the reaction of hydrocarbons with steam. It was shown that this material not only catalyzes the reactions of methane and propane with steam, it also absorbs CO{sub 2} simultaneously, and thereby separates the principal reaction products, H{sub 2} and CO{sub 2}. Furthermore, the absorption of CO{sub 2} permits the water gas shift reaction to proceed much further towards completion at temperatures where otherwise it would be limited severely by thermodynamic equilibrium. Therefore, an additional water gas shift reaction step would not be required to achieve low concentrations of CO. In a laboratory test of methane reforming at 600 C and 1 atm it was possible to produce a gaseous product containing 96 mole% H{sub 2} (dry basis) while also achieving a H{sub 2} yield of 95%. Methane reforming under these conditions without CO{sub 2} absorption provided a H{sub 2} concentration of 75 mole% and yield of 82%. Similar results were achieved in a test of propane reforming at 560 C and 1 atm which produced a product containing 96 mole% H{sub 2} while CO{sub 2} was being absorbed but which contained only 69 mole% H{sub 2} while CO{sub 2} was not being absorbed. These results were achieved with an improved catalyst support that was developed by replacing a portion of the {alpha}-alumina in the original shell material with {gamma}-alumina having a much greater surface area. This replacement had the unfortunate consequence of reducing the overall compressive

  17. Evaluation of Carbon Dioxide Capture From Existing Coal Fired Plants by Hybrid Sorption Using Solid Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Benson, Steven [Univ. of North Dakota, Grand Forks, ND (United States); Srinivasachar, Srivats [Envergex LLC, Sturbridge, MA (United States); Laudal, Daniel [Univ. of North Dakota, Grand Forks, ND (United States); Browers, Bruce [Barr Engineering, Minneapolis, MN (United States)

    2014-12-31

    A novel hybrid solid sorbent technology for CO₂ capture and separation from coal combustion-derived flue gas was evaluated. The technology – Capture of CO₂ by Hybrid Sorption (CACHYS™) – is a solid sorbent technology based on the following ideas: 1) reduction of energy for sorbent regeneration, 2) utilization of novel process chemistry, 3) contactor conditions that minimize sorbent-CO₂ heat of reaction and promote fast CO₂ capture, and 4) low-cost method of heat management. This report provides key information developed during the course of the project that includes sorbent performance, energy for sorbent regeneration, physical properties of the sorbent, the integration of process components, sizing of equipment, and overall capital and operational cost of the integrated CACHYS™ system. Seven sorbent formulations were prepared and evaluated at the lab-scale for energy requirements and CO₂ capture performance. Sorbent heat of regeneration ranged from 30-80 kJ/mol CO₂ and was found to be dependent on process conditions. Two sorbent formulations (designated HCK-4 & HCK-7) were down-selected for additional fixed-bed testing. Additional testing involved subjecting the sorbents to 100 continuous cycles in the fixed-bed reactor to determine performance as a function of time. The working capacity achieved for HCK-4 sorbent ranged from 5.5-8.0 g CO₂/100 g sorbent, while the HCK-7 typically ranged from 8.0-10.0 g CO₂/100 g sorbent. Overall, there was no deterioration in capacity with continuous cycling for either sorbent. The CACHYS™ bench-scale testing system designed and fabricated under this award consists of a dual circulating fluidized-bed adsorber and a moving-bed regenerator. The system takes a flue gas slipstream from the University of North Dakota’s coal-fired steam plant. Prior to being sent to the adsorber, the flue gas is scrubbed to remove SO₂ and particulate. During parametric testing of the adsorber, CO₂ capture achieved using

  18. Effective Uranium (VI) Sorption from Alkaline Solutions Using Bi-Functionalized Silica-Coated Magnetic Nanoparticles

    International Nuclear Information System (INIS)

    Chen, X.; He, L.; Liu, B.; Tang, Y.

    2015-01-01

    High temperature gas reactor is one of generation IV reactors that can adapt the future energy market, of which the preparation of fuel elements will produce a large amount of radioactive wastewater with uranium and high-level ammonia. Sorption treatment is one of the most important method to recover uranium from wastewater. However, there are few report on uranium sorbent that can directly be applied in wastewater with ammonia. Therefore, the development of a sorbent that can recover uranium in basic environment will greatly decrease the cost of fuel element production and the risk of radioactive pollution. In this work, ammonium-phosphonate-bifunctionalized silica-coated magnetic nanoparticles has been developed for effective sorption of uranium from alkaline media, which are not only advantaged in the uranium separation from liquid phase, but also with satisfactory adsorption rate, amount and reusability. The as-prepared sorbent is found to show a maximum uranium sorption capacity of 70.7 mg/g and a fast equilibrium time of 2 h at pH 9.5 under room temperature. Compared with the mono-functionalized (phosphonate alone and ammonium alone) particles, the combination of the bi-functionalized groups gives rise to an excellent ability to remove uranium from basic environment. The sorbent can be used as a promising solid phase candidate for highly-efficient removal of uranium from basic solution. (author)

  19. Validation of SPME-GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects.

    Science.gov (United States)

    Romero, I; García-González, D L; Aparicio-Ruiz, R; Morales, M T

    2015-03-01

    Volatile compounds are responsible for the aroma of virgin olive oil and also for its quality. The high number and different nature of volatile compounds drive to the need of a reliable analytical method that allows their proper quantification to explain the standard method of panel test. Although there are some analytical solutions available, they have not been validated and the regulatory bodies are reluctant to adopt them since they can be subjected to unknown errors. In this regards, the European Union has encouraged the validation of these analytical tools through the research program Horizon2020, which involves gaining knowledge from the analytical properties of the chemical methods for sensory assessment. This work is focused on the analytical validation of the methodology used to determine the actual concentration of volatiles in virgin olive oils when applying SPME-GCMS. The validation process includes the calibration curves for 29 volatile compounds responsible for the most common sensory perceptions in virgin olive oils, the determination of their working ranges with linear response, the detection and quantification limits, the sensitivity, the accuracy estimated as trueness and precision and the selectivity. Sixty-seven percent of the compounds presented a relative standard deviation in repeatability lower than 10%, and this percentage rises to 95% in lampante virgin olive oils. The accuracy was established in 97% of the studied volatile compounds. Finally, an empirical example of the ability of the method to discriminate virgin olive oils of different categories (extra virgin, virgin, ordinary and lampante) by the quantification of their volatiles is provided. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Volatiles and primary metabolites profiling in two Hibiscus sabdariffa (roselle) cultivars via headspace SPME-GC-MS and chemometrics.

    Science.gov (United States)

    Farag, Mohamed A; Rasheed, Dalia M; Kamal, Islam M

    2015-12-01

    Hibiscus sabdariffa (roselle) is a plant of considerable commercial importance worldwide as functional food due to its organic acids, mucilage, anthocyanins, macro and micro-nutrients content. Although Hibiscus flowers are emerging as very competitive targets for phytochemical studies, very little is known about their volatile composition and or aroma, such knowledge can be suspected to be relevant for understanding its olfactory and taste properties. To provide insight into Hibiscus flower aroma composition and for its future use in food and or pharmaceutical industry, volatile constituents from 2 cultivars grown in Egypt, viz. Aswan and Sudan-1 were profiled using solid-phase microextraction (SPME) coupled to GCMS. A total of 104 volatiles were identified with sugar and fatty acid derived volatiles amounting for the major volatile classes. To reveal for cultivar effect on volatile composition in an untargeted manner, multivariate data analysis was applied. Orthogonal projection to latent structures-discriminant analysis (OPLS-DA) revealed for 1-octen-3-ol versus furfural/acetic acid enrichment in Aswan and Sudan-1 cvs., respectively. Primary metabolites contributing to roselle taste and nutritional value viz. sugars and organic acids were profiled using GC-MS after silylation. The impact of probiotic bacteria on roselle infusion aroma profile was further assessed and revealed for the increase in furfural production with Lactobacillus plantarum inoculation and without affecting its anthocyanin content. This study provides the most complete map for volatiles, sugars and organic acids distribution in two Hibiscus flower cultivars and its fermented product. Copyright © 2015 Elsevier Ltd. All rights reserved.

  1. Usefulness of a PARAFAC decomposition in the fiber selection procedure to determine chlorophenols by means SPME-GC-MS.

    Science.gov (United States)

    Morales, Rocío; Cruz Ortiz, M; Sarabia, Luis A

    2012-05-01

    In this work, a procedure based on solid-phase microextraction and gas chromatography coupled with mass spectrometry is proposed to determine chlorophenols in water without derivatization. The following chlorophenols are studied: 2,4-dichlorophenol; 2,4,6-trichlorophenol; 2,3,4,6-tetrachlorophenol and pentachlorophenol. Three kinds of SPME fibers, polyacrylate, polydimethylsiloxane, and polydimethylsiloxane/divinylbenzene are compared to identify the most suitable one for the extraction process on the basis of two criteria: (a) to select the equilibrium time studying the kinetics of the extraction, and (b) to obtain the best values of the figures of merit. In both cases, a three-way PARAllel FACtor analysis decomposition is used. For the first step, the three-way experimental data are arranged as follows: if I extraction times are considered, the tensor of data, X, of dimensions I × J × K is generated by concatenating the I matrices formed by the abundances of the J m/z ions recorded in K elution times around the retention time for each chlorophenol. The second-order property of PARAFAC (or PARAFAC2) assesses the unequivocal identification of each chlorophenol, as consequence, the loadings in the first mode estimated by the PARAFAC decomposition are the kinetic profile. For the second step, a calibration based on a PARAFAC decomposition is used for each fiber. The best figures of merit were obtained with PDMS/DVB fiber. The values of decision limit, CCα, achieved are between 0.29 and 0.67 μg L(-1) for the four chlorophenols. The accuracy (trueness and precision) of the procedure was assessed. This procedure has been applied to river water samples.

  2. Preparation and evaluation of graphene-coated solid-phase microextraction fiber

    Energy Technology Data Exchange (ETDEWEB)

    Chen Jinmei; Zou Jing; Zeng Jingbin; Song Xinhong; Ji Jiaojiao; Wang Yiru [Department of Chemistry and the Key Laboratory of Analytical Sciences of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005 (China); Ha, Jaeho [Food Analysis Center, Korea Food Research Institute, San 46-1, Baekhyun, Bundang, Seongnam, Gyonggi Province 463-746 (Korea, Republic of); Chen Xi, E-mail: xichen@xmu.edu.cn [Department of Chemistry and the Key Laboratory of Analytical Sciences of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005 (China); State Key Laboratory of Marine Environmental Science, Xiamen University, Xiamen 361005 (China)

    2010-09-23

    In this paper, a novel graphene (G) based solid-phase microextraction (SPME) fiber was firstly prepared by immobilizing the synthesized G on stainless steel wire as coating. The new fiber possessed a homogeneous, porous and wrinkled surface and showed excellent thermal (over 330 {sup o}C), chemical and mechanical stability, and long lifespan (over 250 extractions). The SPME performance of the G-coated fiber was evaluated in detail through extraction of six pyrethroid pesticides. Although the thickness of G-coated fiber was only 6-8 {mu}m, its extraction efficiencies were higher than those of two commercial fibers (PDMS, 100 {mu}m; PDMS/DVB, 65 {mu}m). This high extraction efficiency may be mainly attributed to huge delocalized {pi}-electron system of G, which shows strong {pi}-stacking interaction with pyrethroid pesticide. The G-coated fiber was applied in the gas chromatographic determination of six pyrethroids, and their limits of detection were found to be ranged from 3.69 to 69.4 ng L{sup -1}. The reproducibility for each single fiber was evaluated and the relative standard deviations (RSDs) were calculated to be in the range from 1.9% to 6.5%. The repeatability of fiber-to-fiber and batch-to-batch was 4.3-9.2% and 4.1-9.9%. The method developed was successfully applied to three pond water samples, and the recoveries were 83-110% at a spiking of 1 {mu}g L{sup -1}.

  3. Kinetics of Mn-based sorbents for hot coal gas desulfurization. Quarterly progress report, July 15, 1995--September 15, 1995

    Energy Technology Data Exchange (ETDEWEB)

    Hepworth, M.T.

    1995-09-15

    The Morgantown Energy Technology Center (METC) of the U.S. Department of Energy (DOE) is actively pursuing the development of reliable and cost-effective processes to clean coal gasifier gases for application to integrated gasification combined cycle (IGCC) and molten carbonate fuel cell (MCFC) power plants. A large portion of gas cleanup research has been directed towards hot gas desulfurization using Zn-based sorbents. However, zinc titinate sorbents undergo reduction to the metal at temperatures approaching 700{degrees}C. In addition, sulfate formation during regeneration leads to spalling of reactive 293 surfaces. Due to zinc-based sorbent performance, METC has shown interest in formulating and testing manganese-based sorbents. Westmoreland and Harrison evaluated numerous candidate sulfur sorbents and identified Mn as a good candidate. Later, Turkdogan and Olsson tested manganese-based sorbents which demonstrated superior desulfurization capacity under high temperatures, and reducing conditions. Recently, Ben-Slimane and Hepworth conducted several studies on formulating Mn-sorbents and desulfurizing a simulated fuel gas. Although thermodynamics predicts higher over-pressures with Mn verses Zn, under certain operating conditions Mn-based sorbents may obtain < 20 ppmv. In addition, the manganese-sulfur-oxygen (Mn-S-O) system does not reduce to the metal under even highly reducing gases at high temperatures (550-900{degrees}C). Currently, many proposed IGCC processes include a water quench prior to desulfurization. This is for two reasons; limitations in the process hardware (1000{degrees}C), and excessive Zn-based sorbent loss (about 700{degrees}C). With manganese the water quench is obviated due to sorbent loss, as Mn-based sorbents have been shown to retain reactivity under cycling testing at 900{degrees}C. This reduces system hardware, and increases thermal efficiency while decreasing the equilibrium H{sub 2}S over-pressure obtainable with a manganese sorbent.

  4. Efficient separations and processing crosscutting program: Develop and test sorbents

    International Nuclear Information System (INIS)

    Bray, L.A.

    1995-09-01

    This report summarizes work performed during FY 1995 under the task open-quotes Develop and Test Sorbents,close quotes the purpose of which is to develop high-capacity, selective solid extractants to recover cesium, strontium, and technetium from nuclear wastes. This work is being done for the Efficient Separations and Processing Crosscutting Program (ESP), operated by the U.S. Department of Energy's Office of Environmental Management's Office of Technology Development. The task is under the direction of staff at Pacific Northwest Laboratory (PNL) with key participation from industrial and university staff at 3M, St. Paul, Minnesota; IBC Advanced Technologies, Inc., American Forks, Utah; AlliedSignal, Inc., Des Plaines, Illinois, and Texas A ampersand M University, College Station, Texas. 3M and IBC are responsible for ligand and membrane technology development; AlliedSignal and Texas A ampersand M are developing sodium titanate powders; and PNL is testing the materials developed by the industry/university team members. Major accomplishments for FY 1995 are summarized in this report

  5. Polyacrylonitrile-chalcogel hybrid sorbents for radioiodine capture.

    Science.gov (United States)

    Riley, Brian J; Pierce, David A; Chun, Jaehun; Matyáš, Josef; Lepry, William C; Garn, Troy G; Law, Jack D; Kanatzidis, Mercouri G

    2014-05-20

    Powders of a Sn2S3 chalcogen-based aerogel (chalcogel) were combined with powdered polyacrylonitrile (PAN) in different mass ratios (SnS33, SnS50, and SnS70; # = mass% of chalcogel), dissolved in dimethyl sulfoxide, and added dropwise to deionized water to form pellets of a porous PAN-chalcogel hybrid material. These pellets, along with pure powdered (SnSp) and granular (SnSg) forms of the chalcogel, were then used to capture iodine gas under both dynamic (dilute) and static (concentrated) conditions. Both SnSp and SnSg chalcogels showed very high iodine loadings at 67.2 and 68.3 mass%, respectively. The SnS50 hybrid sorbent demonstrated a high, although slightly reduced, maximum iodine loading (53.5 mass%) with greatly improved mechanical rigidity. In all cases, X-ray diffraction results showed the formation of crystalline SnI4 and SnI4(S8)2, revealing that the iodine binding in these materials is mainly due to a chemisorption process, although a small amount of physisorption was observed.

  6. Efficient separations and processing crosscutting program: Develop and test sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Bray, L.A.

    1995-09-01

    This report summarizes work performed during FY 1995 under the task {open_quotes}Develop and Test Sorbents,{close_quotes} the purpose of which is to develop high-capacity, selective solid extractants to recover cesium, strontium, and technetium from nuclear wastes. This work is being done for the Efficient Separations and Processing Crosscutting Program (ESP), operated by the U.S. Department of Energy`s Office of Environmental Management`s Office of Technology Development. The task is under the direction of staff at Pacific Northwest Laboratory (PNL) with key participation from industrial and university staff at 3M, St. Paul, Minnesota; IBC Advanced Technologies, Inc., American Forks, Utah; AlliedSignal, Inc., Des Plaines, Illinois, and Texas A&M University, College Station, Texas. 3M and IBC are responsible for ligand and membrane technology development; AlliedSignal and Texas A&M are developing sodium titanate powders; and PNL is testing the materials developed by the industry/university team members. Major accomplishments for FY 1995 are summarized in this report.

  7. Modeling and analysis of circulation variables of continuous sorbent loop cycling for CO{sub 2} capture

    Energy Technology Data Exchange (ETDEWEB)

    Yoo, Kee-Youn [Seoul National University of Science and Technology, Seoul (Korea, Republic of); Park, Jun-Soo; Park, Myung-June [Ajou University, Suwon (Korea, Republic of)

    2016-04-15

    Carbon capture and storage (CCS) technologies are a cornerstone for reducing CO{sub 2} emissions from energy and energy-intensive industries. Among the various CCS technologies, solid sorbent looping systems are considered to be potentially promising solutions for reducing CO{sub 2} capture energy penalty. We present an evaluation module for a carbonator with sorbent looping cycle to calculate the carbonation efficiency. The module incorporates a simple sorbent activity model, and the solid/gas balances are constructed by assuming simple reactor mixing quality. By conducting simulations, we examine the variation in the carbonation efficiencies as a function of the sorbent looping operation factors and discuss an optimum operating strategy.

  8. Adsorption Equilibrium for Heavy Metal Divalent Ions (Cu2+, Zn2+, and Cd2+) into Zirconium-Based Ferromagnetic Sorbent

    OpenAIRE

    Agnes Yung Weng Lee; Soh Fong Lim; S. N. David Chua; Khairuddin Sanaullah; Rubiyah Baini; Mohammad Omar Abdullah

    2017-01-01

    Zirconium-based ferromagnetic sorbent was fabricated by coprecipitation of Fe2+/Fe3+ salts in a zirconium solution and explored as a potential sorbent for removing the Cu2+, Zn2+, and Cd2+ from aqueous solution. The sorbent could easily be separated from aqueous solution under the influence of external magnetic field due to the ferromagnetism property. A trimodal distribution was obtained for the sorbent with average particle size of 22.74 μm. The –OH functional groups played an important rol...

  9. Nanofiber polymers as novel sorbents for on-line solid phase extraction in chromatographic system: A comparison with monolithic reversed phase C18 sorbent.

    Science.gov (United States)

    Háková, Martina; Havlíková, Lucie Chocholoušová; Chvojka, Jiří; Švec, František; Solich, Petr; Šatínský, Dalibor

    2018-08-14

    A novel application of nanofiber polymers in the wide area of a sample preparation techniques known as solid phase extraction has been studied. We demonstrated application of nanofibers as sorbents for use in a system including on-line extraction coupled with column-switching high performance liquid chromatography. Four types of nanofibers including polyamide 6 with two different surface densities, poly(ε-caprolactone), and polystyrene were tested. We found that three of them were very efficient extraction sorbents sufficiently stable for application in the on-line system. Our results confirmed that the extraction efficiency of the nanofibers depended on the type and chemistry of the spun polymer as well as on the fabrication process of the nanofibrous mats that affected their density, structure, surface density, and mechanical functionality. We also compared performance of all four nanofibers with a conventional monolithic reversed-phase C18 sorbent in terms of extraction efficiency using on-line solid-phase extraction-HPLC system. Polyamide 6 was found to be the best sorbent for lipophilic analytes with a retention and extraction efficiency for the target analytes comparable with that of the C18 monolith. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. The use of a polymer inclusion membrane as a sorbent for online preconcentration in the flow injection determination of thiocyanate impurity in ammonium sulfate fertilizer.

    Science.gov (United States)

    Ohshima, Takumi; Kagaya, Shigehiro; Gemmei-Ide, Makoto; Cattrall, Robert W; Kolev, Spas D

    2014-11-01

    A polymer inclusion membrane (PIM) is used for the first time as a sorbent in the construction of a preconcentration column to enhance the sensitivity in flow injection analysis (FIA). The PIM-coated column is readily prepared by coating the PIM containing poly(vinyl chloride), Aliquat 336, and 1-tetradecanol onto glass beads packed in a glass tube. The determination of trace amounts of thiocyanate in ammonium sulfate fertilizer demonstrates the potential of the proposed PIM-coated column in FIA. Thiocyanate standards or samples of relatively large volume (e.g. up to 2000 µL) are injected into a nitrate carrier stream. The sample zone passes through the proposed preconcentration column where thiocyanate is concentrated in a smaller volume of a carrier solution thus resulting in up to 7.4 fold increase in sensitivity. Thiocyanate is detected spectrophotometrically after its reaction with Fe(III) downstream of the preconcentration column. The limits of detection of thiocyanate in the absence and presence of 20 g L(-1) ammonium sulfate (S/N=2) are 0.014 and 0.024 mg L(-1), respectively. Thiocyanate was successfully determined in several samples of ammonium sulfate fertilizer. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. CNTs reinforced super-hydrophobic-oleophilic electrospun polystyrene oil sorbent for enhanced sorption capacity and reusability

    KAUST Repository

    Wu, Jingya

    2016-12-05

    To meet the challenges of global oil spills and oil-water contamination, the development of a low-cost and reusable sorbents with good hydrophobicity and oleophilic nature is crucial. In this study, functionalized carbon nanotubes (CNTs) were wrapped in polystyrene (PS) polymer (PS-CNTs) and electrospun to create an effective and rigid sorbent for oil. Covalent modification and fluorination of CNTs improved their dispersibility and interfacial interaction with the polymer, resulting in a well-aligned CNTs configuration inside the porous fiber structure. Interestingly, the oil sorption process using PS-CNTs was observed to have two phases. First, the oil swiftly entered the membrane pores formed by interconnected nanofibers due to oleophilic properties of the micro-sized void. In the second phase, the oil not only moved to nano interior spaces of the fibers by capillary forces but also adsorbed on the surface of fibers where the latter was retained due to Van der Waals force. The sorption process fits well with the intra particle diffusion model. Maximum oil sorption capacity of the PS-CNTs sorbent for sunflower oil, peanut oil, and motor oils were 116, 123, and 112 g/g, respectively, which was 65% higher than that of the PS sorbent without CNTs. Overall, a significant increase in the porosity, surface area, water contact angle, and oleophilic nature was observed for the PS-CNTs composite sorbents. Not only did the PS-CNTs sorbents exhibited a promising oil sorption capacity but also showed potential for reusability, which is an important factor to be considered in determining the overall performance of the sorbent and its environmental impacts.

  12. Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

    Science.gov (United States)

    Tran, MinhPhuong; Turner, Erica B; Segro, Scott S; Fang, Li; Seyyal, Emre; Malik, Abdul

    2017-11-03

    A sol-gel organic-inorganic hybrid sorbent, consisting of chemically integrated tantalum (V) ethoxide (TaEO) and polypropylene glycol methacrylate (PPGM), was developed for capillary microextraction (CME). The sol-gel sorbent was synthesized within a fused silica capillary through hydrolytic polycondensation of TaEO and chemical incorporation of PPGM into the evolving sol-gel tantala network. A part of the organic-inorganic hybrid sol-gel network evolving in the vicinity of the capillary walls had favorable conditions to get chemically bonded to the silanol groups on the capillary surface forming a surface-bonded coating. The newly developed sol-gel sorbent was employed to isolate and enrich a variety of analytes from aqueous samples for on-line analysis by high-performance liquid chromatography (HPLC) equipped with a UV detector. CME was performed on aqueous samples containing trace concentrations of analytes representing polycyclic aromatic hydrocarbons, ketones, alcohols, amines, nucleosides, and nucleotides. This sol-gel hybrid coating provided efficient extraction with CME-HPLC detection limits ranging from 4.41pM to 28.19 pM. Due to direct chemical bonding between the sol-gel sorbent coating and the fused silica capillary inner surface, this sol-gel sorbent exhibited enhanced solvent stability. The sol-gel tantala-based sorbent also exhibited excellent pH stability over a wide pH range (pH 0-pH 14). Furthermore, it displayed great performance reproducibility in CME-HPLC providing run-to-run HPLC peak area relative standard deviation (RSD) values between 0.23% and 3.83%. The capillary-to-capillary RSD (n=3), characterizing capillary preparation method reproducibility, ranged from 0.24% to 4.11%. The results show great performance consistency and application potential for the sol-gel tantala-PPGM sorbent in various fields including biomedical, pharmaceutical, and environmental areas. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Coating materials

    International Nuclear Information System (INIS)

    Ozeki, Takao; Kimura, Tadashi; Kobayashi, Juichi; Maeda, Yutaka; Nakamoto, Hideo.

    1969-01-01

    A non-solvent type coating material composition having properties as good as thermosetting acrylic or amino alkid resins is provided by employing active energy irradiation, particularly electron beams, using a radically polymerizable low molecular compound (A) (hereafter called an oligomer) containing at least two vinyl radicals in one molecule. This oligomer is produced by reacting an epoxy-containing vinyl monomer with alpha-, beta-ethylene unsaturated carboxylic acids or their anhydrides. The composition (I) contains 10% - 100% of this oligomer. In embodiments, an oligomer having a fiberous trivinyl construction is produced by reacting 180 parts by weight of glycidyl methacrylate ester with 130 parts of itaconic acid in the presence of a polymerization-inhibitor and an addition reaction catalyst at 90 0 C for 6 hours. In practice, the coating material compositions (1), consist of the whole oligomer [I-1]; (2), consist of 10-90% of (A) component and 90%-10% of vinyl monomers containing at least 30% (meth) acrylic monomer [I-2]; (3), 10%-90% of component (A) and 90%-10% of other monomers containing at least two vinyl radicals [I-3]; (4), a mixture of (I-2) and (I-3), [I-4]; and (5), consist of 50% or less unsaturated polyester of 500-5,000 molecular weight range or drying oil, or alkyd resin of 500-5,000 molecular weight range modified by drying oil, [I-5]. As a catalyst a tertiary amino vinyl compound is preferred. Five examples are given. (Iwakiri, K.)

  14. Optimization of total vaporization solid-phase microextraction (TV-SPME) for the determination of lipid profiles of Phormia regina, a forensically important blow fly species.

    Science.gov (United States)

    Kranz, William; Carroll, Clinton; Dixon, Darren; Picard, Christine; Goodpaster, John

    2017-11-01

    A new method has been developed for the determination of fatty acids, sterols, and other lipids which naturally occur within pupae of the blow fly Phormia regina. The method relies upon liquid extraction in non-polar solvent, followed by derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) w/ 1% trimethylchlorsilane (TMCS) carried out inside the sample vial. The analysis is facilitated by total vaporization solid-phase microextraction (TV-SPME), with gas chromatography-mass spectrometry (GC-MS) serving as the instrumentation for analysis. The TV-SPME delivery technique is approximately a factor of five more sensitive than traditional liquid injection, which may alleviate the need for rotary evaporation, reconstitution, collection of high performance liquid chromatography fractions, and many of the other pre-concentration steps that are commonplace in the current literature. Furthermore, the ability to derivatize the liquid extract in a single easy step while increasing sensitivity represents an improvement over current derivatization methods. The most common lipids identified in fly pupae were various saturated and unsaturated fatty acids ranging from lauric acid (12:0) to arachinoic acid (20:4), as well as cholesterol. The concentrations of myristic acid (14:0), palmitelaidic acid (16:2), and palmitoleic acid (16:1) were the most reliable indicators of the age of the pupae. Graphical abstract Blow fly pupae were extracted prior to emerging as adults. The extracts were analyzed via total vaporization solid-phase microextraction (TV-SPME), revealing a complex mixture of lipids that could be associated with the age of the insect. This information may assist in determining a post-mortum interval (PMI) in a death investigation.

  15. Cannabinoids determination in oral fluid by SPME-GC/MS and UHPLC-MS/MS and its application on suspected drivers.

    Science.gov (United States)

    Anzillotti, Luca; Castrignanò, Erika; Strano Rossi, Sabina; Chiarotti, Marcello

    2014-12-01

    The confirmation of Δ9-tetrahydrocannabinol (THC) in oral fluid (OF) is an important issue for assessing Driving Under the Influence of Drugs (DUID). The aim of this research was to develop a highly sensitive method with minimal sample pre-treatment suitable for the analysis of small OF volumes (100 μL) for the confirmation of cannabinoids in DUID cases. Two methods were compared for the confirmation of THC in residual OF samples, obtained from a preliminary on-site screening with commercial devices. An ultra high performance LC-MS (UHPLC-MS/MS) method and an SPME-GC/MS method were hence developed. 100 μL of the residual mixture OF/preservative buffer or neat OF was simply added to 10 μL of THC-D3 (1 μg/mL) and submitted to the two different analyses: A - direct injection of 10 μL in UHPLC-MS/MS in positive electrospray ionisation (ESI) mode and B - sampling for 30 min with SPME (100 μm polydimethylsiloxane or PDMS fibre) and direct injection by desorption of the fibre in the GC injection port. The lowest limit of detection (LLOD) of THC was 2 ng/mL in UHPLC-MS/MS and 0.5 ng/mL in SPME-GC/MS. In addition, cannabidiol (CBD) and cannabinol (CBN) could be detected in GC/MS equipment at 2 ng/mL, whilst in UHPLC-MS/MS the LLOD was 20 ng/mL. Both methods were applied to 70 samples coming from roadside tests. By SPME-GC/MS analysis, THC was confirmed in 42 samples, whilst CBD was detected in 21 of them, along with CBN in 14 samples. THC concentrations ranged from traces below the lowest limit of quantification or LLOQ (2 ng/mL) up to 690 ng/mL. Copyright © 2014 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  16. SOLID PHASE MICRO EXTRACTION (SPME) FLAVOR ANALYSIS OF APPLE JUICE AND COFFEE MIXTURES USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY (GC-MS)

    OpenAIRE

    Mi Ja Kim; Jeehyun Lee; Jaeyoung Byun; Sunmi Choi; Wonsik Choi

    2016-01-01

    This research was conducted to evaluate the flavor of apple juice and coffee mixtures and the sensory quality of SPME extracts using gas chromatography-mass spectrometry (GC-MS). Three samples with different compositions were examined. Sample A1 contained85% apple juiceand 15% coffee, sample A2 had87.5% apple and 12.5% coffee, and sample A3 had90% apple juiceand 10% coffee. The sensory analysis involved 100 panelists and a sequential monadic test. Sample presentation orders were balanced in ...

  17. Predicting sorption of organic acids to a wide range of carbonized sorbents

    Science.gov (United States)

    Sigmund, Gabriel; Kah, Melanie; Sun, Huichao; Hofmann, Thilo

    2016-04-01

    Many contaminants and infochemicals are organic acids that undergo dissociation under environmental conditions. The sorption of dissociated anions to biochar and other carbonized sorbents is typically lower than that of neutral species. It is driven by complex processes that are not yet fully understood. It is known that predictive approaches developed for neutral compounds are unlikely to be suitable for organic acids, due to the effects of dissociation on sorption. Previous studies on the sorption of organic acids to soils have demonstrated that log Dow, which describes the decrease in hydrophobicity of acids upon dissociation, is a useful alternative to log Kow. The aim of the present study was to adapt a log Dow based approach to describe the sorption of organic acids to carbonized sorbents. Batch experiments were performed with a series of 9 sorbents (i.e., carbonized wood shavings, pig manure, and sewage sludge, carbon nanotubes and activated carbon), and four acids commonly used for pesticidal and biocidal purposes (i.e., 2,4-D, MCPA, 2,4-DB, and triclosan). Sorbents were comprehensively characterized, including by N2 and CO2 physisorption, Fourier transform infrared spectroscopy, and elemental analysis. The wide range of sorbents considered allows (i) discussing the mechanisms driving the sorption of neutral and anionic species to biochar, and (ii) their dependency on sorbate and sorbent properties. Results showed that the sorption of the four acids was influenced by factors that are usually not considered for neutral compounds (i.e., pH, ionic strength). Dissociation affected the sorption of the four compounds, and sorption of the anions ranged over five orders of magnitude, thus substantially contributing to sorption in some cases. For prediction purposes, most of the variation in sorption to carbonized sorbents (89%) could be well described with a two-parameter regression equation including log Dow and sorbent specific surface area. The proposed model

  18. Extended evaluation of polymeric and lipophilic sorbents for passive sampling of marine toxins.

    Science.gov (United States)

    Zendong, Zita; Herrenknecht, Christine; Abadie, Eric; Brissard, Charline; Tixier, Céline; Mondeguer, Florence; Séchet, Véronique; Amzil, Zouher; Hess, Philipp

    2014-12-01

    Marine biotoxins are algal metabolites that can accumulate in fish or shellfish and render these foodstuffs unfit for human consumption. These toxins, released into seawater during algal occurrences, can be monitored through passive sampling. Acetone, methanol and isopropanol were evaluated for their efficiency in extracting toxins from algal biomass. Isopropanol was chosen for further experiments thanks to a slightly higher recovery and no artifact formation. Comparison of Oasis HLB, Strata-X, BondElut C18 and HP-20 sorbent materials in SPE-mode led to the choice of Oasis HLB, HP-20 and Strata-X. These three sorbents were separately exposed as passive samplers for 24 h to seawater spiked with algal extracts containing known amounts of okadaic acid (OA), azaspiracids (AZAs), pinnatoxin-G (PnTX-G), 13-desmethyl spirolide-C (SPX1) and palytoxins (PlTXs). Low density polyethylene (LDPE) and silicone rubber (PDMS) strips were tested in parallel on similar mixtures of spiked natural seawater for 24 h. These strips gave significantly lower recoveries than the polymeric sorbents. Irrespective of the toxin group, the adsorption rate of toxins on HP-20 was slower than on Oasis HLB and Strata-X. However, HP-20 and Strata-X gave somewhat higher recoveries after 24 h exposure. Irrespective of the sorbent tested, recoveries were generally highest for cyclic imines and OA group toxins, slightly lower for AZAs, and the lowest for palytoxins. Trials in re-circulated closed tanks with mussels exposed to Vulcanodinium rugosum or Prorocentrum lima allowed for further evaluation of passive samplers. In these experiments with different sorbent materials competing for toxins in the same container, Strata-X accumulated toxins faster than Oasis HLB, and HP-20, and to higher levels. The deployment of these three sorbents at Ingril French Mediterranean lagoon to detect PnTX-G in the water column showed accumulation of higher levels on HP-20 and Oasis HLB compared to Strata-X. This study

  19. Coatings and Corrosion Laboratory

    Data.gov (United States)

    Federal Laboratory Consortium — Purpose: The mission of the Coatings and Corrosion Laboratory is to develop and analyze the effectiveness of innovative coatings test procedures while evaluating the...

  20. Preparation and characterization of polymer coated partially esterified sugarcane bagasse for separation of oil from seawater.

    Science.gov (United States)

    Abdelwahab, N A; Shukry, N; El-Kalyoubi, S F

    2017-08-01

    Sugarcane bagasse (B), a low-cost agricultural waste, was modified via esterification and coating with polyacrylonitrile (PAN) and evaluated as a hydrophobic sorbent for diesel oil removal from artificial seawater. Esterification was carried out using stearic acid (SA) and CaO, the reaction conditions, including B:SA mass ratio, CaO concentration, reaction time and temperature were optimized. Additional hydrophobicity was achieved by coating the esterified bagasse (EB) with a hydrophobic polymer (PAN). The advantages of hydrophobicity were clearly expressed by decreased water absorption capacity and increased oil adsorption capacity. The presence of hydrophobic groups was evidenced through Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM) measurements. FTIR spectroscopy showed some changes in the spectrum of B. XRD patterns indicated that the crystalline structure of B turned amorphous. SEM micrographs illustrated that the surface of EB roughened and PAN was unevenly deposited on it, which led to an increase in the surface area of both sorbents. Moreover, efficient desorption and resorption of diesel oil, paraffin oil, gasoline oil and vegetable oil were recorded in six cycles. Generally, the results are promising and the prepared sorbents can positively contribute to environmental remediation.

  1. Regenerable sorbents for mercury capture in simulated coal combustion flue gas.

    Science.gov (United States)

    Rodríguez-Pérez, Jorge; López-Antón, M Antonia; Díaz-Somoano, Mercedes; García, Roberto; Martínez-Tarazona, M Rosa

    2013-09-15

    This work demonstrates that regenerable sorbents containing nano-particles of gold dispersed on an activated carbon are efficient and long-life materials for capturing mercury species from coal combustion flue gases. These sorbents can be used in such a way that the high investment entailed in their preparation will be compensated for by the recovery of all valuable materials. The characteristics of the support and dispersion of gold in the carbon surface influence the efficiency and lifetime of the sorbents. The main factor that determines the retention of mercury and the regeneration of the sorbent is the presence of reactive gases that enhance mercury retention capacity. The capture of mercury is a consequence of two mechanisms: (i) the retention of elemental mercury by amalgamation with gold and (ii) the retention of oxidized mercury on the activated carbon support. These sorbents were specifically designed for retaining the mercury remaining in gas phase after the desulfurization units in coal power plants. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Hot coal gas desulfurization with manganese-based sorbents. Final report, September 1992--December 1994

    Energy Technology Data Exchange (ETDEWEB)

    Hepworth, M.T.; Slimane, R.B.

    1994-11-01

    The focus of much current work being performed by the Morgantown Energy Technology Center (METC) of the Department of Energy on hot coal-derived fuel gas desulfurization is in the use of zinc-based sorbents. METC has shown interest in formulating and testing manganese-based pellets as alternative effective sulfur sorbents in the 700 to 1200{degree}C temperature range. To substantiate the potential superiority of Mn-based pellets, a systematic approach toward the evaluation of the desulfurizing power of single-metal sorbents is developed based on thermodynamic considerations. This novel procedure considered several metal-based sorbents and singled out manganese oxide as a prime candidate sorbent capable of being utilized under a wide temperature range, irrespective of the reducing power (determined by CO{sub 2}/CO ratio) of the fuel gas. Then, the thermodynamic feasibility of using Mn-based pellets for the removal of H{sub 2}S from hot-coal derived fuel gases, and the subsequent oxidative regeneration of loaded (sulfided) pellets was established. It was concluded that MnO is the stable form of manganese for virtually all commercially available coal-derived fuel gases. In addition, the objective of reducing the H{sub 2}S concentration below 150 ppMv to satisfy the integrated gasification combined cycle system requirement was shown to be thermodynamically feasible. A novel process is developed for the manufacture of Mn-based spherical pellets which have the desired physical and chemical characteristics required.

  3. Bioaffinity sorbent based on immobilized protein A Staphylococcus aureus: development and application

    Directory of Open Access Journals (Sweden)

    Kordium V. A.

    2012-04-01

    Full Text Available Aim. The obtaining of bioaffinity sorbent based on the immobilized protein A of S. aureus (SPA using two cellulose-binding domains (CBD, and its application for purification of antibodies. Methods. The DNA sequences encoding SPA and two CBD were genetically fused, expressed in the high-productive Escherichia coli system and the protein SPA-CBD2 was obtained in a soluble form. The SPA-CBD2 fusion protein was affinity immobilized on the microcrystalline cellulose. Results. Capacity of bioaffinity sorbent (1 mg SPA-CBD2/1 ml CC31-cellulose, dynamic capacity (3 mg mouse IgG/1 ml bioaffinity sorbent, efficiency and stability during prolonged storage were determined. The bioffinity sorbent was used for purification of antibodies. The purity of antibodies in eluted fractions was more than 95 %. The purified antibodies detected target antigens with a high sensitivity. Conclusions. The designed bioaffinity sorbent provides obtaining pure poly- and monoclonal antibodies in functionally active form and can be useful for the fractionation of mouse immunoglobulin G.

  4. Waste Derived Sorbents and Their Potential Roles in Heavy Metal Remediation Applications

    Directory of Open Access Journals (Sweden)

    Chiang Y. W.

    2013-04-01

    Full Text Available Inorganic waste materials that have the suitable inherent characteristics could be used as precursors for the synthesis of micro- and mesoporous materials, which present great potential to be re-utilized as sorbent materials for heavy metal remediation. Three inorganic waste materials were studied in the present work: water treatment residuals (WTRs from an integrated drinking water/wastewater treatment plant, and fly ash and bottom ash samples from a municipal solid waste incinerator (MSWI. These wastes were converted into three sorbent materials: ferrihydrite-like materials derived from drying of WTRs, hydroxyapatite-like material derived from ultrasound assisted synthesis of MSWI fly ash with phosphoric acid solution, and a zeolitic material derived from alkaline hydrothermal conversion of MSWI bottom ash. The performance of these materials, as well as their equivalent commercially available counterparts, was assessed for the adsorption of multiple heavy metals (As, Cd, Co, Ni, Pb, Zn from synthetic solutions, contaminated sediments and surface waters; and satisfactory results were obtained. In addition, it was observed that the combination of sorbents into sorbent mixtures enhanced the performance levels and, where applicable, stabilized inherently mobile contaminants from the waste derived sorbents.

  5. The use of lightweight expanded clay aggregate (LECA) as sorbent for PAHs removal from water.

    Science.gov (United States)

    Nkansah, Marian Asantewah; Christy, Alfred A; Barth, Tanja; Francis, George William

    2012-05-30

    Lightweight expanded clay aggregate (LECA) has been explored as a sorbent for the removal of PAHs (phenanthrene, fluoranthene and pyrene) from water. The efficacy of LECA as a sorbent for PAHs was assessed using contact time, mass of sorbent and sorption isotherms in a series of batch experiments. Maximum (optimum) sorption was reached at 21 h after which the amount of PAHs sorbed remained almost constant. Batch experiments were conducted by shaking a 100ml solution mixture of individual PAHs (containing 0.02 mg/L) with LECA. The maximum sorption was 70.70, 70.82 and 72.12%, respectively for phenanthrene, fluoranthene and pyrene when a mass of 0.2 g of sorbent was used. There was an increase in sorption as a result of an increase in mass of sorbent until a maximum was reached at a mass of 4.0 g LECA with 92.61, 93.91 and 94.15% sorption of phenanthrene, fluoranthene and pyrene respectively. Sorption data were fitted to the linearised forms of the Freundlich and Langmuir isotherm models to determine the water-LECA partitioning coefficient. Physical sorption caused by the aromatic nature of the compounds was the main mechanism that governed the removal process while the hydrophobicity of the PAHs also influenced the sorption capacity. LECA can be used as an alternative method for aqueous PAHs removal. Copyright © 2012 Elsevier B.V. All rights reserved.

  6. A new and efficient Solid Phase Microextraction approach for analysis of high fat content food samples using a matrix-compatible coating.

    Science.gov (United States)

    De Grazia, Selenia; Gionfriddo, Emanuela; Pawliszyn, Janusz

    2017-05-15

    The current work presents the optimization of a protocol enabling direct extraction of avocado samples by a new Solid Phase Microextraction matrix compatible coating. In order to further extend the coating life time, pre-desorption and post-desorption washing steps were optimized for solvent type, time, and degree of agitation employed. Using optimized conditions, lifetime profiles of the coating related to extraction of a group of analytes bearing different physical-chemical properties were obtained. Over 80 successive extractions were carried out to establish coating efficiency using PDMS/DVB 65µm commercial coating in comparison with the PDMS/DVB/PDMS. The PDMS/DVB coating was more prone to irreversible matrix attachment on its surface, with consequent reduction of its extractive performance after 80 consecutive extractions. Conversely, the PDMS/DVB/PDMS coating showed enhanced inertness towards matrix fouling due to its outer smooth PDMS layer. This work represents the first step towards the development of robust SPME methods for quantification of contaminants in avocado as well as other fatty-based matrices, with minimal sample pre-treatment prior to extraction. In addition, an evaluation of matrix components attachment on the coating surface and related artifacts created by desorption of the coating at high temperatures in the GC-injector port, has been performed by GCxGC-ToF/MS. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Performance of a novel synthetic Ca-based solid sorbent suitable for desulfurizing flue gases in a fluidized bed

    Energy Technology Data Exchange (ETDEWEB)

    Pacciani, R.; Muller, C.R.; Davidson, J.F.; Dennis, J.S.; Hayhurst, A.N. [University of Cambridge, Cambridge (United Kingdom). Dept. of Chemical Engineering & Biotechnology

    2009-08-05

    The extent and mechanism of sulfation and carbonation of limestone, dolomite, and chalk, were compared with a novel, synthetic sorbent (85 wt % CaO and 15 wt % Ca{sub 12}A{sub l14}O{sub 33}), by means of experiments undertaken in a small, electrically heated fluidized bed. The sorbent particles were used either (I) untreated, sieved to two particle sizes and reacted with two different concentrations of SO{sub 2}, or (ii) after being cycled 20 times between carbonation, in 15 vol % CO{sub 2} in N2, and calcination, in pure N2, at 750 degrees C. The uptake of untreated limestone and dolomite was generally low (<0.2 g(SO{sub 2})/g(sorbent)), confirming previous results, However, the untreated chalk and the synthetic sorbent were found to be substantially more reactive with SO{sub 2}, and their final uptake was significantly higher (>0.5 g(SO{sub 2})/g(sorbent)) and essentially independent of the particle size. Here, comparisons are made on the basis of the sorbents in the calcined state. The capacities for the uptake of SO{sub 2}, on a basis of unit mass of calcined sorbent, were comparable for the chalk and the synthetic sorbent. However, previous work has demonstrated the ability of the synthetic sorbent to retain its capacity for CO{sub 2} over many cycles of carbonation and calcination: much more so than natural sorbents such as chalk and limestone. Accordingly, the advantage of the synthetic sorbent is that it could be used to remove CO{sub 2} from flue gases and, at the end of its life, to remove SO{sub 2} on a once-through basis.

  8. Evaluation of Dry Sorbent Injection Technology for Pre-Combustion CO{sub 2} Capture

    Energy Technology Data Exchange (ETDEWEB)

    Richardson, Carl [URS Group, Inc., Austin, TX (United States); Steen, William [URS Group, Inc., Austin, TX (United States); Triana, Eugenio [URS Group, Inc., Austin, TX (United States); Machalek, Thomas [URS Group, Inc., Austin, TX (United States); Davila, Jenny [URS Group, Inc., Austin, TX (United States); Schmit, Claire [URS Group, Inc., Austin, TX (United States); Wang, Andrew [URS Group, Inc., Austin, TX (United States); Temple, Brian [URS Group, Inc., Austin, TX (United States); Lu, Yongqi [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Lu, Hong [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Zhang, Luzheng [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Ruhter, David [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Rostam-Abadi, Massoud [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Sayyah, Maryam [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Ito, Brandon [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States); Suslick, Kenneth [Illinois State Geological Survey - University of Illinois at Urbana-Champaign (United States)

    2013-09-30

    This document summarizes the work performed on Cooperative Agreement DE-FE0000465, “Evaluation of Dry Sorbent Technology for Pre-Combustion CO{sub 2} Capture,” during the period of performance of January 1, 2010 through September 30, 2013. This project involves the development of a novel technology that combines a dry sorbent-based carbon capture process with the water-gas-shift reaction for separating CO{sub 2} from syngas. The project objectives were to model, develop, synthesize and screen sorbents for CO{sub 2} capture from gasified coal streams. The project was funded by the DOE National Energy Technology Laboratory with URS as the prime contractor. Illinois Clean Coal Institute and The University of Illinois Urbana-Champaign were project co-funders. The objectives of this project were to identify and evaluate sorbent materials and concepts that were suitable for capturing carbon dioxide (CO{sub 2}) from warm/hot water-gas-shift (WGS) systems under conditions that minimize energy penalties and provide continuous gas flow to advanced synthesis gas combustion and processing systems. Objectives included identifying and evaluating sorbents that efficiently capture CO{sub 2} from a gas stream containing CO{sub 2}, carbon monoxide (CO), and hydrogen (H{sub 2}) at temperatures as high as 650 °C and pressures of 400-600 psi. After capturing the CO{sub 2}, the sorbents would ideally be regenerated using steam, or other condensable purge vapors. Results from the adsorption and regeneration testing were used to determine an optimal design scheme for a sorbent enhanced water gas shift (SEWGS) process and evaluate the technical and economic viability of the dry sorbent approach for CO{sub 2} capture. Project work included computational modeling, which was performed to identify key sorbent properties for the SEWGS process. Thermodynamic modeling was used to identify optimal physical properties for sorbents and helped down-select from the universe of possible sorbent

  9. CO{sub 2} capture by solid sorbents carbonates

    Energy Technology Data Exchange (ETDEWEB)

    Kruczek, Halina; Trzaska, Kinga [Wroclaw Univ. of Technology (Poland)

    2006-01-15

    The climate change problem requires new technologies to obtain energy from fossil fuels without emitting CO{sub 2} to the atmosphere. CO{sub 2}-capture and storage system applied to large stationary sources of CO{sub 2} are among a set of existing technologies that could help to stabilized in the next 50 years the CO{sub 2} concentration in the atmosphere. The use of a CaO/CaCO{sub 3} chemical loop is emerging as a viable technique for the capture of CO{sub 2} from combustion gases or from fuel gases to obtain H{sub 2}-rich gases. The CaO is used to strip the CO{sub 2} contained in the gases, by forming CaCO{sub 3}. The CaO is produced in the process of calcinations of some limestone. Limestone can be obtained from a huge variety of sources and various limestones differ considerably in their chemical composition and physical structure. The chemical reactivity of different limestones shows a large variation due to their differences in crystalline structure and also because of the nature of impurities such as silicon, iron, magnesium, sodium and potassium. The use of natural calcium carbonates as regenerable CO{sub 2} sorbents is limited by the decay of the carbonation conversion with the number of cycles carbonation/calcinations. This work presents an analysis of a carbonation/calcinations cycle to capture CO{sub 2} for 10 different natural calcium carbonates from different geological age (from chalk to dolomite). Thermogravimetric analysis of calcinations/carbonation process in multicycles at different parameter: temperature and atmosphere was carried out. Effect of concentration of carbon dioxide and steam water on calcination and carbonization was investigated. The capacity of sorption CO{sub 2} depending on initial parameters of limestone as chemical composition and structure and as well as on process parameters was determined. The parametric analysis of loss of carbonization was carried out.

  10. Silver-Loaded Aluminosilicate Aerogels As Iodine Sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Riley, Brian J. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Kroll, Jared O. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Peterson, Jacob A. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Matyáš, Josef [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Olszta, Matthew J. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Li, Xiaohong [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Vienna, John D. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States

    2017-09-14

    This paper discusses the development of aluminosilicates aerogels as scaffolds for Ag0 nanoparticles used for chemisorption of I2(g). The starting materials for these scaffolds included both Na-Al-Si-O and Al-Si-O aerogels, both synthesized from metal alkoxides. The Ag0 particles are added by soaking the aerogels in AgNO3 followed by drying and flowing under H2/Ar to reduce Ag+ → Ag0. In some cases, samples were soaked in 3-(mercaptopropyl)trimethoxysilane under supercritical CO2 to add –SH tethers to the aerogel surfaces for more effective binding of Ag+. During the Ag+-impregnation steps, for the Na-Al-Si-O aerogels, Na was replaced with Ag, and for the Al-Si-O aerogel, Si was replaced with Ag. The Ag-loading of thiolated versus non-thiolated Na-Al-Si-O aerogels was comparable at ~35 at% whereas the Ag-loading in unthiolated Al-Si-O aerogels was significantly lower at ~ 7 at% after identical treatment. Iodine loadings in both thiolated and unthiolated Ag0-functionalized Na-Al-Si-O aerogels were > 0.5 g g-1 showing almost complete utilization of the Ag through chemisorption to form AgI. Iodine loading in the thiolated Al-Si-O aerogel was 0.31 g g-1. The control of Ag uptake over solution residence time and [AgNO3] demonstrates the ability to customize the Ag-loading in the base sorbent to regulate the capacity of iodine chemisorption. Consolidation experimental results are also presented.

  11. Therapeutic effects of oral sorbent in undialyzed uremia.

    Science.gov (United States)

    Sanaka, T; Sugino, N; Teraoka, S; Ota, K

    1988-08-01

    The present study was carried out to clarify whether an oral sorbent, AST-120 (Kureha Chemical Ind Co, Tokyo), may postpone the initiation of dialysis therapy. The subjects were randomly divided into two groups, control and AST. The AST group consisted of 27 undialyzed uremic patients. Serum creatine concentrations (SCr) were 4.3 to 8.1 mg/dL (5.8 +/- 1.1 mg/dL, mean +/- SD). The control group consisted of 24 uremic patients who were not given AST-120 during the conservative therapy period before the initiation of hemodialysis. AST-120 (3.2 to 7.2 g/d) was administered to the patients in the AST group for 2.4 to 30.1 months (13.2 +/- 7.4) before the initiation of hemodialysis. The slopes of reciprocal creatinine v time in the control group were -1,251 +/- 856 x 10(-5) dL/mg/month during the 6 to 12 months before the initiation of dialysis therapy, and in the AST group, they were -1,004 +/- 1,012 x 10(-5) dL/mg/month before administration, and -347 +/- 509 x 10(-5) dL/mg/month after administration of AST-120 (P less than 0.01). All 24 patients in the control group and 21 of 27 in the AST group were introduced to hemodialysis. SCr and serum urea nitrogen (SUN) at the initiation of hemodialysis did not differ between the control and AST group: 10.8 +/- 2.6 and 11.0 +/- 2.2 mg/dL and 92.7 +/- 22.2 and 94.1 +/- 21.6 mg/dL, respectively. The times to the 50% undialyzed level were 5.0 months in the control group, and 14.3 months in the AST group.(ABSTRACT TRUNCATED AT 250 WORDS)

  12. Graphene Coatings

    DEFF Research Database (Denmark)

    Stoot, Adam Carsten; Camilli, Luca; Bøggild, Peter

    2014-01-01

    Owing to its remarkable electrical and mechanical properties, graphene has been attracting tremendous interest in materials science. In particular, its chemical stability and impermeability make it a promising protective membrane. However, recent investigations reveal that single layer graphene...... cannot be used as a barrier in the long run, due to galvanic corrosion phenomena arising when oxygen or water penetrate through graphene cracks or domain boundaries. Here, we overcome this issue by using a multilayered (ML) graphene coating. Our lab- as well as industrial-scale tests demonstrate that ML...... graphene can effectively protect Ni in harsh environments, even after long term exposure. This is made possible by the presence of a high number of graphene layers, which can efficiently mask the cracks and domain boundaries defects found in individual layers of graphene. Our findings thus show...

  13. Coating materials

    International Nuclear Information System (INIS)

    Ozeki, Takao; Kimura, Tadashi; Kobayashi, Juichi; Maeda, Yutaka; Nakamoto, Hideo.

    1969-01-01

    A non-solvent type coating material composition is provided which can be hardened by irradiation with active energy, particularly electron beams, using a composition which contains 10%-100% of a radically polymerizable low molecular compound (A), (hereafter called an oligomer), having at least two vinyl radicals in one molecule. These compositions have a high degree of polymerization and characteristics equivalent to thermosetting acrylic or amino alkyd resin. The oligomer (A) is produced by reacting an epoxy-containing vinyl monomer with saturated polycarboxylic acids or anhydrides. In one embodiment, 146 parts by weight of adipic acid and 280 parts of glycidyl methacrylate ester undergo addition reaction in the presence of a polymerization-inhibitor and a catalyst at 90 0 C for 6 hours to produce an oligomer having a fiberous divinyl construction. The coating composition utilizes this oligomer in the forms of (I-1), a whole oligomer; (I-2), 0%-90% of this oligomer and 90%-10% of a vinyl monomer containing at least 30% of (meth) acrylic monomer; (I-3), 10%-90% of such oligomer and 90%-10% of other monomers containing at least two vinyl radicals in one molecule; (I-4), a mixture of (I-2) and (I-3) in proportion of 1/9 to 9/1, and (I-5), above four compositions each containing 50% or less unsaturated polyester or drying oil having 500-5,000 molecules or a drying oil-modified alkyd resin having 500-5,000 molecules. Four examples are given. (Iwakiri, K.)

  14. Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

    Science.gov (United States)

    Alhendal, Abdullah; Mengis, Stephanie; Matthews, Jacob; Malik, Abdul

    2016-10-14

    Nonhydrolytic sol-gel (NHSG) route was used for the creation of novel zirconia-polypropylene oxide (ZrO 2 -PPO) sol-gel hybrid sorbents in the form of surface coatings for the extraction and preconcentration of catecholamine neurotransmitters and molecules structurally related to their deaminated metabolites. In comparison to other sorbents made of inorganic transition metal oxides, the presented hybrid organic-inorganic sorbents facilitated reversible sorption properties that allowed for efficient desorption of the extracted analytes by LC-MS compatible mobile phases. The presented sol-gel hybrid sorbents effectively overcame the major drawbacks of traditional silica- or polymer-based sorbents by providing superior pH stability (pH range: 0-14), and a variety of intermolecular interactions. Nonaqueous sol-gel treatment of PPO with ZrCl 4 was employed for the derivatization of the terminal hydroxyl groups on PPO, providing zirconium trichloride-containing end groups characterized by enhanced sol-gel reactivity. NHSG ZrO 2 -PPO sorbent provided excellent microextraction performance for catecholamines, low detection limits (5.6-9.6pM), high run-to-run reproducibility (RSD 0.6-5.1%), high desorption efficiency (95.0-99.5%) and high enrichment factors (∼1480-2650) for dopamine and epinephrine, respectively, extracted from synthetic urine samples. The presented sol-gel sorbents provided effective alternative to conventional extraction media providing unique physicochemical characteristics and excellent extraction capability. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Lanthanide sorbent based on magnetite nanoparticles functionalized with organophosphorus extractants

    OpenAIRE

    Basualto, C.; Gaete, J.; Molina, L.; Valenzuela, F.; Yáñez, C.; Marco, J.F.

    2015-01-01

    © 2015 National Institute for Materials Science. In this work, an adsorbent was prepared based on the attachment of organophosphorus acid extractants, namely, D2EHPA, CYANEX 272, and CYANEX 301, to the surface of superparamagnetic magnetite (Fe3O4) nanoparticles. The synthesized nanoparticles were coated with oleic acid, first by a chemisorption mechanism and later by the respective extractant via physical adsorption. The obtained core-shell functionalized magnetite nanoparticle composites we...

  16. Synthesis and characterization of sulfur functionalized graphene oxide nanosheets as efficient sorbent for removal of Pb2+, Cd2+, Ni2+ and Zn2+ ions from aqueous solution: A combined thermodynamic and kinetic studies

    Science.gov (United States)

    Pirveysian, Mahtab; Ghiaci, Mehran

    2018-01-01

    A very simple, one pot method was used for preparation of sulfur functionalized graphene oxide (GO-SOxR) with sodium sulfide and water in reflux condition. The elemental analysis data showed high sulfur content up to 15%. EDS and XPS analysis also proved introduction of sulfur element. To make the sorbent more efficient operationally, the GO-SOxR was coated with a mesoporous shell of TiO2 or SiO2. The prepared sorbents were characterized by SEM, TEM, TGA, XPS, XRD, IR and EDS. GO-SOxR@TiO2 and GO-SOxR@SiO2 composites were tested for removal of Pb(II), Cd(II), Ni(II) and Zn(II) as heavy metal ions from aqueous solution in batch method. Adsorption of the heavy metal ions was studied kinetically, and the adsorption capacities of GO-SOxR, GO-SOxR@TiO2, and GO-SOxR@SiO2 were evaluated using equilibrium adsorption isotherms, and compared to other adsorbents used for removal of these heavy metals. Kinetic studies showed that the experimental data was fitted with pseudo second order model. The adsorption capacity of GO was significantly improved by sulfur functionalization and TiO2 coating.

  17. Adsorption of Polycyclic Aromatic Hydrocarbons (PAHS from Aqueous Solutions on Different Sorbents

    Directory of Open Access Journals (Sweden)

    Smol Marzena

    2014-12-01

    Full Text Available This paper presents the results of the possibility and effectiveness of PAHs removal from a model aqueous solution, during the sorption on the selected sorbents. Six PAHs (naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene listed by EPA for the analysis in the environmental samples were determined. Model aqueous solution was prepared with RESTEK 610 mix PAHs standard. After the sorption process, decrease in the concentration of individual hydrocarbons was observed. The removal percentage was dependent on the type of sorbent (quartz sand, mineral sorbent, activated carbon. The highest efficiency (98.1% was observed for activated carbon.. The results shows that the sorption processes can be used in aqueous solutions treatment procedures.

  18. Removal of dissolved textile dyes from wastewater by a compost sorbent

    Science.gov (United States)

    Tsui, L.S.; Roy, W.R.; Cole, M.A.

    2003-01-01

    The objective of this study was to evaluate the potential for treating dye-contaminated waste streams by sorption using compost as a low-cost sorbent. A mature, thermophilic compost sample was used to sorb CI Acid Black 24, CI Acid Orange 74, CI Basic Blue 9, CI Basic Green 4, CI Direct Blue 71, CI Direct Orange 39, CI Reactive Orange 16 and CI Reactive Red 2 from solution using a batch-sorption method. With the exception of the two reactive dyes, the sorption kinetics were favourable for a continuous-flow treatment process with the compost-dye mixtures reaching a steady state within 3-5 h. Based on limited comparisons, the affinity of the compost for each dye appeared to be competitive with other non-activated carbon sorbents. The results suggest that additional research on using compost as a sorbent for dye-contaminated solutions is warranted.

  19. Ionic liquid-functionalized mesoporous sorbents and their use in the capture of polluting gases

    Science.gov (United States)

    Lee, Jong Suk; Koros, William J.; Bhuwania, Nitesh; Hillesheim, Patrick C.; Dai, Sheng

    2016-01-12

    A composite structure for capturing a gaseous electrophilic species, the composite structure comprising mesoporous refractory sorbent particles on which an ionic liquid is covalently attached, wherein said ionic liquid includes an accessible functional group that is capable of binding to said gaseous electrophilic species. In particular embodiments, the mesoporous sorbent particles are contained within refractory hollow fibers. Also described is a method for capturing a gaseous electrophilic species by use of the above-described composite structure, wherein the gaseous electrophilic species is contacted with the composite structure. In particular embodiments thereof, cooling water is passed through the refractory hollow fibers containing the IL-functionalized sorbent particles in order to facilitate capture of the gaseous electrophilic species, and then steam is passed through the refractory hollow fibers to facilitate release of the gaseous electrophilic species such that the composite structure can be re-used to capture additional gas.

  20. Collection of lanthanides and actinides from natural waters with conventional and nanoporous sorbents.

    Science.gov (United States)

    Johnson, Bryce E; Santschi, Peter H; Chuang, Chia-Ying; Otosaka, Shigeyoshi; Addleman, Raymond Shane; Douglas, Matt; Rutledge, Ryan D; Chouyyok, Wilaiwan; Davidson, Joseph D; Fryxell, Glen E; Schwantes, Jon M

    2012-10-16

    Effective collection of trace-level lanthanides and actinides is advantageous for recovery and recycling of valuable resources, environmental remediation, chemical separations, and in situ monitoring. Using isotopic tracers, we have evaluated a number of conventional and nanoporous sorbent materials for their ability to capture and remove selected lanthanides (Ce and Eu) and actinides (Th, Pa, U, and Np) from fresh and salt water systems. In general, the nanostructured materials demonstrated a higher level of performance and consistency. Nanoporous silica surface modified with 3,4-hydroxypyridinone provided excellent collection and consistency in both river water and seawater. The MnO(2) materials, in particular the high surface area small particle material, also demonstrated good performance. Other conventional sorbents typically performed at levels below the nanostructured sorbents and demonstrate a larger variability and matrix dependency.

  1. DEVELOPMENT OF DISPOSABLE SORBENTS FOR CHLORIDE REMOVAL FROM HIGH TEMPERATURE COAL-DERIVED GASES

    Energy Technology Data Exchange (ETDEWEB)

    Gopala Krishnan; Raghubir Gupta

    1999-09-01

    Advanced integrated-gasification combined-cycle (IGCC) and integrated-gasification fuel cell (IGFC) systems require the development of high temperature sorbents for the removal of hydrogen chloride (HCl) vapor to less than 1 parts-per-million (ppm) levels. HCl is a highly reactive, corrosive, and toxic gas which must be removed to meet environmental regulations, to protect power generation equipment, and to minimize deterioration of hot gas desulfurization sorbents. The objective of this program was to develop disposable, alkali-based sorbents capable of reducing HCl vapor levels to less than 1 ppm in the temperature range from 400 to 750 C and pressures in the range from 1 to 20 atm. The primary areas of focus of this program were to investigate different methods of sorbent fabrication, testing their suitability for different reactor configurations, obtaining reaction kinetics data, and conducting a preliminary economic feasibility assessment. This program was a joint effort between SRI International (SRI), Research Triangle Institute (RTI), and General Electric Corporate Research and Development (GE-CRD). SRI, the prime contractor and RTI, a major subcontractor, performed most of the work in this program. Thermochemical calculations indicated that sodium-based sorbents were capable of reducing HCl vapor levels to less than 1 ppm at temperatures up to 650 C, but the regeneration of spent sorbents would require complex process steps. Nahcolite (NaHCO{sub 3}), a naturally-occurring mineral, could be used as an inexpensive sorbent to remove HCl vapor in hot coal gas streams. In the current program, nahcolite powder was used to fabricate pellets suitable for fixed-bed reactors and granules suitable for fluidized-bed reactors. Pilot-scale equipment were used to prepare sorbents in large batches: pellets by disk pelletization and extrusion techniques, and granules by granulation and spray-drying techniques. Bench-scale fixed- and fluidized-bed reactors were assembled at

  2. Adsorption of arsenazo (III due by phosphorus-containing polymer sorbent

    Directory of Open Access Journals (Sweden)

    Alosmanov Rasim M.

    2016-01-01

    Full Text Available Phosphorus-containing polymer sorbent was employed for removal hazardous Arsenazo (III dye from water. The adsorption characteristics were determined by the study at different parameters such as effect of solution pH, effect of initial dye concentration, sorbent dose, phase contact time, and temperature. The equilibrium data were analyzed on the basis of various adsorption isotherm models, namely Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich. The highest monolayer adsorption capacity has been obtained (24.75 mg g-1 at 55°C. Different thermodynamic parameters such as free energy, enthalpy, and entropy have been calculated and it was concluded that when temperature rises, adsorption increases, indicating the endothermic nature of the process. Kinetic parameters were derived by pseudo-first-order, pseudo-second-order and intraparticle kinetic models. Scanning Electron Microscopy and Fourier Transform Infrared spectroscopy were used to characterize the sorbent and also to validate the adsorption mechanism.

  3. Efficiency of sugarcane bagasse-based sorbents for oil removal from engine washing wastewater.

    Science.gov (United States)

    Guilharduci, Viviane Vasques da Silva; Martelli, Patrícia Benedini; Gorgulho, Honória de Fátima

    2017-01-01

    This work evaluates the efficiency of sugarcane bagasse-based sorbents in the sorption of oil from engine washing wastewater. The sorbents were obtained from sugarcane bagasse in the natural form (SB-N) and modified with either acetic anhydride (SB-Acet) or 3-aminopropyltriethoxysilane (SB-APTS). The results showed that the sorption capacity of these materials decreased in the following order: SB-APTS > SB-N > SB-Acet. The superior oil sorption capacity observed for SB-APTS was attributed to the polar amino end groups in the silane structure, which acted to increase the hydrophilic character of the fibers. However, all the sorbents obtained in this study were able to clean a real sample of wastewater from engine washing, leading to significant reductions in suspended matter, sediment, anionic surfactants, and turbidity.

  4. Adsorption of Carbon Dioxide, Ammonia, Formaldehyde, and Water Vapor on Regenerable Carbon Sorbents

    Science.gov (United States)

    Wojtowicz, Marek A.; Cosgrove, Joseph E.; Serio, Michael A.; Wilburn, Monique

    2015-01-01

    Results are presented on the development of reversible sorbents for the combined carbon dioxide, moisture, and trace-contaminant (TC) removal for use in Extravehicular Activities (EVAs), and more specifically in the Primary Life Support System (PLSS). The currently available life support systems use separate units for carbon dioxide, trace contaminants, and moisture control, and the long-term objective is to replace the above three modules with a single one. Furthermore, the current TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal, which is nonregenerable, and the carbon-based sorbent under development in this project can be regenerated by exposure to vacuum at room temperature. In this study, several carbon sorbents were fabricated and tested for simultaneous carbon dioxide, ammonia, formaldehyde, and water sorption. Multiple adsorption/vacuum-regeneration cycles were demonstrated at room temperature, and also the enhancement of formaldehyde sorption by the presence of ammonia in the gas mixture.

  5. Electrocurtain coating process for coating solar mirrors

    Science.gov (United States)

    Kabagambe, Benjamin; Boyd, Donald W.; Buchanan, Michael J.; Kelly, Patrick; Kutilek, Luke A.; McCamy, James W.; McPheron, Douglas A.; Orosz, Gary R.; Limbacher, Raymond D.

    2013-10-15

    An electrically conductive protective coating or film is provided over the surface of a reflective coating of a solar mirror by flowing or directing a cation containing liquid and an anion containing liquid onto the conductive surface. The cation and the anion containing liquids are spaced from, and preferably out of contact with one another on the surface of the reflective coating as an electric current is moved through the anion containing liquid, the conductive surface between the liquids and the cation containing liquid to coat the conductive surface with the electrically conductive coating.

  6. Multifunctional humate-based magnetic sorbent: Preparation, properties and sorption of Cu (II), phosphates and selected pesticides

    Czech Academy of Sciences Publication Activity Database

    Janoš, P.; Kormunda, M.; Novák, František; Životský, O.; Fuitová, J.; Pilařová, V.

    2013-01-01

    Roč. 73, č. 1 (2013), s. 46-52 ISSN 1381-5148 Grant - others:GA ČR(CZ) GAP106/12/1116 Program:GA Institutional support: RVO:60077344 Keywords : magnetic sorbent * humate-based sorbent * heavy metals * phosphate * pesticides Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.822, year: 2013

  7. The use of the chelating sorbent polyarsenazo-N for the concentration of uranium(VI) in water analysis

    International Nuclear Information System (INIS)

    Shvoeva, O.P.; Kuchava, G.P.; Myasoedova, G.V.; Savvin, S.B.; Mezhirov, M.S.; Boiko, V.A.

    1988-01-01

    Uranium(VI) sorption has been studied on Polyarsenazo-N, a new type of sorbent, which is a polyacrylonitrile fiber filled with the finely divided chelating sorbent Polyarsenazo. Sorption and desorption curves were obtained, and conditions for concentrating uranium(VI) under dynamic conditions were chosen. A procedure was developed for the sorption-spectrophotometric determination of uranium in water

  8. Technology assessment guide for application of engineered sorbent barriers to low-level radioactive waste disposal sites

    Energy Technology Data Exchange (ETDEWEB)

    Freeman, H.D.; Jones, E.O.; Depner, J.P.

    1989-06-01

    An engineered sorbent barrier (ESB) uses sorbent materials (such as activated carbon or natural zeolites) to restrict migration of radionuclides from low-level waste sites. The permeability of the ESB allows moisture to pass while the sorbent material traps or absorbs contaminants. In contrast, waste sites with impermeable barriers could fill with water, especially those waste sites in humid climates. A sorbent barrier can be a simple, effective, and inexpensive method for restricting radionuclide migration. This report provides information and references to be used in assessing the sorbent barrier technology for low-level waste disposal. The ESB assessment is based on sorbent material and soil properties, site conditions, and waste properties and inventories. These data are used to estimate the thickness of the barrier needed to meet all performance requirements for the waste site. This document addresses the following areas: (1) site information required to assess the need and overall performance of a sorbent barrier; (2) selection and testing of sorbent materials and underlying soils; (3) use of radionuclide transport models to estimate the required barrier thickness and long-term performance under a variety of site conditions; (4) general considerations for construction and quality assurance; and (5) cost estimates for applying the barrier. 37 refs., 6 figs., 2 tabs.

  9. Development of Superior Sorbents for Separation of CO2 from Flue Gas at a Wide Temperature Range During Coal Combustion

    Energy Technology Data Exchange (ETDEWEB)

    Panagiotis G. Smirniotis

    2007-06-30

    In chapter 1, the studies focused on the development of novel sorbents for reducing the carbon dioxide emissions at high temperatures. Our studies focused on cesium doped CaO sorbents with respect to other major flue gas compounds in a wide temperature range. The thermo-gravimetric analysis of sorbents with loadings of CaO doped on 20 wt% cesium demonstrated high CO{sub 2} sorption uptakes (up to 66 wt% CO{sub 2}/sorbent). It is remarkable to note that zero adsorption affinity for N{sub 2}, O{sub 2}, H{sub 2}O and NO at temperatures as high as 600 C was observed. For water vapor and nitrogen oxide we observed a positive effect for CO{sub 2} adsorption. In the presence of steam, the CO{sub 2} adsorption increased to the highest adsorption capacity of 77 wt% CO{sub 2}/sorbent. In the presence of nitrogen oxide, the final CO{sub 2} uptake remained same, but the rate of adsorption was higher at the initial stages (10%) than the case where no nitrogen oxide was fed. In chapter 2, Ca(NO{sub 3}){sub 2} {center_dot} 4H{sub 2}O, CaO, Ca(OH){sub 2}, CaCO{sub 3}, and Ca(CH{sub 3}COO){sub 2} {center_dot} H{sub 2}O were used as precursors for synthesis of CaO sorbents on this work. The sorbents prepared from calcium acetate (CaAc{sub 2}-CaO) resulted in the best uptake characteristics for CO{sub 2}. It possessed higher BET surface area and higher pore volume than the other sorbents. According to SEM images, this sorbent shows 'fluffy' structure, which probably contributes to its high surface area and pore volume. When temperatures were between 550 and 800 C, this sorbent could be carbonated almost completely. Moreover, the carbonation progressed dominantly at the initial short period. Under numerous adsorption-desorption cycles, the CaAc{sub 2}-CaO demonstrated the best reversibility, even under the existence of 10 vol % water vapor. In a 27 cyclic running, the sorbent sustained fairly high carbonation conversion of 62%. Pore size distributions indicate that their

  10. Mercury removal from MSW incineration flue gas by mineral-based sorbents.

    Science.gov (United States)

    Rumayor, M; Svoboda, K; Švehla, J; Pohořelý, M; Šyc, M

    2018-03-01

    Three samples of commercially available mineral-based sorbents (zeolite, bentonite and diatomaceous earth) were selected and evaluated for Hg capture under conditions of simulated dry flue gas atmosphere typical in Municipal Solid Waste Incineration (MSWI). The experiments were carried out in a lab-scale fixed-bed device at temperatures between 120 and 200 °C. Two samples of activated carbons (AC) (raw-AC and sulphur impregnated AC) were tested under the same conditions. The mineral-based sorbents were chemically promoted by sulphur, FeCl 3 and CaBr 2 , achieving an improvement in the overall reduction percentage of Hg 0 out (g) up to 85%, which was comparable to that obtained using a commercial activated carbon for Hg capture (sulphur impregnated AC). The study demonstrates that sorbents with a matrix relatively richer in TiO 2 , Fe 2 O 3 and Al 2 O 3 , as bentonite, favour Hg heterogeneous oxidation. The best Hg capture capacity was achieved with a zeolite sorbent sample characterized by high specific surface (132 m 2 /g) and impregnated with elemental sulphur. The final form of mercury retained in this sorbent was HgS with proved long-term stability in disposal and landfilling. The higher the temperature, the lower the efficiency of Hg capture being the optimum temperature for Hg-capture in the range of 120-150 °C. This study provides a basis for the development of new efficient non-carbon sorbents for mercury removal in the air pollution control lines of MSWI facilities considering the non-hazardous final form of mercury and its long-term landfilling/sequestration. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Development and validation of automatic HS-SPME with a gas chromatography-ion trap/mass spectrometry method for analysis of volatiles in wines.

    Science.gov (United States)

    Paula Barros, Elisabete; Moreira, Nathalie; Elias Pereira, Giuliano; Leite, Selma Gomes Ferreira; Moraes Rezende, Claudia; Guedes de Pinho, Paula

    2012-11-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed in order to quantify a large number of volatile compounds in wines such as alcohols, ester, norisoprenoids and terpenes. The procedures were optimized for SPME fiber selection, pre-incubation temperature and time, extraction temperature and time, and salt addition. A central composite experimental design was used in the optimization of the extraction conditions. The volatile compounds showed optimal extraction using a DVB/CAR/PDMS fiber, incubation of 5 ml of wine with 2g NaCl at 45 °C during 5 min, and subsequent extraction of 30 min at the same temperature. The method allowed the identification of 64 volatile compounds. Afterwards, the method was validated successfully for the most significant compounds and was applied to study the volatile composition of different white wines. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Comparison between solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HFLPME) for determination of extractables from post-consumer recycled PET into food simulants.

    Science.gov (United States)

    Oliveira, Éder Costa; Echegoyen, Yolanda; Cruz, Sandra Andrea; Nerin, Cristina

    2014-09-01

    Hollow fiber liquid phase microextraction (HFLPME) and solid phase microextraction (SPME) methods for pre-concentration of contaminants (toluene, benzophenone, tetracosane and chloroform) in food simulants were investigated. For HFLPME 1-heptanol, 2-octanone and dibutyl-ether were studied as extracting solvents. Analysis by gas chromatography coupled to mass spectrometry (GC-MS), flame ionization (GC-FID) and electron capture detectors (GC-ECD) were carried out. In addition, the methods were employed to evaluate the safety in use of a PET material after the recycling process (comprising washing, extrusion and solid state polymerization (SSP)) through extractability studies of the contaminants using 10% (v/v) ethanol in deionized water and 3% (w/v) acetic acid in deionized water as food simulants in different conditions: 10 days at 40°C and 2h at 70°C. The HFLPME preconcentration method provided increased sensitivity when compared to the SPME method and allowed to analyze concentration levels below 10 µg surrogate per kg food simulant. The results of the extractability studies showed considerable reductions after the extrusion and SSP processes and indicated the compliance with regulations for using recycled PET in contact with food. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Scalable improvement of SPME multipolar electrostatics in anisotropic polarizable molecular mechanics using a general short-range penetration correction up to quadrupoles.

    Science.gov (United States)

    Narth, Christophe; Lagardère, Louis; Polack, Étienne; Gresh, Nohad; Wang, Qiantao; Bell, David R; Rackers, Joshua A; Ponder, Jay W; Ren, Pengyu Y; Piquemal, Jean-Philip

    2016-02-15

    We propose a general coupling of the Smooth Particle Mesh Ewald SPME approach for distributed multipoles to a short-range charge penetration correction modifying the charge-charge, charge-dipole and charge-quadrupole energies. Such an approach significantly improves electrostatics when compared to ab initio values and has been calibrated on Symmetry-Adapted Perturbation Theory reference data. Various neutral molecular dimers have been tested and results on the complexes of mono- and divalent cations with a water ligand are also provided. Transferability of the correction is adressed in the context of the implementation of the AMOEBA and SIBFA polarizable force fields in the TINKER-HP software. As the choices of the multipolar distribution are discussed, conclusions are drawn for the future penetration-corrected polarizable force fields highlighting the mandatory need of non-spurious procedures for the obtention of well balanced and physically meaningful distributed moments. Finally, scalability and parallelism of the short-range corrected SPME approach are addressed, demonstrating that the damping function is computationally affordable and accurate for molecular dynamics simulations of complex bio- or bioinorganic systems in periodic boundary conditions. Copyright © 2016 Wiley Periodicals, Inc.

  14. The dynamics of the HS/SPME-GC/MS as a tool to assess the spoilage of minced beef stored under different packaging and temperature conditions.

    Science.gov (United States)

    Argyri, Anthoula A; Mallouchos, Athanasios; Panagou, Efstathios Z; Nychas, George-John E

    2015-01-16

    The aim of the current study was to assess meat spoilage through the evolution of volatile compounds using chemometrics. Microbiological and sensory assessment, pH measurement and headspace solid phase microextraction gas chromatography/mass spectroscopy (headspace SPME-GC/MS) analysis were carried out in minced beef stored aerobically and under modified atmosphere packaging (MAP) at 0, 5, 10, and 15 °C. It was shown that the HS/SPME-GC/MS analysis provided useful information about a great number of volatile metabolic compounds detected during meat storage. Many of the identified and semi-quantified compounds were correlated with the sensory scores through the use of chemometrics, depicting possible spoilage indicators such as 2-pentanone, 2-nonanone, 2-methyl-1-butanol, 3-methyl-1-butanol, ethyl hexanoate, ethyl propanoate, ethyl lactate, ethyl acetate, ethanol, 2-heptanone, 3-octanone, diacetyl, and acetoin. Finally, the applied GC/MS global models were able to estimate the microbial counts of the different microorganisms and the sensory scores of a meat sample regardless of storage conditions (i.e. packaging and temperature). Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Disposable Polydimethylsiloxane (PDMS-Coated Fused Silica Optical Fibers for Sampling Pheromones of Moths.

    Directory of Open Access Journals (Sweden)

    Rik Lievers

    Full Text Available In the past decades, the sex pheromone composition in female moths has been analyzed by different methods, ranging from volatile collections to gland extractions, which all have some disadvantage: volatile collections can generally only be conducted on (small groups of females to detect the minor pheromone compounds, whereas gland extractions are destructive. Direct-contact SPME overcomes some of these disadvantages, but is expensive, the SPME fiber coating can be damaged due to repeated usage, and samples need to be analyzed relatively quickly after sampling. In this study, we assessed the suitability of cheap and disposable fused silica optical fibers coated with 100 μm polydimethylsiloxane (PDMS by sampling the pheromone of two noctuid moths, Heliothis virescens and Heliothis subflexa. By rubbing the disposable PDMS fibers over the pheromone glands of females that had called for at least 15 minutes and subsequently extracting the PDMS fibers in hexane, we collected all known pheromone compounds, and we found a strong positive correlation for most pheromone compounds between the disposable PDMS fiber rubs and the corresponding gland extracts of the same females. When comparing this method to volatile collections and the corresponding gland extracts, we generally found comparable percentages between the three techniques, with some differences that likely stem from the chemical properties of the individual pheromone compounds. Hexane extraction of cheap, disposable, PDMS coated fused silica optical fibers allows for sampling large quantities of individual females in a short time, eliminates the need for immediate sample analysis, and enables to use the same sample for multiple chemical analyses.

  16. Data summary report for M.W. Kellogg Z-sorb sorbent tests. CRADA 92-008 Final report

    Energy Technology Data Exchange (ETDEWEB)

    Everett, C E; Monaco, S J

    1994-05-01

    A series of tests were undertaken from August 6, 1992 through July 6, 1993 at METC`s High Pressure Bench-Scale Hot Gas Desulfurization Unit to support a Cooperative Research and Development Agreement (CRADA) between METC`s Sorbent Development Cluster and M.W. Kellogg. The M.W. Kellogg Company is currently developing a commercial offering of a hot gas clean-up system to be used in Integrated Gasification Combined Cycle (IGCC) systems. The intent of the CRADA agreement was to identify a suitable zinc-based desulfurization sorbent for the Sierra Pacific Power Company Clean Coal Technology Project, to identify optimum operating conditions for the sorbent, and to estimate potential sorbent loss per year. This report presents results pertaining to Phillips Petroleum`s Z-Sorb III sorbent.

  17. Development of disposal sorbents for chloride removal from high-temperature coal-derived gases

    Energy Technology Data Exchange (ETDEWEB)

    Krishnan, G.N.; Wood, B.J.; Canizales, A.; Gupta, R.; Sheluker, S.D.; Ayala, R.

    1994-10-01

    The goal of this program is to develop alkali-based disposable sorbents capable of reducing HCl vapor concentrations to less than 1 ppm in coal gas streams at temperatures in the 480 degree C to 750 degree C range and pressures in the range 1 to 20 atm. The primary areas of focus of this program are investigation of different processes for fabricating the sorbents, testing their suitability for different reactor configurations (fixed-, moving-, and fluidized-bed reactors), obtaining kinetic data for commercial reactor design, and updating the economics of the process.

  18. Development of disposal sorbents for chloride removal from high-temperature coal-derived gases

    Energy Technology Data Exchange (ETDEWEB)

    Krishnan, G.N.; Wood, B.J.; Canizales, A. [and others

    1995-11-01

    The objective of this program is to develop alkali-based disposable sorbents capable of reducing HCl vapor concentrations to less than 1 ppmv in coal gas streams at temperatures in the range 400{degrees} to 750{degrees}C and pressures in the range 1 to 20 atm. The primary areas of focus of this program are investigation of different processes for fabricating the sorbents, testing their suitability for different reactor configurations, obtaining kinetic data for commercial reactor design, and updating the economics of the process.

  19. Removal of Pb2+, Cd2+ and Co2+ ions by means of various magnetic sorbents

    Directory of Open Access Journals (Sweden)

    Hredzák Slavomír

    2002-03-01

    Full Text Available The contribution presents the results of the cleaning of waters contaminated by heavy metal ions by means of magnetic sorbents that in special cases are also called magnetic carriers. The wastes from metallurgical industry and thermal power generation, such as the so called Albanian magnetite-containing leaching residuum (produced in the former Ni-hydrometallurgical plant in Sereï, a hematite-bearing red mud from Al2O3 production in Žiar n/Hronom and a magnetic fraction of ash from the coal-fired power plant EVO Vojany, were applied as magnetic sorbents.The sorbents coming out from Ni and Al2O3 production were subjected to the mechanical activation in a vibration mill before their using in cleaning tests, while the magnetic fraction of ash was applied without the activation. As to the sorbents properties, the grain size, the mineralogical and/or chemical composition as well as the magnetic susceptibility have been studied with the aim to assess and compare their possible sorption capacity.As contaminated waters the prepared water solutions containing ions of Pb2+, Cd2+, Co2+ were used. The magnetic sorbents after their mixing with contaminated waters have been filtered through a layer of spherical inductive bodies located in a magnetic field. The influence of the magnetic carrier concentration, time of agitation, and the pH value on the efficiency of water cleaning process was investigated.An efficacious sorption capacity was observed for all three applied sorbents. The most expressive reduction of Pb2+, Cd2+ and Co2+ content was achieved at the pH value of 9. During experiments on the Pb2+ content decrease, a reduction from 85 µg.ml-1 to <1 µg.ml-1 was observed for all three sorbents. Generally, regarding the Cd2+content decrease, it was showed, that a reduction from 105 µg.ml-1 to <0.1 µg.ml-1 can be attained. In the case of Co2+ content in water, the strongest reduction, i. e. from 99.2 µg.ml-1 to 0.06 µg.ml-1, was obtained by

  20. Structure and properties of magnetic composite sorbents based on hypercrosslinked polystyrenes

    Science.gov (United States)

    Pastukhov, A. V.; Davankov, V. A.; Lubentsova, K. I.; Kosandrovich, E. G.; Soldatov, V. S.

    2013-10-01

    Magnetic composite sorbents based on microporous and biporous hypercrosslinked polystyrenes (HCPs) with inclusions of iron oxide nanoparticles were studied by X-ray diffraction and differential thermal analysis. In microporous composites, the size of impregnated magnetite nanoparticles was less than ˜6 nm, the nanocomposites remaining optically transparent. Biporous HCPs (with micro- and macropores) had larger nanoparticles (˜16 nm). The sorption studies revealed that composite magnetic sorbents, as well as the starting hypercrosslinked polystyrenes, are effective adsorbents with high capacity for many compounds including toxic and physiologically active compounds.

  1. Remediation of hydrocarbon contaminants in cold environments - Electrokinetically enhanced bioremediation and biodegradable oil sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Suni, S. [Helsinki Univ. (Finland). Dept. of Environmental and Ecological Sciences

    2006-07-01

    Owing to the vast amounts of oil in the world, oil spills are common on land as well as at sea. In addition to oil products, other industrially used hydrocarbons, such as creosote, also contaminate soils. Most hydrocarbons are biodegradable. Hence, bioremediation is an attractive alternative for cleaning up hydrocarbon spills. In cold climate areas, however, biodegradation is often a slow process. The aim of this thesis was to develop efficient, cost-effective, and ecologically sound techniques for cold climate areas for the treatment of both oil spills on water or solid surfaces and for subsurface contamination. For subsurface hydrocarbon spills, the approach was to use electrokinetics in order to deliver nutrients and possibly microorganisms to contaminated soils, and in order to heat the soil to increase contaminant bioavailability and microbial activity. Electroosmosis proved to be an effective method to disperse bacteria and nutrients in medium- or fine-grained soils, where uncharged particles migrated with water through the soil towards the cathode. Creosote degradation proceeded faster with electroosmotically added nutrients than in controls without additions. However, inoculation with enriched creosote-degraders was not necessary because the indigenous microbes of the soil were well adapted to the creosote contaminants. For small-scale oil spills, the usual remediation method involves absorption with oil sorbents. Most sorbents in use today are synthetic and incineration is the only method for their disposal. A biodegradable sorbent, however, could be processed, for instance, in compost-like systems. Cotton grass is a common plant in peat bogs and its water-repellent fibre is a by-product of peat excavation. Cotton grass proved to be an excellent oil sorbent especially for spills on the surface of water: It absorbed up to three times as much oil as a commercial, synthetic oil sorbent. Cotton grass performed extremely well also in conditions simulating

  2. Application of selective inorganic sorbents to decontamination of NPP liquid effluents

    International Nuclear Information System (INIS)

    Boguslavskij, V.B.; Galkin, V.M.; Kuz'mina, R.V.

    1987-01-01

    Sorbtion-selective and physico-chemical properties of the zirconium and titanium ferricyanides base spherical sorbents, produced by sol-gel technique, are studied. Results on the enlarged bench tests of these sorbents at decontamination of the Beloyarsk NPP low-active effluents off 137 Cs, 134 Cs and 60 Co are presented. Tests have shown high efficiency (by more, than one order) of decontamination of waste water, containing surface-active agents and detergents, off cesium radionuclides. Water decontamination for 60 Co is less effective

  3. Selective Removal of Nitrosamines from a Model Amine Carbon-Capture Waterwash Using Low-Cost Activated-Carbon Sorbents.

    Science.gov (United States)

    Widger, Leland R; Combs, Megan; Lohe, Amit R; Lippert, Cameron A; Thompson, Jesse G; Liu, Kunlei

    2017-09-19

    Nitrosamines generated in the amine solvent loop of postcombustion carbon capture systems are potent carcinogens, and their emission could pose a serious threat to the environment or human health. Nitrosamine emission control strategies are critical for the success of amine-based carbon capture as the technology approaches industrial-scale deployment. Waterwash systems have been used to control volatile and aerosol emissions, including nitrosamines, from carbon-capture plants, but it is still necessary to remove or destroy nitrosamines in the circulating waterwash to prevent their subsequent emission into the environment. In this study, a cost-effective method for selectively removing nitrosamines from the absorber waterwash effluent with activated-carbon sorbents was developed to reduce the environmental impact associated with amine-based carbon capture. The results show that the commercial activated-carbon sorbents tested have a high capacity and selectivity for nitrosamines over the parent solvent amines, with capacities up to 190 mg/g carbon, under simulated amine waterwash conditions. To further reduce costs, an aerobic thermal sorbent regeneration step was also examined due to the low thermal stability of nitrosamines. To model the effect of oxidation on the sorbent performance, thermal- and acid-oxidized sorbents were also prepared from the commercial sorbents and analyzed. The chemical and physical properties of nitrosamines, the parent amine, and the influence of the physical properties of the carbon sorbents on nitrosamine adsorption was examined. Key sorbent properties included the sorbent hydrophilicity and hydrophobicity, surface pK a of the sorbent, and chemical structure of the parent amine and nitrosamine.

  4. High-Performance Sorbents for Carbon Dioxide Capture from Air

    Energy Technology Data Exchange (ETDEWEB)

    Sholl, David; Jones, Christopher

    2013-03-13

    This project has focused on capture of CO{sub 2} from ambient air (“air capture”). If this process is technically and economically feasible, it could potentially contribute to net reduction of CO{sub 2} emissions in ways that are complementary to better developed techniques for CO{sub 2} from concentrated point sources. We focused on cyclic adsorption processes for CO{sub 2} capture from air in which the entire cycle is performed at moderate temperatures. The project involved both experimental studies of sorbent materials and process level modeling of cyclic air capture processes. In our experimental work, a series of amine-functionalized silica adsorbents were prepared and characterized to determine the impact of molecular architecture on CO{sub 2} capture. Some key findings were: • Amine functionalized silicas can be prepared with high enough CO{sub 2} capacities under ambient conditions to merit consideration for use in air capture processes. • Primary amines are better candidates for CO{sub 2} capture than secondary or tertiary amines, both in terms of amine efficiency for CO{sub 2} adsorption and enhanced water affinity. • Mechanistic understanding of degradation of these materials can enable control of molecular architecture to significantly improve material stability. Our process modeling work provided the first publically available cost and energy estimates for cyclic adsorption processes for air capture of CO{sub 2}. Some key findings were: • Cycles based on diurnal ambient heating and cooling cannot yield useful purities or amounts of captured CO{sub 2}. • Cycles based on steam desorption at 110 oC can yield CO{sub 2} purities of ~88%. • The energy requirements for cycles using steam desorption are dominated by needs for thermal input, which results in lower costs than energy input in the form of electricity. Cyclic processes with operational costs of less than $100 tCO{sub 2}-net were described, and these results point to process and

  5. Flow coating apparatus and method of coating

    Science.gov (United States)

    Hanumanthu, Ramasubrahmaniam; Neyman, Patrick; MacDonald, Niles; Brophy, Brenor; Kopczynski, Kevin; Nair, Wood

    2014-03-11

    Disclosed is a flow coating apparatus, comprising a slot that can dispense a coating material in an approximately uniform manner along a distribution blade that increases uniformity by means of surface tension and transfers the uniform flow of coating material onto an inclined substrate such as for example glass, solar panels, windows or part of an electronic display. Also disclosed is a method of flow coating a substrate using the apparatus such that the substrate is positioned correctly relative to the distribution blade, a pre-wetting step is completed where both the blade and substrate are completed wetted with a pre-wet solution prior to dispensing of the coating material onto the distribution blade from the slot and hence onto the substrate. Thereafter the substrate is removed from the distribution blade and allowed to dry, thereby forming a coating.

  6. Niobium pentoxide coating replacing zinc phosphate coating

    OpenAIRE

    RODRIGUES, P.R.P.; TERADA, M.; JUNIOR, O.R.A.; LOPES, A.C.; COSTA, I.; BANCZEK, E.P.

    2015-01-01

    A new coating made of niobium pentoxide, obtained through the sol-gel process, was developed for the carbon steel (SAE 1010). The corrosion protection provided by this coating was evaluated through electrochemical tests such as: open circuit potential, electrochemical impedance spectroscopy and anodic potentiodynamic polarization in NaCl 0,5 mol L-1 solution. The morphology and composition of the coatings were analyzed using scanning electronic microscopy, energy dispersive spectroscopy and X...

  7. Production of sorbent from paper industry solid waste for oil spill cleanup.

    Science.gov (United States)

    Demirel Bayık, G; Altın, A

    2017-12-15

    The aim of the study is to select a cellulosic waste material from paper industry solid wastes and process it for sorbent production. Four different solid wastes were collected from a local paper production facility and rejects were selected due to its sorption capacity and processability. Oil sorption experiments were conducted according to the ASTM F 726-12 method. Effect of sorbent dosage, contact and dripping time, recovery of the oil, reusability of the sorbent and sorption from the water surface were also determined. Maximum oil sorption capacity was determined as 9.67, 12.92 and 12.84g/g for diesel oil, 0W30 and 10W30 motor oils respectively for the static test and 8.27, 10.45 and 11.69g/g for the dynamic test. An efficient and low-cost sorbent was produced from paper industry rejects that can be used on land and on water. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Recovery of Lithium from Geothermal Brine with Lithium-Aluminum Layered Double Hydroxide Chloride Sorbents.

    Science.gov (United States)

    Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi; Hoke, Thomas; Ucar, Huseyin; Moyer, Bruce A; Harrison, Stephen

    2017-11-21

    We report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloride from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ∼91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. The present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.

  9. ACTIVATION AND REACTIVITY OF NOVEL CALCIUM-BASED SORBENTS FOR DRY SO2 CONTROL IN BOILERS

    Science.gov (United States)

    Chemically modified calcium hydroxide (Ca(OH)2) sorbents developed in the U.S. Environmental Protection Agency's Air and Energy Engineering Research Laboratory (AEERL) for sulfur dioxide (SO2) control in utility boilers were tested in an electrically heated, bench-scale isotherma...

  10. Contribution of individual sorbents to the control of heavy metal activity in sandy soil

    NARCIS (Netherlands)

    Weng, L.; Temminghoff, E.J.M.; Riemsdijk, van W.H.

    2001-01-01

    A multisurface model is used to evaluate the contribution of various sorption surfaces to the control of heavy metal activity in sandy soil samples at pH 3.7-6.1 with different sorbent contents. This multisurface model considers soil as a set of independent sorption surfaces, i.e. organic matter

  11. Mercury Removal from MSW Incineration Flue Gas by Mineral-based Sorbents.

    Czech Academy of Sciences Publication Activity Database

    Rumayor, Marta; Svoboda, Karel; Švehla, Jaroslav; Pohořelý, Michael; Šyc, Michal

    Roč. 73, DEC 13 ( 2018 ), s. 265-270 ISSN 0956-053X R&D Projects: GA TA ČR TE02000236 Institutional support: RVO:67985858 Keywords : mercury * removal * mineral sorbents Subject RIV: DI - Air Pollution ; Quality OBOR OECD: Environmental sciences (social aspects to be 5.7) Impact factor: 4.030, year: 2016

  12. Microbial consortia in mesocosm bioremediation trial using oil sorbents, slow-release fertilizer and bioaugmentation.

    Science.gov (United States)

    Gertler, Christoph; Gerdts, Gunnar; Timmis, Kenneth N; Golyshin, Peter N

    2009-08-01

    An experimental prototype oil boom including oil sorbents, slow-release fertilizers and biomass of the marine oil-degrading bacterium, Alcanivorax borkumensis, was applied for sorption and degradation of heavy fuel oil in a 500-L mesocosm experiment. Fingerprinting of DNA and small subunit rRNA samples for microbial activity conducted to study the changes in microbial communities of both the water body and on the oil sorbent surface showed the prevalence of A. borkumensis on the surface of the oil sorbent. Growth of this obligate oil-degrading bacterium on immobilized oil coincided with a 30-fold increase in total respiration. A number of DNA and RNA signatures of aromatic hydrocarbon-degrading bacteria were detected both in samples of water body and on oil sorbent. Ultimately, the heavy fuel oil in this mesocosm study was effectively removed from the water body. This is the first study to successfully investigate the fate of oil-degrading microbial consortia in an experimental prototype for a bioremediation strategy in offshore, coastal or ship-bound oil spill mitigation using a combination of mechanical and biotechnological techniques.

  13. Adsorption of gaseous RuO4 by various sorbents. II

    International Nuclear Information System (INIS)

    Vujisic, L.; Nikolic, R.

    1983-01-01

    Sorption of gaseous RuO 4 on impregnated Alcoa Alumina H-151, impregnated charcoal, silica gel and HEPA filter was investigated. The results obtained on various sorbents are compared and discussed in connection with possibilities to use the chosen material in air cleaning systems

  14. High temperature capture of CO2 on lithium-based sorbents from rice husk ash.

    Science.gov (United States)

    Wang, Ke; Guo, Xin; Zhao, Pengfei; Wang, Fanzi; Zheng, Chuguang

    2011-05-15

    Highly efficient Li(4)SiO(4) (lithium orthosilicate)-based sorbents for CO(2) capture at high temperature, was developed using waste materials (rice husk ash). Two treated rice husk ash (RHA) samples (RHA1 and RHA2) were prepared and calcined at 800°C in the presence of Li(2)CO(3). Pure Li(4)SiO(4) and RHA-based sorbents were characterized by X-ray fluorescence, X-ray diffraction, scanning electron microscopy, nitrogen adsorption, and thermogravimetry. CO(2) sorption was tested through 15 carbonation/calcination cycles in a fixed bed reactor. The metals of RHA were doped with Li(4)SiO(4) resulting to inhibited growth of the particles and increased pore volume and surface area. Thermal analyses indicated a much better CO(2) absorption in Li(4)SiO(4)-based sorbent prepared from RHA1 (higher metal content sample) because the activation energies for the chemisorption process and diffusion process were smaller than that of pure Li(4)SiO(4). RHA1-based sorbent also maintained higher capacities during the multiple cycles. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. CO2 removal from biogas with supported amine sorbents : First technical evaluation based on experimental data

    NARCIS (Netherlands)

    Sutanto, Stevia; Dijkstra, J. W.; Pieterse, J. A.Z.; Boon, J; Hauwert, P.; Brilman, D. W.F.

    2017-01-01

    Biogas from fermentation of manure and organic residues produces a gas stream that can be fed into the natural gas grid, provided impurities (CO2, H2S and H2O) are removed according to specifications prior to grid injection. Compared to conventional technologies, supported amine sorbents (SAS) seem

  16. Anaerobic co-digestion of cork based oil sorbent and cow manure or sludge

    NARCIS (Netherlands)

    Cavaleiro, A.J.; Neves, T.M.; Guedes, A.P.; Alves, M.M.; Pinto, P.; Silva, S.P.; Machado de Sousa, Diana

    2015-01-01

    Cork, a material with great economic, social and environmental importance in Portugal, is also a good oil sorbent that can be used in the remediation of oil spills. The oil-impregnated cork can be easily removed, but requires further treatment. In the case of vegetable oil spills, anaerobic

  17. Theoretical evaluation on selective adsorption characteristics of alkali metal-based sorbents for gaseous oxidized mercury.

    Science.gov (United States)

    Tang, Hongjian; Duan, Yufeng; Zhu, Chun; Cai, Tianyi; Li, Chunfeng; Cai, Liang

    2017-10-01

    Alkali metal-based sorbents are potential for oxidized mercury (Hg 2+ ) selective adsorption but show hardly effect to elemental mercury (Hg 0 ) in flue gas. Density functional theory (DFT) was employed to investigate the Hg 0 and HgCl 2 adsorption mechanism over alkali metal-based sorbents, including calcium oxide (CaO), magnesium oxide (MgO), potassium chloride (KCl) and sodium chloride (NaCl). Hg 0 was found to weakly interact with CaO (001), MgO (001), KCl (001) and NaCl (001) surfaces while HgCl 2 was effectively adsorbed on top-O and top-Cl sites. Charge transfer and bond population were calculated to discuss the covalency and ionicity of HgCl 2 bonding with the adsorption sites. The partial density of states (PDOS) analysis manifests that HgCl 2 strongly interacts with surface sites through the orbital hybridizations between Hg and top O or Cl. Frontier molecular orbital (FMO) energy and Mulliken electronegativity are introduced as the quantitative criteria to evaluate the reactivity of mercury species and alkali metal-based sorbents. HgCl 2 is identified as a Lewis acid and more reactive than Hg 0 . The Lewis basicity of the four alkali metal-based sorbents is predicted as the increasing order: NaCl < MgO < KCl < CaO, in consistence with the trend of HgCl 2 adsorption energies. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Super-Hydrophobic High Throughput Electrospun Cellulose Acetate (CA) Nanofibrous Mats as Oil Selective Sorbents

    Science.gov (United States)

    Han, Chao

    The threat of oil pollution increases with the expansion of oil exploration and production activities, as well as the industrial growth around the world. Use of sorbents is a common method to deal with the oil spills. In this work, an advanced sorbent technology is described. A series of non-woven Cellulose Acetate (CA) nanofibrous mats with a 3D fibrous structure were synthesized by a novel high-throughput electrospinning technique. The precursor was solutions of CA/ acetic acid-acetone in various concentrations. Among them, 15.0% CA exhibits a superhydrophobic surface property, with a water contact angle of 128.95°. Its oil sorption capacity is many times higher the oil sorption capacity of the best commercial sorbent available in the market. Also, it showed good buoyancy properties on the water both as dry-mat and oil-saturated mat. In addition, it is biodegradable, easily available, easily manufactured, so the CA nanofibrous mat is an excellent candidate as oil sorbent for oil spill in water treatment.

  19. Crosslinked agarose encapsulated sorbents resistant to steam sterilization. Preparation and mechanical properties

    NARCIS (Netherlands)

    de Koning, H. W.; Chamuleau, R. A.; Bantjes, A.

    1984-01-01

    The application of agarose in hemoperfusion is hampered by the lack of a suitable sterilization method. A technique has been developed for the crosslinking of agarose encapsulated sorbents by the reaction with 1,3-dichloro-2-propanol (DCP) under strong alkaline conditions. A twofold molar excess of

  20. A highly efficient and selective polysilsesquioxane sorbent for heavy metal removal

    KAUST Repository

    Duan, Xiaonan

    2012-02-29

    Suited for heavy stuff: An efficient mesoporous sorbent based on a pure ethylendiamine-bridged polysilsesquioxane is presented. This material, with both a high amine loading and a high surface area, is applied for heavy metal ion removal. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Adsorption of CO2 and H2O on supported amine sorbents

    NARCIS (Netherlands)

    Veneman, Rens; Zhao, W.; Li, Z.; Cai, N.; Brilman, Derk Willem Frederik

    2014-01-01

    In this work we have evaluated the H2O and CO2 adsorption characteristics of Lewatit VP OC 1065 in view of the potential application of solid sorbents in post combustion CO2 capture. Here we present single component adsorption isotherms for H2O and CO2 as well as co-adsorption experiments. It was

  2. Mercury Removal from MSW Incineration Flue Gas by Mineral-based Sorbents.

    Czech Academy of Sciences Publication Activity Database

    Rumayor, Marta; Svoboda, Karel; Švehla, Jaroslav; Pohořelý, Michael; Šyc, Michal

    2018-01-01

    Roč. 73, DEC 13 (2018), s. 265-270 ISSN 0956-053X R&D Projects: GA TA ČR TE02000236 Institutional support: RVO:67985858 Keywords : mercury * removal * mineral sorbents Subject RIV: DI - Air Pollution ; Quality OBOR OECD: Environmental sciences (social aspects to be 5.7) Impact factor: 4.030, year: 2016

  3. Performance and Mechanism of Uranium Adsorption from Seawater to Poly(dopamine)-Inspired Sorbents.

    Science.gov (United States)

    Wu, Fengcheng; Pu, Ning; Ye, Gang; Sun, Taoxiang; Wang, Zhe; Song, Yang; Wang, Wenqing; Huo, Xiaomei; Lu, Yuexiang; Chen, Jing

    2017-04-18

    Developing facile and robust technologies for effective enrichment of uranium from seawater is of great significance for resource sustainability and environmental safety. By exploiting mussel-inspired polydopamine (PDA) chemistry, diverse types of PDA-functionalized sorbents including magnetic nanoparticle (MNP), ordered mesoporous carbon (OMC), and glass fiber carpet (GFC) were synthesized. The PDA functional layers with abundant catechol and amine/imine groups provided an excellent platform for binding to uranium. Due to the distinctive structure of PDA, the sorbents exhibited multistage kinetics which was simultaneously controlled by chemisorption and intralayer diffusion. Applying the diverse PDA-modified sorbents for enrichment of low concentration (parts per billion) uranium in laboratory-prepared solutions and unpurified seawater was fully evaluated under different scenarios: that is, by batch adsorption for MNP and OMC and by selective filtration for GFC. Moreover, high-resolution X-ray photoelectron spectroscopic and extended X-ray absorption fine structure studies were performed for probing the underlying coordination mechanism between PDA and U(VI). The catechol hydroxyls of PDA were identified as the main bidentate ligands to coordinate U(VI) at the equatorial plane. This study assessed the potential of versatile PDA chemistry for development of efficient uranium sorbents and provided new insights into the interaction mechanism between PDA and uranium.

  4. Feasibility Study of Commercial Sorbent in Coal-derived Syngas Desulfurization Field.

    Czech Academy of Sciences Publication Activity Database

    Chien, H.-Y.; Chyou, Y.-P.; Svoboda, Karel

    2015-01-01

    Roč. 6, č. 4 (2015), s. 236-242 ISSN 2078-0737 R&D Projects: GA ČR GC14-09692J Grant - others:MOST(TW) NSC 103-2923-E-042A-001 -MY3 Institutional support: RVO:67985858 Keywords : gasification * desulfurization * sorbent Subject RIV: CI - Industrial Chemistry, Chemical Engineering

  5. Using sorbent waste materials to enhance treatment of micro-point source effluents by constructed wetlands

    Science.gov (United States)

    Green, Verity; Surridge, Ben; Quinton, John; Matthews, Mike

    2014-05-01

    Sorbent materials are widely used in environmental settings as a means of enhancing pollution remediation. A key area of environmental concern is that of water pollution, including the need to treat micro-point sources of wastewater pollution, such as from caravan sites or visitor centres. Constructed wetlands (CWs) represent one means for effective treatment of wastewater from small wastewater producers, in part because they are believed to be economically viable and environmentally sustainable. Constructed wetlands have the potential to remove a range of pollutants found in wastewater, including nitrogen (N), phosphorus (P), biochemical oxygen demand (BOD) and carbon (C), whilst also reducing the total suspended solids (TSS) concentration in effluents. However, there remain particular challenges for P and N removal from wastewater in CWs, as well as the sometimes limited BOD removal within these treatment systems, particularly for micro-point sources of wastewater. It has been hypothesised that the amendment of CWs with sorbent materials can enhance their potential to treat wastewater, particularly through enhancing the removal of N and P. This paper focuses on data from batch and mesocosm studies that were conducted to identify and assess sorbent materials suitable for use within CWs. The aim in using sorbent material was to enhance the combined removal of phosphate (PO4-P) and ammonium (NH4-N). The key selection criteria for the sorbent materials were that they possess effective PO4-P, NH4-N or combined pollutant removal, come from low cost and sustainable sources, have potential for reuse, for example as a fertiliser or soil conditioner, and show limited potential for re-release of adsorbed nutrients. The sorbent materials selected for testing were alum sludge from water treatment works, ochre derived from minewater treatment, biochar derived from various feedstocks, plasterboard and zeolite. The performance of the individual sorbents was assessed through

  6. Fixing atmospheric CO2 by environment adaptive sorbent and renewable energy

    Science.gov (United States)

    Wang, T.; Liu, J.; Ge, K.; Fang, M.

    2014-12-01

    Fixing atmospheric CO2, followed by geologic storage in remote areas is considered an environmentally secure approach to climate mitigation. A moisture swing sorbent was investigated in the laboratory for CO2 capture at a remote area with humid and windy conditions. The energy requirement of moisture swing absorption could be greatly reduced compared to that of traditional high-temperature thermal swing, by assuming that the sorbent can be naturally dried and regenerated at ambient conditions. However, for currently developed moisture swing materials, the CO2 capacity would drop significantly at high relative humidity. The CO2 capture amount can be reduced by the poor thermodynamics and kinetics at high relative humidity or low temperature. Similar challenges also exist for thermal or vacuum swing sorbents. Developing sorbent materials which adapt to specific environments, such as high humidity or low temperature, can ensure sufficient capture capacity on the one hand, and realize better economics on the other hand (Figure 1) .An environment adaptive sorbent should have the abilities of tunable capacity and fast kinetics at extreme conditions, such as high humidity or low temperature. In this presentation, the possibility of tuning CO2 absorption capacity of a polymerized ionic liquid material is discussed. The energy requirement evaluation shows that tuning the CO2 binding energy of sorbent, rather than increasing the temperature or reducing the humidity of air, could be much more economic. By determining whether the absorption process is controlled by physical diffusion controlled or chemical reaction, an effective approach to fast kinetics at extreme conditions is proposed. A shrinking core model for mass transfer kinetics is modified to cope with the relatively poor kinetics of air capture. For the studied sample which has a heterogeneous structure, the kinetic analysis indicates a preference of sorbent particle size optimization, rather than support layer

  7. Lead, Chromium and Cadmium Removal from Contaminated Water Using Phosphate Sorbents

    Directory of Open Access Journals (Sweden)

    Fariborz Riahi

    2010-06-01

    Full Text Available Sorption of 3 poisonous metal ions (Pb2+, Cd2+, Cr3+ in aqueous solutions by two phosphate sorbents under dynamic and static conditions was studied. Phosphate sorbents (MgNH4PO4. H2O, Mg3(PO42. 6H2O were synthesized by known procedures. The resulting crystalline samples were analyzed for the contents of Mg2+, Pb2+, P, N using spectrophotometric and elemental analysis methods. Likewise, the amounts of Pb2+, Cd2+, Cr3+ in solutions were determined before and after the sorption process using the atomic absorption method. The relative standard deviations for Pb2+, Cd2+, Cr3+ were 4.7%, 2.17%, and 1.61% and the detection limits were 5 g/L, 0.05 mg/L, and 0.1 mg/L, respectively. The sorbents showed a high performance in the purification of contaminated solutions under static conditions. The sorption capacity levels of Mg3 (PO42. 6H2O and MgNH4 PO4. H2O were 9.8m.mol/gr and 8.9m.mol/gr for Pb2+; 10.5m.mol/gr and 9m.mol/gr for Cd2+; and 6.6m.mol/gr and 5.3m.mol/gr for Cr3+, respectively. Pb2+ , Cd2+, Cr3+. sorption by inorganic phosphate sorbents from solutions is associated with complicated chemical transformations of the sorbents. A proper account of these transformations allows for the sorption process to be optimized. The data on Pb2+, Cd2+, Cr3+ sorption under static conditions (24-h contact of Mg3 (PO42. 6H2O, MgNH4PO4. H2O, with solutions at 20oC and under dynamic conditions were obtained and the sorption behaviors of the metal ions were investigated in response to the sorbents used. It was found that Mg3 (PO42. 6H2O was the best sorbent for Pb2+, Cd2+, Cr3+ under dynamic conditions.

  8. Anticorrosive coatings: a review

    DEFF Research Database (Denmark)

    Sørensen, Per Aggerholm; Kiil, Søren; Dam-Johansen, Kim

    2009-01-01

    of volatile organic compounds (VOCs) have caused significant changes in the anticorrosive coating industry. The requirement for new VOC-compliant coating technologies means that coating manufacturers can no longer rely on the extensive track record of their time-served products to convince consumers...... and durability of anticorrosive coatings have been included. The different types of anticorrosive coatings are presented, and the most widely applied generic types of binders and pigments in anticorrosive coatings are listed and described. Furthermore, the protective mechanisms of barrier, sacrificial...

  9. Adsorption Equilibrium for Heavy Metal Divalent Ions (Cu2+, Zn2+, and Cd2+ into Zirconium-Based Ferromagnetic Sorbent

    Directory of Open Access Journals (Sweden)

    Agnes Yung Weng Lee

    2017-01-01

    Full Text Available Zirconium-based ferromagnetic sorbent was fabricated by coprecipitation of Fe2+/Fe3+ salts in a zirconium solution and explored as a potential sorbent for removing the Cu2+, Zn2+, and Cd2+ from aqueous solution. The sorbent could easily be separated from aqueous solution under the influence of external magnetic field due to the ferromagnetism property. A trimodal distribution was obtained for the sorbent with average particle size of 22.74 μm. The –OH functional groups played an important role for efficient removal of divalent ions. The surface of the sorbent was rough with abundant protuberance while the existence of divalent ions on the sorbent surface after the sorption process was demonstrated. Decontamination of the heavy metal ions was studied as a function of initial metal ions concentration and solution pH. Uptake of the heavy metal ions showed a pH-dependent profile with maximum sorption at around pH 5. The presence of the ferromagnetic sorbent in solution at different initial pH has shown a buffering effect. Equilibrium isotherms were analyzed using Langmuir, Freundlich, Dubinin-Radushkevich, and Temkin isotherm models. Adequacy of fit for the isotherm models based on evaluation of R2 and ARE has revealed that heavy metal ions decontamination was fitted well with the Freundlich model.

  10. Feeding Essential Oils and 2-Heptanone in Sugar Syrup and Protein Diets to Honey Bees (Apis mellifera L.) as Potential Varroa Mite (Varroa destructor) Controls and Traced by SPME (Solid Phase Micro Extraction) Fibers

    Science.gov (United States)

    Essential oils and oil components were fed to honey bees in a sugar syrup and liquid protein diet in order to determine if the oils were being incorporated into the bee larvae and could be traced by means of SPME. The compounds used were origanum, 2-heptanone, thymol and connamon oil. The main com...

  11. Comparative Analyses of the Volatile Components of Citrus Aurantium L. Flowers Using Ultrasonic-Assisted Headspace SPME and Hydrodistillation Combined with GC-MS and Evaluation of their Antimicrobial Activities

    Directory of Open Access Journals (Sweden)

    Akram Rahimi

    2014-12-01

    Full Text Available The volatile components of Citrus aurantium L. flowers were characterized by GC-MS with two different extraction techniques, hydrodistillation (HD and ultrasonic-assisted headspace solid phase microextraction (UA-HS-SPME. In the SPME method, the volatile components of the samples, irradiated by ultrasonic radiation, were collected on a polydimethyl siloxane (PDMS commercial fiber as well as some manually prepared nanoporous fibers from the samples headspace. To reach the better results, the extraction conditions were carefully optimized for the PDMS fiber. Under the optimized conditions (i.e. sonication time 15 min, extraction time 30 min and extraction temperature 55 ºC, 54 compounds were identified by the UA-HS-SPME-GC/MS method. The essential oil components of Citrus aurantium L. flower samples from two different regions of Iran and new and old samples from the same region were compared to one another. The major components identified for the samples with both the SPME and HD methods were linalool, linalyl acetate, limonene, β-myrcene, geranyl acetate, and neryl acetate, respectively. However, a substantial variation in the percentages of the components was identified for different samples and different extraction methods. The antimicrobial activities of the oil were also examined against six standard bacteria. There was some activity against Enterococcus fecalis, Escherichia coli, and Bacillus cereus, indicating important biological activities of the oil.

  12. Removal of metals from industrial wastewater and urban runoff by mineral and bio-based sorbents.

    Science.gov (United States)

    Gogoi, Harshita; Leiviskä, Tiina; Heiderscheidt, Elisangela; Postila, Heini; Tanskanen, Juha

    2018-03-01

    The study was performed to evaluate chemically modified biosorbents, hydrochloric acid treated peat (HCl-P) and citric acid treated sawdust (Citric acid-SD) for their metal removal capacity from dilute industrial wastewater and urban runoff and compare their efficiency with that of commercially available mineral sorbents (AQM PalPower M10 and AQM PalPower T5M5 magnetite). Batch and column experiments were conducted using real water samples to assess the sorbents' metal sorption capacity. AQM PalPower M10 (consisting mainly of magnesium, iron and silicon oxides) exhibited excellent Zn removal from both industrial wastewater and spiked runoff water samples even at low dosages (0.1 g/L and 0.05 g/L, respectively). The high degree of Zn removal was associated with the release of hydroxyl ions from the sorbent and subsequent precipitation of zinc hydroxide. The biosorbents removed Ni and Cr better than AQM PalPower M10 from industrial wastewater and performed well in removing Cr and Cu from spiked runoff water, although at higher dosages (0.3-0.75 g/L). The main mechanism of sorption by biosorbents was ion exchange. The sorbents required a short contact time to reach equilibrium (15-30 min) in both tested water samples. AQM PalPower T5M5 magnetite was the worst performing sorbent, leaching Zn into both industrial and runoff water and Ni into runoff water. Column tests revealed that both HCl-P and AQM PalPower M10 were able to remove metals, although some leaching was witnessed, especially As from AQM PalPower M10. The low hydraulic conductivity observed for HCl-P may restrict the possibilities of using such small particle size peat material in a filter-type passive system. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. A Low Cost, High Capacity Regenerable Sorbent for Pre-combustion CO{sub 2} Capture

    Energy Technology Data Exchange (ETDEWEB)

    Alptekin, Gokhan

    2012-09-30

    The overall objective of the proposed research is to develop a low cost, high capacity CO{sub 2} sorbent and demonstrate its technical and economic viability for pre-combustion CO{sub 2} capture. The specific objectives supporting our research plan were to optimize the chemical structure and physical properties of the sorbent, scale-up its production using high throughput manufacturing equipment and bulk raw materials and then evaluate its performance, first in bench-scale experiments and then in slipstream tests using actual coal-derived synthesis gas. One of the objectives of the laboratory-scale evaluations was to demonstrate the life and durability of the sorbent for over 10,000 cycles and to assess the impact of contaminants (such as sulfur) on its performance. In the field tests, our objective was to demonstrate the operation of the sorbent using actual coal-derived synthesis gas streams generated by air-blown and oxygen-blown commercial and pilot-scale coal gasifiers (the CO{sub 2} partial pressure in these gas streams is significantly different, which directly impacts the operating conditions hence the performance of the sorbent). To support the field demonstration work, TDA collaborated with Phillips 66 and Southern Company to carry out two separate field tests using actual coal-derived synthesis gas at the Wabash River IGCC Power Plant in Terre Haute, IN and the National Carbon Capture Center (NCCC) in Wilsonville, AL. In collaboration with the University of California, Irvine (UCI), a detailed engineering and economic analysis for the new CO{sub 2} capture system was also proposed to be carried out using Aspen PlusTM simulation software, and estimate its effect on the plant efficiency.

  14. Sorbent Injection for Small ESP Mercury Control in Low Sulfur Eastern Bituminous Coal Flue Gas

    Energy Technology Data Exchange (ETDEWEB)

    Carl Richardson; Katherine Dombrowski; Douglas Orr

    2006-12-31

    This project Final Report is submitted to the U.S. Department of Energy (DOE) as part of Cooperative Agreement DE-FC26-03NT41987, 'Sorbent Injection for Small ESP Mercury Control in Low Sulfur Eastern Bituminous Coal Flue Gas.' Sorbent injection technology is targeted as the primary mercury control process on plants burning low/medium sulfur bituminous coals equipped with ESP and ESP/FGD systems. About 70% of the ESPs used in the utility industry have SCAs less than 300 ft2/1000 acfm. Prior to this test program, previous sorbent injection tests had focused on large-SCA ESPs. This DOE-NETL program was designed to generate data to evaluate the performance and economic feasibility of sorbent injection for mercury control at power plants that fire bituminous coal and are configured with small-sized electrostatic precipitators and/or an ESP-flue gas desulfurization (FGD) configuration. EPRI and Southern Company were co-funders for the test program. Southern Company and Reliant Energy provided host sites for testing and technical input to the project. URS Group was the prime contractor to NETL. ADA-ES and Apogee Scientific Inc. were sub-contractors to URS and was responsible for all aspects of the sorbent injection systems design, installation and operation at the different host sites. Full-scale sorbent injection for mercury control was evaluated at three sites: Georgia Power's Plant Yates Units 1 and 2 [Georgia Power is a subsidiary of the Southern Company] and Reliant Energy's Shawville Unit 3. Georgia Power's Plant Yates Unit 1 has an existing small-SCA cold-side ESP followed by a Chiyoda CT-121 wet scrubber. Yates Unit 2 is also equipped with a small-SCA ESP and a dual flue gas conditioning system. Unit 2 has no SO2 control system. Shawville Unit 3 is equipped with two small-SCA cold-side ESPs operated in series. All ESP systems tested in this program had SCAs less than 250 ft2/1000 acfm. Short-term parametric tests were conducted on Yates

  15. Waste treatment and immobilization technologies involving inorganic sorbents. Final report of a co-ordinated research programme 1992-1996

    International Nuclear Information System (INIS)

    1997-06-01

    A Coordinated Research Programme (CRP) for the application of inorganic sorbents in liquid waste treatment and immobilization was initiated by the IAEA in 1992. The results of this CRP are presented in this report. Fifteen institutions from fourteen countries were involved in this programme. The framework of this CRP was: (1) to conduct fundamental studies on sorbent structure and sorption mechanism; (2) to obtain thermodynamic and kinetic data of the treatment process; (3) to define sorption mechanism of radionuclides on different soils; (4) to identify sorbents appropriate for treatment of liquid waste streams; (5) to develop standard tests to be able to compare results of different groups of investigations. Refs, figs, tabs

  16. Coupling of SPME with MCC/UV-IMS as a tool for rapid on-site detection of groundwater and surface water contamination

    Energy Technology Data Exchange (ETDEWEB)

    Walendzik, G.; Baumbach, J.I.; Klockow, D. [ISAS-Institute for Analytical Sciences, Dortmund (Germany)

    2005-08-01

    The combination of headspace solid phase microextraction (HS-SPME) [1] with fast chromatographic pre-separation by means of multi-capillary columns (MCC) coupled to an ion mobility spectrometer equipped with a 10.6 eV photoionisation source was applied to rapid on-site monitoring of ground and surface water contaminations. Under field conditions, water contaminants were directly detectable down to the upper {mu}g/L range. The potential of the developed method is illustrated by measurements of BTEX, naphthalene, chlorinated alkenes and chlorinated benzenes in water. Practical results from investigations of contaminated groundwater at a former gasworks site and groundwater from the site of a metal processing plant, focusing on the key substances benzene, naphthalene and tetrachloroethene, demonstrate the feasibility of the system for field studies. (orig.)

  17. Use of Polymerase Chain Reaction Enzyme Linked Oligonucleotide Sorbent Assay (Pcr-Elosa for Detection of Disease Agents

    Directory of Open Access Journals (Sweden)

    Simson Tarigan

    2016-03-01

    Full Text Available Diagnostic tool comprises one of the vital components in the control of infectious diseases. One of the most common techniques in the diagnosis of infectious disease currently available is the polymerase chain reaction (PCR because this technique is very sensitive, specific, and rapid. This technique requires an adjunct technique to indicate the formation of the right reaction product. Agarose gel electrophoresis has been the most common technique to visualise the PCR product or amplicon. Enzyme linked oligonucleotide sorbent assay (ELOSA is an alternative technique which is more sensitive and gives more important identity of the amplicon. This technique can be more than 100 times as sensitive as a gel agarose electrophoresis, and very specific since confirmation of the amplicon is carried out by DNA hibridisation. The capacity of the ELOSA can also be extended to the detection of disease-causal agent at subtype level, or detection of mutation at particular location in a gene. Since the equipment used for ELOSA is similar to that for ELISA (enzyme linked immunosorbent assay, a large number of samples can be accomplished rapidly. As in ELISA, a number of variation can be made in ELOSA depend on the requirement. Nucleotide can be immobilised on the microwell plate either by passive adsorbtion, by first conjugation of nucleotide with biotin then immobilisation on streptavidin-coated microwell plate, or immobilisaion by covalent bonding. The PCR and ELOSA can be performed at separate or in a single tube by first immobilising the PCR primers on the surface of microwell plates.

  18. European coatings conference - Marine coatings. Proceedings

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2008-07-01

    This volume contains 13 lectures (manuscripts or powerpoint foils) with the following topics: 1. Impact of containerization on polyurethane and polyurea in marine and protective coatings (Malte Homann); 2. The application of combinatorial/high-throughput methods to the development of marine coatings (Bret Chisholm); 3. Progress and perspectives in the AMBIO (advanced nanostructured surfaces for the control of biofouling) Project (James Callow); 4. Release behaviour due to shear and pull-off of silicone coatings with a thickness gradient (James G. Kohl); 5. New liquid rheology additives for high build marine coatings (Andreas Freytag); 6. Effective corrosion protection with polyaniline, polpyrrole and polythiophene as anticorrosice additives for marine paints (Carlos Aleman); 7. Potential applications of sol gel technology for marine applications (Robert Akid); 8: Performance of biocide-free Antifouling Coatings for leisure boats (Bernd Daehne); 9. Novel biocidefree nanostructured antifouling coatings - can nano do the job? (Corne Rentrop); 10. One component high solids, VOC compliant high durability finish technology (Adrian Andrews); 11. High solid coatings - the hybrid solution (Luca Prezzi); 12. Unique organofunctional silicone resins for environmentally friendly high-performance coatings (Dieter Heldmann); 13. Silicone-alkyd paints for marine applications: from battleship-grey to green (Thomas Easton).

  19. Seal coat research project

    Science.gov (United States)

    1999-12-01

    This study evaluates the use of seal coating as a method to protect bituminous pavements from oxidation, water infiltration, and raveling. The Minnesota Department of Transportation (Mn/DOT) applied seal coating to a roadway segment of Trunk Highway ...

  20. Evaluation of masonry coatings.

    Science.gov (United States)

    1969-08-01

    This report describes the evaluation of five coating systems to replace the conventional Class 2 rubbed finish now required on concrete structures. The evaluation consisted of preparing test specimens with each of the five coatings and conducting abs...

  1. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    Energy Technology Data Exchange (ETDEWEB)

    Kächele, Martin [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Hochschule Mannheim, Paul-Wittsack-Strasse 10, D-68163 Mannheim (Germany); Monakhova, Yulia B. [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Bruker Biospin GmbH, Silbersteifen, 76287 Rheinstetten (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012 Saratov (Russian Federation); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Lachenmeier, Dirk W., E-mail: lachenmeier@web.de [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Ministry of Rural Affairs and Consumer Protection, Kernerplatz 10, 70182 Stuttgart (Germany)

    2014-04-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L⁻¹. • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L⁻¹). Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L⁻¹. Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L⁻¹), followed by fruit spirits (86%, mean 591 μg/L⁻¹), tequila (86%, mean 404 μg L⁻¹), Asian spirits (43%, mean 54 μg L⁻¹) and wine (9%, mean 0.7 μg L⁻¹). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L⁻¹.

  2. Use of solid-phase microextraction (SPME) for the determination of methadone and EDDP in human hair by GC-MS.

    Science.gov (United States)

    Lucas, A C; Bermejo, A M; Tabernero, M J; Fernández, P; Strano-Rossi, S

    2000-01-10

    Solid-phase microextraction (SPME) is a new extraction technique with many advantages: small sample volume, simplicity, quickness and solvent-free. It is mainly applied to environmental analysis, but is also useful for the extraction of drugs from biological samples. In this paper the use of SPME is proposed for the determination of methadone and its main metabolite EDDP in hair by GC-MS. The hair samples were washed, cut into 1-mm segments, and incubated with Pronase E for 12 h. A 100-micron polydimethylsiloxane (PDMS) film fibre was submerged for 30 min in a diluted solution of the hydrolysis liquid (1:4 with borax buffer) containing methadone-d3 and EDDP-d3 as internal standards. Once the microextraction was concluded the fibre was directly inserted into the CG injection port. Linearity was found for methadone and EDDP in the range studied, 1.0-50 ng/mg hair, with correlation coefficients higher than 0.99. Interassay relative standard deviation (R.S.D) was determined to be less than 13.30% for methadone and less than 8.94% for EDDP, at 3.0 and 30.0 ng/mg. Analytical recoveries were close to 100% for both compounds on spiked samples. The method was applied to the analysis of real hair samples from eight patients of a methadone maintenance programme. The concentration of methadone in hair ranged from 2.45 to 78.10 ng/mg, and for EDDP from 0.98 to 7.76 ng/mg of hair.

  3. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    International Nuclear Information System (INIS)

    Kächele, Martin; Monakhova, Yulia B.; Kuballa, Thomas; Lachenmeier, Dirk W.

    2014-01-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L −1 ). • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L −1 ). - Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L −1 . Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L −1 ), followed by fruit spirits (86%, mean 591 μg/L −1 ), tequila (86%, mean 404 μg L −1 ), Asian spirits (43%, mean 54 μg L −1 ) and wine (9%, mean 0.7 μg L −1 ). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L −1

  4. Optimization of biological and instrumental detection of explosives and ignitable liquid residues including canines, SPME/ITMS and GC/MSn

    Science.gov (United States)

    Furton, Kenneth G.; Harper, Ross J.; Perr, Jeannette M.; Almirall, Jose R.

    2003-09-01

    A comprehensive study and comparison is underway using biological detectors and instrumental methods for the rapid detection of ignitable liquid residues (ILR) and high explosives. Headspace solid phase microextraction (SPME) has been demonstrated to be an effective sampling method helping to identify active odor signature chemicals used by detector dogs to locate forensic specimens as well as a rapid pre-concentration technique prior to instrumental detection. Common ignitable liquids and common military and industrial explosives have been studied including trinitrotoluene, tetryl, RDX, HMX, EGDN, PETN and nitroglycerine. This study focuses on identifying volatile odor signature chemicals present, which can be used to enhance the level and reliability of detection of ILR and explosives by canines and instrumental methods. While most instrumental methods currently in use focus on particles and on parent organic compounds, which are often involatile, characteristic volatile organics are generally also present and can be exploited to enhance detection particularly for well-concealed devices. Specific examples include the volatile odor chemicals 2-ethyl-1-hexanol and cyclohexanone, which are readily available in the headspace of the high explosive composition C-4; whereas, the active chemical cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX) is not. The analysis and identification of these headspace 'fingerprint' organics is followed by double-blind dog trials of the individual components using certified teams in an attempt to isolate and understand the target compounds to which dogs are sensitive. Studies to compare commonly used training aids with the actual target explosive have also been undertaken to determine their suitability and effectiveness. The optimization of solid phase microextraction (SPME) combined with ion trap mobility spectrometry (ITMS) and gas chromatography/mass spectrometry/mass spectrometry (GC/MSn) is detailed including interface development

  5. Magnetic solid-phase extraction based on mesoporous silica-coated magnetic nanoparticles for analysis of oral antidiabetic drugs in human plasma

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Karynne Cristina de; Andrade, Gracielle Ferreira [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil); Vasconcelos, Ingrid; Oliveira Viana, Iara Maíra de; Fernandes, Christian [Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Belo Horizonte, MG (Brazil); Martins Barros de Sousa, Edésia, E-mail: sousaem@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear, CDTN/CNEN, Rua Professor Mário Werneck, s/n. Campus Universitário, Belo Horizonte, MG CEP 30.123-970 (Brazil)

    2014-07-01

    In the present work, magnetic nanoparticles embedded into mesoporous silica were prepared in two steps: first, magnetite was synthesized by oxidation–precipitation method, and next, the magnetic nanoparticles were coated with mesoporous silica by using nonionic block copolymer surfactants as structure-directing agents. The mesoporous SiO{sub 2}-coated Fe{sub 3}O{sub 4} samples were functionalized using octadecyltrimethoxysilane as silanizing agent. The pure and functionalized silica nanoparticles were physicochemically and morphologically characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N{sub 2} adsorption, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The resultant magnetic silica nanoparticles were applied as sorbents for magnetic solid-phase extraction (MSPE) of oral antidiabetic drugs in human plasma. Our results revealed that the magnetite nanoparticles were completely coated by well-ordered mesoporous silica with free pores and stable pore walls, and that the structural and magnetic properties of the Fe{sub 3}O{sub 4} nanoparticles were preserved in the applied synthesis route. Indeed, the sorbent material was capable of extracting the antidiabetic drugs from human plasma, being useful for the sample preparation in biological matrices. - Highlights: • SBA-15/Fe{sub 3}O{sub 4} was synthesized and functionalized with octadecyltrimethoxysilane. • Magnetite nanoparticles were completely coated by well-ordered mesoporous silica. • The samples were used as sorbent for magnetic solid-phase extraction (MSPE). • The sorbent material was capable of extracting drugs from human plasma. • The extraction ability makes the material a candidate to be employed as MSPE.

  6. Bioinspired Polyelectrolyte-Assembled Graphene-Oxide-Coated C18 Composite Solid-Phase Microextraction Fibers for In Vivo Monitoring of Acidic Pharmaceuticals in Fish.

    Science.gov (United States)

    Qiu, Junlang; Chen, Guosheng; Liu, Shuqin; Zhang, Tianlang; Wu, Jiayi; Wang, Fuxin; Xu, Jianqiao; Liu, Yan; Zhu, Fang; Ouyang, Gangfeng

    2016-06-07

    A novel solid-phase microextraction (SPME) fiber was prepared by gluing poly(diallyldimethylammonium chloride) (PDDA) assembled graphene oxide (GO)-coated C18 composite particles (C18@GO@PDDA) onto a quartz fiber with polyaniline (PANI). The fiber surface coating was sequentially modified with bioinspired polynorepinephrine, which provided a smooth biointerface and makes the coating suitable for in vivo sampling. The novel custom-made coating was used to extract acidic pharmaceuticals, and high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was employed for analysis. The custom-made coating exhibited a much higher extraction efficiency than the previously used commercial polydimethylsiloxane (PDMS) and polyacrylate (PA) coatings. The custom-made coating also possessed satisfactory stability (the relative standard deviations (RSDs) ranged from 1.60% to 10.3% for six sampling-desorption cycles), interfiber reproducibility (the RSDs ranged from 2.61% to 11.5%), and resistance to matrix effects. The custom-made fibers were used to monitor the presence of acid pharmaceuticals in dorsal-epaxial muscle of living fish, and satisfactory sensitivities (limits of detection ranged from 0.13 ng/g to 7.56 ng/g) were achieved. The accuracies were verified by the comparison with liquid extraction. Moreover, the novel fibers were successfully used to monitor the presence of acidic pharmaceuticals in living fish, which demonstrated that the custom-made fibers were feasible for possible long-term in vivo continuous pharmaceutical monitoring.

  7. METHOD FOR TESTING COATINGS

    Science.gov (United States)

    Johns, I.B.; Newton, A.S.

    1958-09-01

    A method is described for detecting pin hole imperfections in coatings on uranium-metal objects. Such coated objects are contacted with a heated atmosphere of gaseous hydrogen and imperfections present in the coatings will allow the uranlum to react with the hydrogen to form uranium hydride. Since uranium hydride is less dense than uranium metal it will swell, causing enlargement of the coating defeot and rendering it visible.

  8. PIT Coating Requirements Analysis

    Energy Technology Data Exchange (ETDEWEB)

    MINTEER, D.J.

    2000-10-20

    This study identifies the applicable requirements for procurement and installation of a coating intended for tank farm valve and pump pit interior surfaces. These requirements are intended to be incorporated into project specification documents and design media. This study also evaluates previously recommended coatings and identifies requirement-compliant coating products.

  9. Ceramic with zircon coating

    Science.gov (United States)

    Wang, Hongyu (Inventor)

    2003-01-01

    An article comprises a silicon-containing substrate and a zircon coating. The article can comprise a silicon carbide/silicon (SiC/Si) substrate, a zircon (ZrSiO.sub.4) intermediate coating and an external environmental/thermal barrier coating.

  10. Coatings for laser fusion

    International Nuclear Information System (INIS)

    Lowdermilk, W.H.

    1981-01-01

    Optical coatings are used in lasers systems for fusion research to control beam propagation and reduce surface reflection losses. The performance of coatings is important in the design, reliability, energy output, and cost of the laser systems. Significant developments in coating technology are required for future lasers for fusion research and eventual power reactors

  11. PIT Coating Requirements Analysis

    International Nuclear Information System (INIS)

    MINTEER, D.J.

    2000-01-01

    This study identifies the applicable requirements for procurement and installation of a coating intended for tank farm valve and pump pit interior surfaces. These requirements are intended to be incorporated into project specification documents and design media. This study also evaluates previously recommended coatings and identifies requirement-compliant coating products

  12. Radiation-hardening coatings

    International Nuclear Information System (INIS)

    Sellmer, H.

    1989-01-01

    Lacquers and coating agents hardened by radiation have replaced conventional coating in some fields. By means of single developments (glass-fiber coating, photosensitive lacquers for films and printing plates, photoresists, additives and fillers) the latest tendencies are shown in a survey. (HP) [de

  13. Coating of graphene

    OpenAIRE

    Schneider, G.F.; Dekker, C.

    2014-01-01

    The present invention is in the field of highly crystalline graphene and coating said graphene with a layer. Said graphene may have further structures, such as nanopores, nanogaps, and nanoribbons. The coated graphene can be used for biomolecular analysis and modification, such as DNA-sequencing, as a sensor, etc. The invention therefor also relates to use of coated graphene.

  14. Development of Spheroidal Inorganic Sorbents for Treatment of Acidic Salt-Bearing Liquid Waste

    Energy Technology Data Exchange (ETDEWEB)

    Collins, J.L.

    2001-09-07

    A spheroidal composite inorganic sorbent was developed for U.S. Department of Energy-Efficient Separations and Processing Crosscutting Program (USDOE-ESP) for potential use in removing radioactive cesium isotopes from acidic high-salt waste streams such as those at Idaho National Engineering and Environmental Laboratory (INEEL). The sorbent, zirconium monohydrogen phosphate (ZrHP) embedded with fine powder of ammonium molybdophosphate (AMP), was prepared using a unique internal gelation process which can be used to make porous reproducible microspheres that are structurally strong, have a low tendency for surface erosion, and improve the flow dynamics for column operations. Both ZrHP and AMP are excellent sorbent materials and, being inorganic, are stable in high radiation fields. AMP is a very effective sorbent for removing cesium from salt-bearing waste streams for a wide range of acidity. In the pH range of 2 to 10, ZrHP is also a very effective sorbent for removing Cs, Sr, Th, U(VI), Pu(IV), Am(III), Hg, and Pb from streams of lower ionic concentrations. Crucial to developing the spheroidal AMP-ZrHP sorbent was to determine the ideal weight percentage of AMP that could be embedded in the ZrHP microspheres in order to maintain the structural integrity of the microspheres and also achieve a good cesium separation. A total of 12 preparations were made. The dry weight percentage of AMP ranged from 30 to 60. Overall, the best composite microspheres prepared contained 50% AMP (by dry weight measurement). Another composite microsphere, which was composed of titanium monohydrogen phosphate (TiHP) embedded with 18 wt % (air-dried weight) potassium cobalt hexacyanoferrate (KCoCF) and developed for a different separations application, was also batch tested for comparison. It proved to be as effective in removing,the cesium as the air-dried AMP (50 wt %)-ZrHP. Granular KCoCF was also prepared and was very effective. Large samples of each of these materials were sent to

  15. The cleaning of the soils polluted by oil and radionuclides by natural sorbents

    International Nuclear Information System (INIS)

    Farajov, M.F.; Shamilov, E.N.; Abdullayev, A.S.; Huseynov, V.I.

    2005-01-01

    Full text : Problem of environmental pollution in oil extracting areas of Absheron peninsula became the very important discussion object lately. It this areas for many years oil and well waters were flowed to environmental areas caused a lot of pools in that areas and at the result the soil and plants were polluted with oil and radionuclides. By last years researches it was revealed that amount of radium 226 oil well water contains 10 - 500 Bq/l. Sometimes amount of radium 226 in polluted soils is increasing to 2000--5000 Bq/l and at the result it is raising probability of entering radionuclides by the way of migration from ground to plants into the nutrition chain cycle. Thus the polluted areas with oil and radionuclides and also when oil spills from oil-pipes by an accident the deactivation of soils is one of the main and most actual problems. In researches for cleaning of polluted soils with radionuclides for the first time were used the phyto sorbent modified breccias forms taken from Chaildag, Gobu, and Lokbatan mud volcano areas. The mineral contain of volcano mud generally consists of clay rocks -(kaolinit, montmorillonit, zeolite, chlorite, biotit) pyrite, and i.e.[2]. The polluted soil samples were taken in Surakhani region from area with the 150 mikroroentgen per hour radiation background. The contain and amount of radionuclides were determined with the radio spectrometer P rogress - Beta - Gamma . Polluted soil samples firstly are washed by hot water and HCl solution by mixing for 3-5 hours. At the next level by adding pieced sorbent into the solution is intensively mixing by mixer and putting for sedimentation for 24 hours. After sedimentation the stiring process is repeated by adding HCl on the sediment again. The soil is stirred by water for last time. Decomposed solutions from soil are adhering and are maked with sorbent again. Thus the soil is quite cleaned from oil and radionuclides by the sorbents we offer. At the same time this sorbents may be

  16. Metallic coating of microspheres

    International Nuclear Information System (INIS)

    Meyer, S.F.

    1980-01-01

    Extremely smooth, uniform metal coatings of micrometer thicknesses on microscopic glass spheres (microspheres) are often needed as targets for inertial confinement fusion (ICF) experiments. The first part of this paper reviews those methods used successfully to provide metal coated microspheres for ICF targets, including magnetron sputtering, electro- and electroless plating, and chemical vapor pyrolysis. The second part of this paper discusses some of the critical aspects of magnetron sputter coating of microspheres, including substrate requirements, the sticking of microspheres during coating (preventing a uniform coating), and the difficulties in growing the desired dense, smooth, uniform microstructure on continuously moving spherical substrates

  17. Metallic coating of microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, S.F.

    1980-08-15

    Extremely smooth, uniform metal coatings of micrometer thicknesses on microscopic glass spheres (microspheres) are often needed as targets for inertial confinement fusion (ICF) experiments. The first part of this paper reviews those methods used successfully to provide metal coated microspheres for ICF targets, including magnetron sputtering, electro- and electroless plating, and chemical vapor pyrolysis. The second part of this paper discusses some of the critical aspects of magnetron sputter coating of microspheres, including substrate requirements, the sticking of microspheres during coating (preventing a uniform coating), and the difficulties in growing the desired dense, smooth, uniform microstructure on continuously moving spherical substrates.

  18. ATHENA optimized coating design

    DEFF Research Database (Denmark)

    Ferreira, Desiree Della Monica; Christensen, Finn Erland; Jakobsen, Anders Clemen

    2012-01-01

    The optimization of coating design for the ATHENA mission si described and the possibility of increasing the telescope effective area in the range between 0.1 and 10 keV is investigated. An independent computation of the on-axis effective area based on the mirror design of ATHENA is performed...... in order to review the current coating baseline. The performance of several material combinations, considering a simple bi-layer, simple multilayer and linear graded multilayer coatings are tested and simulation of the mirror performance considering both the optimized coating design and the coating...

  19. Antibacterial polymer coatings.

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Mollye C.; Allen, Ashley N.; Barnhart, Meghan; Tucker, Mark David; Hibbs, Michael R.

    2009-09-01

    A series of poly(sulfone)s with quaternary ammonium groups and another series with aldehyde groups are synthesized and tested for biocidal activity against vegetative bacteria and spores, respectively. The polymers are sprayed onto substrates as coatings which are then exposed to aqueous suspensions of organisms. The coatings are inherently biocidal and do not release any agents into the environment. The coatings adhere well to both glass and CARC-coated coupons and they exhibit significant biotoxicity. The most effective quaternary ammonium polymers kills 99.9% of both gram negative and gram positive bacteria and the best aldehyde coating kills 81% of the spores on its surface.

  20. Effect of precursor and preparation method on manganese based activated carbon sorbents for removing H2S from hot coal gas.

    Science.gov (United States)

    Wang, Jiancheng; Qiu, Biao; Han, Lina; Feng, Gang; Hu, Yongfeng; Chang, Liping; Bao, Weiren

    2012-04-30

    Activated carbon (AC) supported manganese oxide sorbents were prepared by the supercritical water impregnation (SCWI) using two different precursor of Mn(NO(3))(2) (SCW(N)) and Mn(Ac)(2)·4H(2)O (SCW(A)). Their capacities of removing H(2)S from coal gas were evaluated and compared to the sorbents prepared by the pore volume impregnation (PVI) method. The structure and composition of different sorbents were characterized by XRD, SEM, TEM, XPS and XANES techniques. It is found that the precursor of active component plays the crucial role and SCW(N) sorbents show much better sulfidation performance than the SCW(A) sorbents. This is because the Mn(3)O(4) active phase of the SCW(N) sorbents are well dispersed on the AC support, while the Mn(2)SiO(4)-like species in the SCW(A) sorbent can be formed and seriously aggregated. The SCW(N) sorbents with 2.80% and 5.60% manganese are favorable for the sulfidation reaction, since the Mn species are better dispersed on the SCW(N) sorbents than those on the PV(N) sorbents and results in the better sulfidation performance of the SCW(N) sorbents. As the Mn content increases to 11.20%, the metal oxide particles on AC supports aggregate seriously, which leads to poorer sulfidation performance of the SCW(N)11.20% sorbents than that of the PV(N)11.20% sorbents. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Evaluation of HVOF coatings

    Directory of Open Access Journals (Sweden)

    Mariana Landová

    2016-07-01

    Full Text Available Attention in this paper is devoted to the evaluation of wear coatings deposited using HVOF technology (high velocity oxy-fuel. There were evaluated three types of coatings based on WC-Co (next only 1343, WC-Co-Cr (next only 1350 and Cr3C2-25NiCr (next only 1375. There was assessed adherence of coatings, micro hardness, porosity and the tribological properties of erosive, abrasive, adhesive and wear resistance of coatings in terms of cyclic thermal load. Thanks to wide variety of suitable materials and their combinations, the area of utilization thermally sprayed coatings is very broad. It is possible to deposit coatings of various materials from pure metals to special alloys. The best results in the evaluated properties were achieved at the coating with the label 1375.

  2. Concentration and immobilization of 137Cs from liquid radioactive waste using sorbents based on hydrated titanium and zirconium oxides

    Science.gov (United States)

    Voronina, A. V.; Noskova, A. Y.; Gritskevich, E. Y.; Mashkovtsev, M. A.; Semenishchev, V. S.

    2017-09-01

    The possibility of use of sorbents based on hydrated titanium and zirconium oxides (T-3A, T-35, NPF-HTD) for concentration and immobilization of 137Cs from liquid radioactive waste of various chemical composition (fresh water, seawater, solutions containing NaNO3, ammonium acetate, EDTA) was evaluated. It was shown that the NPF-HTD and T-35 sorbents separate 137Cs from fresh water and seawater with distribution coefficients as high as 6.2.104 and 6.1.104, 4.0.105 and 1.6.105 L kg-1 respectively; in 1 M ammonium acetate these values were 2.0.103 and 1.0.103 L kg-1. The NPF-HTD sorbent showed the highest selectivity for cesium in NaNO3 solution: cesium distribution coefficients in 1M NaNO3 was 1.4.106 L kg-1. All studied sorbents are suitable for deactivation of solutions containing EDTA. Cesium distribution coefficients were around 102-103 L kg-1 depending on EDTA concentration. Chemical stability of the sorbents was also studied. It was shown that 137Cs leaching rate from all sorbents meet the requirements for matrix materials.

  3. Polyurethane foams containing residues of petroleum industry catalysts as recoverable pH-sensitive sorbents for aqueous pesticides.

    Science.gov (United States)

    Almeida, Marys Lene B; Ayres, Eliane; Moura, Flávia Cristina C; Oréfice, Rodrigo L

    2018-03-15

    To investigate ways of mitigating the contamination of water with herbicides, which is a well-recognized global problem, we prepared natural resource-based polyurethane foams containing different amounts of petroleum industry catalyst residue (RC) and tested them as atrazine (ATZ, a common herbicide) sorbents in aqueous solutions. The above sorbents were characterized by infrared spectroscopy, electron microscopy, microtomography, thermogravimetric analysis, and X-ray diffraction. The adsorption/desorption of ATZ thereon was investigated as a function of foam composition, pH, initial ATZ concentration, and time. The obtained results showed that the porosity, pore size, and pore interconnectivity of the prepared sorbents were well suited for optimal ATZ removal. At pH 2, foams with high RC contents achieved higher ATZ removal efficiencies (e.g., 25%) than the pristine foam (12%). Conversely, ATZ removal was disfavored at high pH, which was attributed to restricted ATZ-sorbent interactions due to changes in the sorbent surface charge. The presence of other species (such as pectin, which is usually found in fruits) did not interfere with ATZ removal. ATZ desorption was most effective at high pH, enabling the regeneration and re-use of sorbents and thus reducing large-scale application costs. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Removal of sulfuric acid mist from lead-acid battery plants by coal fly ash-based sorbents.

    Science.gov (United States)

    Shu, Yuehong; Wei, Xiangyu; Fang, Yu; Lan, Bingyan; Chen, Hongyu

    2015-04-09

    Sorbents from coal fly ash (CFA) activated by NaOH, CaO and H2O were prepared for H2SO4 mist removal from lead-acid battery plants. The effects of parameters including temperature, time, the ratios of CFA/activator and water/solid during sorbent preparation were investigated. It is found that the synthesized sorbents exhibit much higher removal capacity for H2SO4 mist when compared with that of raw coal fly ash and CaO except for H2O activated sorbent and this sorbent was hence excluded from the study because of its low capacity. The H2SO4 mist removal efficiency increases with the increasing of preparation time length and temperature. In addition, the ratios of CFA/activator and water/solid also impact the removal efficiency, and the optimum preparation conditions are identified as: a water/solid ratio of 10:1 at 120 °C for 10h, a CFA:CaO weight ratio of 10:1, and a NaOH solution concentration of 3 mol/L. The formation of rough surface structure and an increased surface area after NaOH/CaO activation favor the sorption of H2SO4 mist and possible sorption mechanisms might be electrostatic attractions and chemical precipitation between the surface of sorbents and H2SO4 mist. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Concerns regarding 24-h sampling for formaldehyde, acetaldehyde, and acrolein using 2,4-dinitrophenylhydrazine (DNPH)-coated solid sorbents

    Science.gov (United States)

    Herrington, Jason S.; Hays, Michael D.

    2012-08-01

    There is high demand for accurate and reliable airborne carbonyl measurement methods due to the human and environmental health impacts of carbonyls and their effects on atmospheric chemistry. Standardized 2,4-dinitrophenylhydrazine (DNPH)-based sampling methods are frequently applied for measuring gaseous carbonyls in the atmospheric environment. However, there are multiple short-comings associated with these methods that detract from an accurate understanding of carbonyl-related exposure, health effects, and atmospheric chemistry. The purpose of this brief technical communication is to highlight these method challenges and their influence on national ambient monitoring networks, and to provide a logical path forward for accurate carbonyl measurement. This manuscript focuses on three specific carbonyl compounds of high toxicological interest—formaldehyde, acetaldehyde, and acrolein. Further method testing and development, the revision of standardized methods, and the plausibility of introducing novel technology for these carbonyls are considered elements of the path forward. The consolidation of this information is important because it seems clear that carbonyl data produced utilizing DNPH-based methods are being reported without acknowledgment of the method short-comings or how to best address them.

  6. Use of synthetic zeolites and other inorganic sorbents for the removal of radionuclides from aqueous wastes

    International Nuclear Information System (INIS)

    Samantha, S.K.; Singh, I.J.; Jain, S.; Sathi, S.; Venkatesan, K.; Ramaswamy, M.; Theyyunni, T.K.; Siddiqui, H.R.

    1997-01-01

    Several synthetic zeolites and inorganic sorbents were tested in the laboratory for the sorption of various radionuclides present in radioactive aqueous waste streams originating from nuclear installations. The sorption of the critical radionuclides like 137 Cs, 90 Sr and 60 Co from level waste solutions was studied using the synthetic zeolites 4A, 13X and AR1 of Indian origin. Granulated forms of ammonium molybdophosphate and CaSO 4 -BaSO 4 eutectoid were tested for the sorption of cesium and strontium respectively, from acidic solutions. The removal of radiostrontium from alkaline salt-loaded intermediate level reprocessing wastes was studied using hydrous ferric oxide-activated carbon composite sorbent, hydrous titania and hydrous manganese dioxide.. The results of these investigations are expected to be of value in formulating radioactive waste treatment schemes for achieving high decontamination and volume reduction factors. (author). 12 refs, 5 figs, 18 tabs

  7. An international multi-laboratory investigation of carbon-based hydrogen sorbent materials

    Science.gov (United States)

    Hurst, Katherine E.; Parilla, Philip A.; O'Neill, Kevin J.; Gennett, Thomas

    2016-01-01

    New materials are needed to achieve the hydrogen storage targets set out by the US Department of Energy for fuel cell vehicular applications. In order to enable the pathway toward this discovery, precise and accurate characterization of the hydrogen storage performance of these materials is needed. Determining the precise and accurate hydrogen storage capacity of materials requires rigorous attention to detailed experimental parameters and methodology. Slight errors in even small experimental details can result in a large deviation in the determination of the material's true characteristics. Here, we compare measurements of the gravimetric excess hydrogen uptake capacities for two different carbon sorbent materials measured by different laboratories at ambient and liquid N2 temperatures. The participants for this study consist of research laboratories led by experienced scientists in the hydrogen storage field. This collaborative evaluation of standard sorbents illustrated considerable reproducibility over a broad range of materials' hydrogen sorption gravimetric capacities.

  8. Microbial stabilization of sulfur-landen sorbents; Technical report, September 1--November 30, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Miller, K.W. [Illinois State Univ., Normal, IL (United States)

    1993-12-31

    Clean coal technologies that involve limestone for sulfur capture generate lime/limestone products laden with sulfur at various oxidation states. If sulfur is completely stabilized as sulfate, the spent sorbent is ready for commercial utilization as gypsum. However, the presence of reduced sulfur species requires additional processing. Thermal oxidation of reduced sulfur can result in undesirable release of SO{sub 2}. Microbial oxidation might provide an inexpensive and effective alternative. Sorbents laden with reduced forms of sulfur such as sulfide, sulfite, or various polythionate species serve as growth substrates for sulfur-oxidizing bacteria, which have the potential to convert all sulfur to sulfate. This quarter, efforts focused on determining the combined effects of dibasic acids (DBA) and Ca{sup +2} concentration on several strains of neutrophilic thiobacilli, including Thiobacillus neapolitanus ATCC 23639 and ATCC 23641, and an isolate, TQ1, which was obtained from a commercial sulfur dioxide scrubber that utilizes DBA.

  9. Successful experience with limestone and other sorbents for combustion of biomass in fluid bed power boilers

    Energy Technology Data Exchange (ETDEWEB)

    Coe, D.R. [LG& E Power Systems, Inc., Irvine, CA (United States)

    1993-12-31

    This paper presents the theoretical and practical advantages of utilizing limestone and other sorbents during the combustion of various biomass fuels for the reduction of corrosion and erosion of boiler fireside tubing and refractory. Successful experiences using a small amount of limestone, dolomite, kaolin, or custom blends of aluminum and magnesium compounds in fluid bed boilers fired with biomass fuels will be discussed. Electric power boiler firing experience includes bubbling bed boilers as well as circulating fluid bed boilers in commercial service on biomass fuels. Forest sources of biomass fuels fired include wood chips, brush chips, sawmill waste wood, bark, and hog fuel. Agricultural sources of biomass fuels fired include grape vine prunings, bean straw, almond tree chips, walnut tree chips, and a variety of other agricultural waste fuels. Additionally, some urban sources of wood fuels have been commercially burned with the addition of limestone. Data presented includes qualitative and quantitative analyses of fuel, sorbent, and ash.

  10. Sorption of uranium(VI) by La-Al-carboxymethyl konjac glucomannan microsphere sorbent

    International Nuclear Information System (INIS)

    Siyao Sun; Liping Wu; Xuegang Luo

    2017-01-01

    The microsphere of carboxymethyl konjac glucomannan immobilizing La 3+ and Al 3+ (CMKGM-La-Al) has been explored for sorption of U(VI). The maximum U(VI) sorption capacity of the microsphere is found to be 45.4 mg g -1 at pH 5. Experimental data are fitted well with the linear Langmuir and linear pseudo-first-order kinetic model. The sorption process is endothermic, spontaneous and favorable. The possible mechanism of CMKGM modification and sorption of U(VI) on CMKGM-La-Al involves ion exchange and coordination reaction. The comparison between CMKGM-La-Al and other sorbents suggests that CMKGM-La-Al can be considered as an effective sorbent for U(VI) sorption. (author)

  11. Development of a fiber coating based on molecular sol-gel imprinting technology for selective solid-phase micro extraction of caffeine from human serum and determination by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Rajabi Khorrami, Afshin; Rashidpur, Amene

    2012-05-21

    In this work, a molecular sol-gel imprinting approach has been introduced to produce a fiber coating for selective direct immersion solid-phase microextraction (SPME) of caffeine. The polymerization mixture was composed of vinyl trimethoxysilane and methacrylic acid as vinyl sol-gel precursor and functional monomer, respectively. Caffeine was used as template molecule during polymerization process. The prepared fibers could be coupled directly to gas chromatography/mass spectrometry (GC/MS) and used for trace analysis of caffeine in a complex sample such as human serum. The parameters influencing SPME such as time, temperature and stirring speed were optimized. The prepared coating showed good selectivity towards caffeine in the presence of some structurally related compounds. Also, it offered high imprinting capability in comparison to bare fiber and non-imprinted coating. Linear range for caffeine detection was 1-80 μg mL(-1) and the limit of detection was 0.1 μg mL(-1). The intra-day and inter-day precisions of the peak areas for five replicates were 10 and 16%, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Hot Coal Gas Desulfurization with manganese based sorbents. Quarterly report, August 1, 1993--September 30, 1993

    Energy Technology Data Exchange (ETDEWEB)

    Hepworth, M.T.

    1993-10-01

    The focus of work being performed on Hot Coal Gas Desulfurization at the Morgantown Energy Technology Center is primarily in the use of zinc ferrite and zinc titanate sorbents; however, prior studies at the US Steel Fundamental Research Laboratories in Monroeville, PA, by E. T. Turkdogan indicated that an alternate sorbent, manganese dioxide-containing ore in mixture with alumina (75 wt % ore + 25 wt % Al{sub 2}O{sub 3}) may be a viable alternative to zinc-based sorbents. Manganese, for example, has a lower vapor pressure in the elemental state than zinc hence it is not as likely to undergo depletion from the sorbent surface upon loading and regeneration cycles. Also manganese oxide is less readily reduced to the elemental state than iron hence the range of reduction potentials for oxygen is somewhat greater than for zinc ferrite. In addition, thermodynamic analysis of the manganese-oxygen-sulfur system shows it to be less amenable to sulfation than zinc ferrite. Potential also exists for utilization of manganese at higher temperatures than zinc ferrite or zinc titanate. This report documents progress in pelletizing and testing via thermogravimetric analysis of individual pellet formulations of manganese ore/alumina combinations and also manganese carbonate/alumina with two binders, dextrin and bentonite. Preliminary results indicate that the manganese carbonate material, being of higher purity than the manganese ore, has a higher degree of sulfur capacity and more rapid absorption kinetics. A 2-inch fixed-bed reactor has been fabricated and is now ready for subjecting pellets to cyclic loading and regeneration.

  13. Hot coal gas desulfurization with manganese-based sorbents. Annual report, September 1992--September 1993

    Energy Technology Data Exchange (ETDEWEB)

    Hepworth, M.T.

    1993-12-01

    The focus of work being performed on Hot Coal Gas Desulfurization at the Morgantown Energy Technology Center is primarily in the use of zinc ferrite and zinc titanate sorbents; however, prior studies at the US Steel Fundamental Research Laboratories in Monroeville, PA, by E. T. Turkdogan indicated that an alternate sorbent, manganese dioxide-containing ore in mixture with alumina (75 wt % ore + 25 wt % Al{sub 2}O{sub 3}) may be a viable alternative to zinc-based sorbents. Manganese, for example, has a lower vapor pressure in the elemental state than zinc hence it is not as likely to undergo depletion from the sorbent surface upon loading and regeneration cycles. Also manganese oxide is less readily reduced to the elemental state than iron hence the range of reduction potentials for oxygen is somewhat greater than for zinc ferrite. In addition, thermodynamic analysis of the manganese-oxygen-sulfur system shows it to be less amenable to sulfation than zinc ferrite. Potential also exists for utilization of manganese at higher temperatures than zinc ferrite or zinc titanate. This Annual Topical Report documents progress in pelletizing and testing via thermo-gravimetric analysis of individual pellet formulations of manganese ore/ alumina combinations and also manganese carbonate/alumina with two binders, dextrin and bentonite. It includes the prior Quarterly Technical Reports which indicate that the manganese carbonate material, being of higher purity than the manganese ore, has a higher degree of sulfur capacity and more rapid absorption kinetics. A 2-inch fixed-bed reactor has been fabricated and is now ready for subjecting pellets to cyclic loading and regeneration.

  14. Efficient Theoretical Screening of Solid Sorbents for CO2 Capture Applications*

    Energy Technology Data Exchange (ETDEWEB)

    Duan, Yuhua; Luebke, David; Pennline, Henry

    2012-03-31

    By combining thermodynamic database mining with first principles density functional theory and phonon lattice dynamics calculations, a theoretical screening methodology to identify the most promising CO2 sorbent candidates from the vast array of possible solid materials has been proposed and validated. The ab initio thermodynamic technique has the advantage of allowing identification of thermodynamic properties of CO2 capture reactions without any experimental input beyond crystallographic structural information of the solid phases involved. For a given solid, the first step is to attempt to extract thermodynamic properties from thermodynamic databases and the available literatures. If the thermodynamic properties of the compound of interest are unknown, an ab initio thermodynamic approach is used to calculate them. These properties expressed conveniently as chemical potentials and heat of reactions, which obtained either from databases or from calculations, are further used for computing the thermodynamic reaction equilibrium properties of the CO2 absorption/desorption cycles. Only those solid materials for which lower capture energy costs are predicted at the desired process conditions are selected as CO2 sorbent candidates and are further considered for experimental validations. Solid sorbents containing alkali and alkaline earth metals have been reported in several previous studies to be good candidates for CO2 sorbent applications due to their high CO2 absorption capacity at moderate working temperatures. In addition to introducing our computational screening procedure, in this presentation we will summarize our results for solid systems composed by alkali and alkaline earth metal oxides, hydroxides, and carbon- ates/bicarbonates to validate our methodology. Additionally, applications of our computational method to mixed solid systems of Li2O with SiO2/ZrO2 with different mixing ratios, our preliminary results showed that increasing the Li2O/SiO2 ratio in

  15. In vitro catheter and sorbent-based method for clearance of radiocontrast material during cerebral interventions

    Energy Technology Data Exchange (ETDEWEB)

    Angheloiu, George O., E-mail: goangheloiu@drmc.org [Heart and Vascular Institute, University of Pittsburgh Medical Center, Pittsburgh, PA (United States); Department of Cardiology, Dubois Regional Medical Center, Dubois, PA (United States); Hänscheid, Heribert; Reiners, Christoph [Department of Nuclear Medicine, University of Würzburg, Würzburg (Germany); Anderson, William D. [Cardiology Department, Exempla Healthcare, Denver, CO (United States); Kellum, John A. [CRISMA Center, Department of Critical Care Medicine, University of Pittsburgh Medical Center, Pittsburgh, PA (United States)

    2013-07-15

    Background: Contrast-induced acute kidney injury is a severe condition resulting from the use of radiology contrast in patients with predisposing factors. Hypothesis: We hypothesized that a novel system including a device containing polymer resin sorbent beads and a custom-made suctioning catheter could efficiently remove contrast from an in vitro novel model of circulatory system (MOCS) mimicking the cerebral circulation. Methods: A custom-made catheter was built and optimized for cerebral venous approach. The efficiency of a system made of a polymer resin sorbent beads column (CST 401, Cytosorbents) and this particular catheter was tested in the MOCS running a solution composed of 0.9% saline and radio-contrast. During two series of 18 cycles of first-pass experiments we assessed the catheter's suctioning efficiency and the system's ability to clear radio-contrast injected into the MOCS's cerebral arterial segment. We also assessed the functioning and reliability of the MOCS. Results: Mean suctioning efficiency of the catheter was 84% ± 24%. The polymer sorbent column contrast removal rate was initially 96% and gradually decreased with subsequent cycles in a linear fashion during an experiment lasting approximately 90 minutes. The MOCS had a reliability of 0.9946×min{sup −1} where 1 × min{sup −1} was the optimum value. Conclusion: A system including a polymer resin sorbent beads column and a custom-made suctioning catheter had an excellent initial efficiency in quickly removing contrast from an artificial MOCS mimicking the cerebral circulation. MOCS is an inexpensive and relatively reliable custom-made system that can be used for training or testing purposes.

  16. In vitro catheter and sorbent-based method for clearance of radiocontrast material during cerebral interventions

    International Nuclear Information System (INIS)

    Angheloiu, George O.; Hänscheid, Heribert; Reiners, Christoph; Anderson, William D.; Kellum, John A.

    2013-01-01

    Background: Contrast-induced acute kidney injury is a severe condition resulting from the use of radiology contrast in patients with predisposing factors. Hypothesis: We hypothesized that a novel system including a device containing polymer resin sorbent beads and a custom-made suctioning catheter could efficiently remove contrast from an in vitro novel model of circulatory system (MOCS) mimicking the cerebral circulation. Methods: A custom-made catheter was built and optimized for cerebral venous approach. The efficiency of a system made of a polymer resin sorbent beads column (CST 401, Cytosorbents) and this particular catheter was tested in the MOCS running a solution composed of 0.9% saline and radio-contrast. During two series of 18 cycles of first-pass experiments we assessed the catheter's suctioning efficiency and the system's ability to clear radio-contrast injected into the MOCS's cerebral arterial segment. We also assessed the functioning and reliability of the MOCS. Results: Mean suctioning efficiency of the catheter was 84% ± 24%. The polymer sorbent column contrast removal rate was initially 96% and gradually decreased with subsequent cycles in a linear fashion during an experiment lasting approximately 90 minutes. The MOCS had a reliability of 0.9946×min −1 where 1 × min −1 was the optimum value. Conclusion: A system including a polymer resin sorbent beads column and a custom-made suctioning catheter had an excellent initial efficiency in quickly removing contrast from an artificial MOCS mimicking the cerebral circulation. MOCS is an inexpensive and relatively reliable custom-made system that can be used for training or testing purposes

  17. Seawater uranium sorbents: preparation from a mesoporous copolymer initiator by atom-transfer radical polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Yue, Yanfeng; Mayes, Richard T.; Fulvio, Pasquale F.; Sun, Xiao-Guang [Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Kim, Jungseung; Tsouris, Costas [Energy and Transportation Science Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Chen, Jihua [Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Brown, Suree [Department of Chemistry, University of Tennessee, Knoxville, TN (United States); Dai, Sheng [Chemical Sciences Division, Oak Ridge National Laboratory, Oak Ridge, TN (United States); Department of Chemistry, University of Tennessee, Knoxville, TN (United States)

    2013-12-09

    Nanoporous template-free initiators for atom-transfer radical polymerization (ATRP) were synthesized with surface and framework initiator sites and tailorable pore structures. Polyacrylonitrile grown on one initiator was converted into polyamidoxime to generate a uranium sorbent for seawater extraction with a high uptake rate and capacity relative to those of nonwoven irradiation-grafted polyethylene-fiber composites. (Copyright copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. Biological – chemical regeneration of desulphurization sorbents based on zinc ferrite

    Directory of Open Access Journals (Sweden)

    Šepelák Vladimír

    2002-03-01

    Full Text Available One of the main sources of air pollution is the combustion of fuels by various thermal and power plants, transport facilities, and metallurgical plants. Main components of industrial gases that pollute air are carbon oxides, nitrogen oxides, sulphur oxides and hydrogen sulphide. Sulphur has received a more attention than any other contaminant, because the sulphur released into the atmosphere in the form of sulphur dioxide or hydrogen sulphide is a precursor of the “acid rain” formation. To meet environmental emission regulations, sulphur and other contaminant species released during the gasification of coal must be removed from the fuel gas stream. The removal of contaminat at high temperatures is referred to as hot-gas cleanup in general and hot-gas desulphurization in particular when sulphur species are the primary contaminants to be remove. In recent years, zinc ferrite is the leading candidate for hot-gas desulphurization, capable of removing sulphur-containing species from coal gas at gasifier exit temperatures. It can also be of being regenerated for a continuous use. The conventional methods of the regeneration of sulphurized sorbents are based on oxidizing pyrolysis of sulphides or on the pressure leaching of sulphides in the water environment at high temperatures. The first results of the experiments using the biological-chemical leaching, as a new way of regeneration of sulphurized sorbent based on zinc ferrite, are presented in this paper. The results show that the biological-chemical leaching leads to the removal of sulphides layers (á-ZnS, â-ZnS from the surface of the sorbent at room temperature. The biological-chemical leaching process results in the increase of the active surface area of the regenerated sorbent.

  19. Prototype demonstration of dual sorbent injection for acid gas control on municipal solid waste combustion units

    Energy Technology Data Exchange (ETDEWEB)

    None

    1994-05-01

    This report gathered and evaluated emissions and operations data associated with furnace injection of dry hydrated lime and duct injection of dry sodium bicarbonate at a commercial, 1500 ton per day, waste-to-energy facility. The information compiled during the project sheds light on these sorbents to affect acid gas emissions from municipal solid waste combustors. The information assesses the capability of these systems to meet the 1990 Clean Air Act and 1991 EPA Emission Guidelines.

  20. Options DGA sorbents application for the separation of Pu and Am in radiochemical analyzes

    International Nuclear Information System (INIS)

    Galanda, D.; Matel, L.; Dulanska, S.; Kovac, P.

    2011-01-01

    In this presentation authors present the results of the experiments using a relatively new extraction material with the trade name of the company Eichrom DGA, whose properties were studied in different environments acids HCl and HNO 3 . It has been observed and the potential possibilities of sorbent DGA in combination with other extraction materials. On the basis of these experiments was designed and tuned separation procedure for concentration Pu and Am in the samples from nuclear power plants.

  1. Extractive fixed-site polymer sorbent for selective boron removal from natural water.

    Science.gov (United States)

    Thakur, Neha; Kumar, Sanjukta A; Shinde, Rakesh N; Pandey, Ashok K; Kumar, Sangita D; Reddy, A V R

    2013-09-15

    Water contamination by boron is a widespread environmental problem. The World Health Organization (WHO) recommends maximum boron concentration of 2.4 mg L(-1) for drinking water. The paper presents a simple method for preparation of functionalized sheet sorbent for selective extraction of boron from natural water. The pores of commercially available poly(propylene) membrane were functionalized by room temperature in situ crosslinking of poly(vinylbenzyl chloride) with a cyclic diamine piperazine. The precursor membranes were chemically modified with N-methyl D-glucamine which is selective for boron. Characterization of membrane was carried out using scanning electron microscopy (SEM) and attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) techniques. The functionalized membrane has been characterized in terms of parameters that influence the sorption of boron from aqueous streams like pH, uptake capacity, contact time, effects of competing ions and reusability. The maximum boron sorption capacity determined experimentally was 28 mg g(-1). The studies showed that trace concentrations of boron were quantitatively removed from water at neutral pH. The developed fixed site polymer sorbent exhibited high sorption capacity and fast kinetics as compared to various sorbents reported in literature. It was successfully applied for the removal of boron from ground water and seawater samples in presence of high concentration of interfering ions. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Cesium removal demonstration utilizing crystalline silicotitanate sorbent for processing Melton Valley Storage Tank supernate: Final report

    International Nuclear Information System (INIS)

    Walker, J.F. Jr.; Taylor, P.A.; Cummins, R.L.

    1998-03-01

    This report provides details of the Cesium Removal Demonstration (CsRD), which was conducted at Oak Ridge National Laboratory (ORNL) on radioactive waste from the Melton Valley Storage Tanks. The CsRD was the first large-scale use of state-of-the-art sorbents being developed by private industry for the selective removal of cesium and other radionuclides from liquid wastes stored across the DOE complex. The crystalline silicotitanate sorbent used in the demonstration was chosen because of its effectiveness in laboratory tests using bench-scale columns. The demonstration showed that the cesium could be removed from the supernate and concentrated on a small-volume, solid waste form that would meet the waste acceptance criteria for the Nevada Test Site. During this project, the CsRD system processed > 115,000 L (30,000 gal) of radioactive supernate with minimal operational problems. Sluicing, drying, and remote transportation of the sorbent, which could not be done on a bench scale, were successfully demonstrated. The system was then decontaminated to the extent that it could be contact maintained with the use of localized shielding only. By utilizing a modular, transportable design and placement within existing facilities, the system can be transferred to different sites for reuse. The initial unit has now been removed from the process building and is presently being reinstalled for use in baseline operations at ORNL

  3. Removal of dioxouran (VI) cations from aqueous solution by natural sorbents

    Science.gov (United States)

    Naumova, Lyudmila; Gorlenko, Nikolai; Sarkisov, Yurii; Tsvetkov, Nikolai; Shepelenko, Tat'yana; Chukhlomina, Lyudmila

    2017-01-01

    The paper presents investigations of the mechanism of UO22+ cation sorption by natural zeolites and peat from aqueous solutions using a limited volume method. It is proved that the sorption rate depends on sorbent granulating, dioxouran (VI) temperature and concentration. The results show that sorption of UO22+ cations by natural sorbents is the mixed-diffusional mechanism. The use of 24-hour interruption technique (`kinetic memory') demonstrates that in the mixed-diffusional mechanism for natural peat and zeolites the internal ion diffusion predominates. The coefficients of internal diffusion and activation energy are calculated in this paper. The infrared spectroscopy technique and synchronous thermal test are used to identify the interaction between dioxouran (VI) and energy components of natural sorbents. The synchronous thermal test shows that UO22+ cation sorption decreases the thermal stability of peat as compared to its original state. The peat decomposition is determined after UO22+ cation removal as well as the appearance of end-effect maximum of 777.5°C. An assumption is made on a possible decomposition of different metal oxalates in peat and clay peat bonds which irreversibly absorb UO22+ cations. These research findings can be recommended for water purification at nuclear fuel cycle facility.

  4. The role of graphene-based sorbents in modern sample preparation techniques.

    Science.gov (United States)

    de Toffoli, Ana Lúcia; Maciel, Edvaldo Vasconcelos Soares; Fumes, Bruno Henrique; Lanças, Fernando Mauro

    2018-01-01

    The application of graphene-based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene-based material, their properties, synthesis routes, and the most important applications in both off-line and on-line sample preparation techniques. The discussion of the off-line approaches includes methods derived from conventional solid-phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on-line approaches focus on the use of graphene-based material mainly in on-line solid phase extraction, its variation called in-tube solid-phase microextraction, and on-line microdialysis systems. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Cesium removal demonstration utilizing crystalline silicotitanate sorbent for processing Melton Valley Storage Tank supernate: Final report

    Energy Technology Data Exchange (ETDEWEB)

    Walker, J.F. Jr.; Taylor, P.A.; Cummins, R.L. [and others

    1998-03-01

    This report provides details of the Cesium Removal Demonstration (CsRD), which was conducted at Oak Ridge National Laboratory (ORNL) on radioactive waste from the Melton Valley Storage Tanks. The CsRD was the first large-scale use of state-of-the-art sorbents being developed by private industry for the selective removal of cesium and other radionuclides from liquid wastes stored across the DOE complex. The crystalline silicotitanate sorbent used in the demonstration was chosen because of its effectiveness in laboratory tests using bench-scale columns. The demonstration showed that the cesium could be removed from the supernate and concentrated on a small-volume, solid waste form that would meet the waste acceptance criteria for the Nevada Test Site. During this project, the CsRD system processed > 115,000 L (30,000 gal) of radioactive supernate with minimal operational problems. Sluicing, drying, and remote transportation of the sorbent, which could not be done on a bench scale, were successfully demonstrated. The system was then decontaminated to the extent that it could be contact maintained with the use of localized shielding only. By utilizing a modular, transportable design and placement within existing facilities, the system can be transferred to different sites for reuse. The initial unit has now been removed from the process building and is presently being reinstalled for use in baseline operations at ORNL.

  6. Enhancing the use of coals by gas reburning-sorbent injection

    Energy Technology Data Exchange (ETDEWEB)

    1989-09-27

    The objective of this project is to evaluate and demonstrate a cost effective emission control technology for acid rain precursors, oxides of nitrogen (NO{sub x}) and sulfur (SO{sub x}), on three coal fired utility boilers in Illinois. The units selected are representative of pre-NSPS design practices: tangential, wall, and cyclone fired. The specific objectives are to demonstrate reductions of 60 percent in NO{sub x} and 50 percent in SO{sub x} emissions, by a combination of two developed technologies, gas reburning (GR) and sorbent injection (SI). With GR, about 80--85 percent of the coal fuel is fired in the primary combustion zone. The balance of the fuel is added downstream as natural gas to create a slightly fuel rich environment in which NO{sub x} is converted to N{sub 2}. The combustion process is completed by overfire air addition. SO{sub x} emissions are reduced by injecting dry sorbents (usually calcium based) into the upper furnace. The sorbents trap SO{sub x} as solid sulfates that are collected in the particulate control device.

  7. Boron removal by a composite sorbent: Polyethylenimine/tannic acid derivative immobilized in alginate hydrogel beads.

    Science.gov (United States)

    Bertagnolli, Caroline; Grishin, Andrey; Vincent, Thierry; Guibal, Eric

    2017-03-21

    A novel composite material was prepared by the grafting of tannic acid on polyethylenimine (PEI), which allows an efficient sorption of boron (sorption capacity close to 0.89 mmol B g -1 ). The encapsulation of this chelating sorbent (finely crushed) facilitates its use (readily solid/liquid separation, use in fixed-bed columns) at the expense of a loss in sorption capacity (proportionally decreased by the introduction of alginate having poor efficiency for boron uptake). Sorption isotherms are modeled using the Langmuir equation, while the kinetic profiles are presented a good fit by pseudo-second order rate equation. In addition, the encapsulating matrix introduces supplementary resistance to intraparticle diffusion, especially when the resin is dried without control: freeze-drying partially limits this effect. The stability (at long-term storage) of the sorbent is improved when the sorbent is stored under nitrogen atmosphere. The presence of an excess of NaCl was investigated. The degradation of the hydrogel (by ion-exchange of Ca(II) with Na(I)) leads to a decrease in the sorption performance of composite material but the action of Ca(II) ions in the solutions re-stabilizes the hydrogel.

  8. Biodegradation and ecotoxicity of soil contaminated by pentachlorophenol applying bioaugmentation and addition of sorbents

    Energy Technology Data Exchange (ETDEWEB)

    Zuzana, S.; Katarina, D.; Livia, T. [Slovak Technical University Bratislava, Bratislava (Slovakia). Dept. of Biochemical Technology

    2009-02-15

    Biodegradation of pentachlorophenol (PCP) in soil by autochthonous microorganisms and in soil bioaugmented by the bacterial strain Comamonas testosteroni CCM 7530 was studied. Subsequent addition of organomineral complex (OMC) or lignite as possible sorbents for PCP immobilization has been investigated as well. The OMC was prepared from humic acids (HAs) isolated from lignite by binding them onto zeolite. Biodegradation of PCP and number of colony forming units (CFUs) were determined in the three types of soil, Chernozem, Fluvisol, and Regosol, freshly spiked with PCP and amended separately with tested sorbents. The enhancing effect of sorbent addition and bioaugmentation on PCP biodegradation depended mainly on the soil type and the initial PCP concentration. Microbial activity resulted in biotransformation of PCP into certain toxic substances, probably lower chlorinated phenols that are more soluble than PCP, and therefore more toxic to present biota. Therefore, it was necessary to monitor soil ecotoxicity during biodegradation. Addition of the OMC resulted in a more significant decrease of soil toxicity in comparison with addition of lignite. Lignite and OMC appear to be good traps for PCP with potential application in remediation technology.

  9. Sorbent materials for rapid remediation of wash water during radiological event relief

    Energy Technology Data Exchange (ETDEWEB)

    Jolin, William C.; Kaminski, Michael

    2016-11-01

    Procedures for removing harmful radiation from interior and exterior surfaces of homes and businesses after a nuclear or radiological disaster may generate large volumes of radiologically contaminated waste water. Rather than releasing this waste water to potentially contaminate surrounding areas, it is preferable to treat it onsite. Retention barrels are a viable option because of their simplicity in preparation and availability of possible sorbent materials. This study investigated the use of aluminosilicate clay minerals as sorbent materials to retain 137Cs, 85Sr, and 152Eu. Vermiculite strongly retained 137Cs, though other radionuclides displayed diminished affinity for the surface. Montmorillonite exhibited increased affinity to sorb 85Sr and 152Eu in the presence of higher concentrations of 137Cs. To simulate flow within retention barrels, vermiculite was mixed with sand and used in small-scale column experiments. The GoldSim contaminate fate module was used to model breakthrough and assess the feasibility of using clay minerals as sorbent materials in retention barrels. The modeled radionuclide breakthrough profiles suggest that vermiculite-sand and montmorillonite-sand filled barrels could be used for treatment of contaminated water generated from field operations.

  10. Advanced in-duct sorbent injection for SO{sub 2} control. Final technical report

    Energy Technology Data Exchange (ETDEWEB)

    Stouffer, M.R.; Withium, J.A.; Rosenhoover, W.A.; Maskew, J.T.

    1994-12-01

    The objective of this research project was to develop a second generation duct sorbent injection technology as a cost-effective compliance option for the 1990 Clean Air Act Amendments. Research and development work was focused on the Advanced Coolside process, which showed the potential for exceeding the original performance targets of 90% SO{sub 2} removal and 60% sorbent utilization. Process development was conducted in a 1000 acfm pilot plant. The pilot plant testing showed that the Advanced Coolside process can achieve 90% SO{sub 2} removal at sorbent utilizations up to 75%. The testing also showed that the process has the potential to achieve very high removal efficiency (90 to >99%). By conducting conceptual process design and economic evaluations periodically during the project, development work was focused on process design improvements which substantially lowered process capital and operating costs, A final process economic study projects capital costs less than one half of those for limestone forced oxidation wet FGD. Projected total SO{sub 2} control cost is about 25% lower than wet FGD for a 260 MWe plant burning a 2.5% sulfur coal. A waste management study showed the acceptability of landfill disposal; it also identified a potential avenue for by-product utilization which should be further investigated. Based on the pilot plant performance and on the above economic projections, future work to scale up the Advanced Coolside process is recommended.

  11. Application of Chemically Modified and Unmodified Waste Biological Sorbents in Treatment of Wastewater

    Directory of Open Access Journals (Sweden)

    John Kanayochukwu Nduka

    2012-01-01

    Full Text Available Protein wastes (feathers, goat hair and cellulosic wastes (corn cob, coconut husks were collected and washed with detergent solution, thoroughly rinsed and sun dried for 2 days before drying in an oven, and then ground. One-half of ground material was carbonized at a maximum temperature of 500°C after mixing with H2SO4. The carbonized parts were pulverized; both carbonized and uncarbonized sorbents were sieved into two particle sizes of 325 and 625 μm using mechanical sieve. Sorbents of a given particle size were packed into glass column.Then, textile wastewater that had its physicochemical parameters previously determined was eluted into each glass column and a contact time of 60 and 120 mins was allowed before analysis. Results showed 48.15–99.98 percentage reduction of NO3−, EC, Cl−, BOD, COD, DO, TSS, and TDS, 34.67–99.93 percentage reduction of NO3−, EC, Cl−, BOD, COD, DO, TSS, and TDS, 52.83–97.95 percentage reduction of Pb2+, Ni2+, Cr3+ and Mn2+ and 34.59–94.87 percentage reduction of Pb2+, Ni2+, Cr3+ and Mn2+. Carbonization, small particle, size and longer contact time enhanced the sorption capabilities of the sorbents. These show that protein and cellulosic wastes can be used to detoxify wastewater.

  12. Effects of sorbent materials on the cryofocusing analysis of gaseous reduced sulphur compounds.

    Science.gov (United States)

    Kim, Ki-Hyun; Pandey, Sudhir Kumar; Ahn, J H; Szulejko, J E; Sohn, Jong Ryeul

    2014-08-01

    The relative performance of different sorbent materials employed in the cryofocusing (e.g. in cold trap (CT) unit) stage was investigated at sub-ambient temperature by the thermal desorption (TD)-gas chromatography (GC)-pulsed flame photometric detector. To this end, the TD-based calibration of five reduced sulphur compounds (RSC: H2S, CH3SH, CS2, DMS and DMDS) and SO2 was carried out via the Peltier cooling system with five types of sorbent combinations such as two single-bed (Tenax TA and Silica gel) plus three multibed types (a combination of either two from the following three sorbents: Tenax TA, Silica gel and Carbopack B). Relative performance of each of all five CT options, if evaluated in terms of response factors for each compound, demonstrated that each CT composition acts as an important criterion to distinguish detection properties between light and heavy sulphur species. Although the relative response of H2S and CH3 SH was systematically distinguishable between the CT types, that of SO2 was the most complicated to interpret. According to this study, the two CT types consisting of Carbopack B and Silica gel (CS-0.4 and CS-0.6) were the optimum choices for sulphur gas analysis in terms of basic QA parameters (sensitivity, reproducibility and linearity).

  13. Design, Fabrication, and Shakeout Testing of ATALANTE Dissolver Off-Gas Sorbent-Based Capture System

    Energy Technology Data Exchange (ETDEWEB)

    Walker, Jr, Joseph Franklin [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jubin, Robert Thomas [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jordan, Jacob A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bruffey, Stephanie H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2015-07-31

    A sorbent-based capture system designed for integration into the existing dissolver off-gas (DOG) treatment system at the ATelier Alpha et Laboratoires pour ANalyses, Transuraniens et Etudes de retraitement (ATALANTE) facility has been successfully designed and fabricated and has undergone shakeout testing. Discussions with personnel from the ATALANTE facility provided guidance that was used for the design. All components for this system were specified, procured, and received on site at Oak Ridge National Laboratory (ORNL). The system was then fabricated and tested at ORNL to verify operation. Shakeout testing resulted in a simplified system. This system should be easily installed into the existing facility and should be straightforward to operate during future experimental testing. All parts were selected to be compatible with ATALANTE power supplies, space requirements, and the existing DOG treatment system. Additionally, the system was demonstrated to meet all of four design requirements. These include (1) a dissolver off-gas flow rate of ≤100 L/h (1.67 L/min), (2) an external temperature of ≤50°C for all system components placed in the hot cell, (3) a sorbent bed temperature of ~150°C, and (4) a gas temperature of ~150°C upon entry into the sorbent bed. The system will be ready for shipment and installation in the existing DOG treatment system at ATALANTE in FY 2016.

  14. The natural and man made radioactivity in some local and imported sorbent materials

    International Nuclear Information System (INIS)

    EL AFIFI, E.M.; HILAL, M.A.; DAIFUALLAH, A.M.

    2005-01-01

    The present study was carried out to detect the radioactivity concentrations (Bq/kg dry weight) in some sorbent materials used in several industrial purposes. This radioactivity may be natural or artificial. Five brands of these materials were investigated, three of them were manufactured locally while the other two were imported. The samples were analyzed by gamma ray spectrometry to assess the activity concentration. The results showed that the local samples contained primordial radionuclides of uranium-238 ( 238 U), uranium-235 ( 235 U) and thorium-232 ( 232 Th) and their respective decay progenies ( 226 Ra, 214 Pb, 214 Bi, 210 Pb, 235 U, 228 Ra (Ac), 212 Pb, 208 Tl) and potassium-40 ( 40 K). The two imported samples were found to contain 137 Cs as well as the natural radioactivity. The correlation coefficient (r) was calculated and discussed for total activity and fixed carbon content of samples. Value of correlation coefficient showed poor relation between activity concentration and carbon content (%). The radium equivalent index and the total absorbed dose rates due to gamma emissions were also estimated and evaluated. Based on the obtained results, it is favourable to use the sorbents manufactured locally and if it is necessary to use the imported sorbents, these materials should be surveyed radiologically before use to avoid its radiation hazards for the workers in this field and/or contamination of the treated materials consequently to the public

  15. Preliminary coating design and coating developments for ATHENA

    DEFF Research Database (Denmark)

    Jakobsen, Anders Clemen; Ferreira, Desiree Della Monica; Christensen, Finn Erland

    2011-01-01

    We present initial novel coating design for ATHENA. We make use of both simple bilayer coatings of Ir and B4C and more complex constant period multilayer coatings to enhance the effective area and cover the energy range from 0.1 to 10 keV. We also present the coating technology used...... for these designs and present test results from coatings....

  16. Production and characterization of carbonized sorbent products optimized for anionic contaminants

    Science.gov (United States)

    Viglasova, Eva; Fristak, Vladimir; Galambos, Michal; Hood-Nowotny, Rebecca; Soja, Gerhard

    2017-04-01

    Processing conditions, production methods and feedstock characteristics have been shown to affect the final sorption properties of biochar-based sorbents that have been produced in pyrolysis reactors. The content of O-containing carboxyl, phenolic and hydroxyl functional groups on the biochar surfaces plays a crucial role in sorption chemistry of hazardous materials. The sorption process can be affected by the presence of non-carbonized fractions in biochar matter as well. All these characteristics indicate that biochar shows good potential as a new tool in removal and separation technologies of various pollutants from waste water or contaminated soils. The sorption potential of wood-based biochars for cationic forms of heavy metals has been studied intensively and has already led to successful pilot applications in the field. However, anionic compounds (e.g. phosphate, nitrate, sulphate, As-, Cr-compounds) do not sorb well to unmodified biochar and need specific surface modification of biochar. Based on this fact, we try to obtain data about the sorptive separation of anionic forms of various contaminants from model aqueous solutions by different types of biochar-derived sorbents, or mineral-enriched biochar-derived sorbents. An important part of this research is the assesment of the effects of varying process parameters during biomass carbonisation, the role of biomass feedstock and pre-and/or post-treatment of the biochars onto sorption processes. We specify the most appropriate application strategies with biochar for remediation purposes of waste water or contaminated waters with elevated toxic metal concentrations that might compromise the quality of surface waters. The main aim of research is the preparation of modified biochar sorbent, the characterization of its surface and the investigation about new possibilities of modified biochar sorbent applications for sorption of various contaminants, mainly their anionic forms (e.g. phosphates, nitrates, arsenates

  17. Ecologically friendly ways to clean up oil spills in harbor water areas: crude oil and diesel sorption behavior of natural sorbents.

    Science.gov (United States)

    Paulauskiene, Tatjana

    2018-01-29

    This work aimed to evaluate the sorption capacity of natural sorbents (wool, moss, straw, peat) and their composites during the sorption of crude oil and of diesel overspread on the water surface. The work presents the research results of the maximum sorption capacity of the sorbents/their composites using crude oil/diesel; the sorption capacity of the sorbents/their composites when crude oil/diesel is spilled on the water surface; and the research results of the unrealized part of the crude oil/diesel in the sorbents. The results of the analysis showed that all the sorbents and their composites have their selectivity to crude oil less than 50%. Also the results showed that the distribution of diesel and water in the sorbents and their composites is very different compared with the distribution of crude oil during the sorption analyses. In total, the diesel in the liquid mass absorbed by the straw and the peat amounted to 17 and 20%, respectively. This shows that these sorbents are much more selective for water but not for diesel. A larger part of the diesel was in the liquid amount absorbed by the composites-up to 33%. Accordingly, the use of these composites in watery environments is much more effective than the use of individual sorbents. The composition of sorbents in the composite enhanced both the hydrophobic and the oleophilic properties; as a result, a more effective removal of the diesel and oil from the water surface was achieved.

  18. F- and H-Area Seepage Basins Water Treatment System Process Optimization and Alternative Chemistry Ion Exchange/Sorbent Material Screening Clearwell Overflow Study

    Energy Technology Data Exchange (ETDEWEB)

    Serkiz, S.M.

    2000-08-30

    This study investigated alternative ion exchange/sorbent materials and polishing chemistries designed to remove specific radionuclides not removed during the neutralization/precipitation/clarification process.

  19. Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

    Science.gov (United States)

    Promulgated quality assurance Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

  20. Zinc phosphate conversion coatings

    Energy Technology Data Exchange (ETDEWEB)

    Sugama, Toshifumi (Wading River, NY)

    1997-01-01

    Zinc phosphate conversion coatings for producing metals which exhibit enhanced corrosion prevention characteristics are prepared by the addition of a transition-metal-compound promoter comprising a manganese, iron, cobalt, nickel, or copper compound and an electrolyte such as polyacrylic acid, polymethacrylic acid, polyitaconic acid and poly-L-glutamic acid to a phosphating solution. These coatings are further improved by the incorporation of Fe ions. Thermal treatment of zinc phosphate coatings to generate .alpha.-phase anhydrous zinc phosphate improves the corrosion prevention qualities of the resulting coated metal.

  1. Zinc phosphate conversion coatings

    Energy Technology Data Exchange (ETDEWEB)

    Sugama, T.

    1997-02-18

    Zinc phosphate conversion coatings for producing metals which exhibit enhanced corrosion prevention characteristics are prepared by the addition of a transition-metal-compound promoter comprising a manganese, iron, cobalt, nickel, or copper compound and an electrolyte such as polyacrylic acid, polymethacrylic acid, polyitaconic acid and poly-L-glutamic acid to a phosphating solution. These coatings are further improved by the incorporation of Fe ions. Thermal treatment of zinc phosphate coatings to generate {alpha}-phase anhydrous zinc phosphate improves the corrosion prevention qualities of the resulting coated metal. 33 figs.

  2. Multi-component testing using HZ-PAN and AgZ-PAN Sorbents for OSPREY Model validation

    Energy Technology Data Exchange (ETDEWEB)

    Garn, Troy G. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Greenhalgh, Mitchell [Idaho National Lab. (INL), Idaho Falls, ID (United States); Lyon, Kevin L. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Law, Jack D. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2015-04-01

    In efforts to further develop the capability of the Off-gas SeParation and RecoverY (OSPREY) model, multi-component tests were completed using both HZ-PAN and AgZ-PAN sorbents. The primary purpose of this effort was to obtain multi-component xenon and krypton capacities for comparison to future OSPREY predicted multi-component capacities using previously acquired Langmuir equilibrium parameters determined from single component isotherms. Experimental capacities were determined for each sorbent using two feed gas compositions of 1000 ppmv xenon and 150 ppmv krypton in either a helium or air balance. Test temperatures were consistently held at 220 K and the gas flowrate was 50 sccm. Capacities were calculated from breakthrough curves using TableCurve® 2D software by Jandel Scientific. The HZ-PAN sorbent was tested in the custom designed cryostat while the AgZ-PAN was tested in a newly installed cooling apparatus. Previous modeling validation efforts indicated the OSPREY model can be used to effectively predict single component xenon and krypton capacities for both engineered form sorbents. Results indicated good agreement with the experimental and predicted capacity values for both krypton and xenon on the sorbents. Overall, the model predicted slightly elevated capacities for both gases which can be partially attributed to the estimation of the parameters and the uncertainty associated with the experimental measurements. Currently, OSPREY is configured such that one species adsorbs and one does not (i.e. krypton in helium). Modification of OSPREY code is currently being performed to incorporate multiple adsorbing species and non-ideal interactions of gas phase species with the sorbent and adsorbed phases. Once these modifications are complete, the sorbent capacities determined in the present work will be used to validate OSPREY multicomponent adsorption predictions.

  3. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Science.gov (United States)

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  4. Development of superparamagnetic high-magnetization C18-functionalized magnetic silica nanoparticles as sorbents for enrichment and determination of methylprednisolone in rat plasma by high performance liquid chromatography.

    Science.gov (United States)

    Yu, Panfeng; Wang, Qi; Zhang, Xifeng; Zhang, Xuesong; Shen, Shun; Wang, Yan

    2010-09-23

    In this study, a novel extraction and enrichment technique based on superparamagnetic high-magnetization C(18)-functionalized magnetic silica nanoparticles (C(18)-MNPs) as sorbents was successfully developed for the determination of methylprednisolone (MP) in rat plasma by high performance liquid chromatography (HPLC). The synthesized silica-coated magnetite modified with chlorodimethyl-n-octadecylsilane was about 320 nm in diameter with strong magnetism and high surface area. It provided an efficient way for extraction and concentration of MP in the samples through hydrophobic interaction by the interior C(18) groups. Moreover, MP adsorbed with C(18)-MNPs could be simply and rapidly isolated through placing a strong magnet on the bottom of container, and then easily eluted from C(18)-MNPs by n-hexane solution. Extraction conditions such as amounts of C(18)-MNPs added, adsorption time and desorption solvent, were investigated. Method validations including linear range, detection limit, precision, and recovery were also studied. The results showed that the proposed method based on C(18)-MNPs was a simple, accurate and high efficient approach for the analysis of MP in the complex plasma samples. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. A Simple and Fast Method Based on New Magnetic Ion Imprinted Polymer as a Highly Selective Sorbent for Preconcentration and Determination of Cadmium in Environmental Samples.

    Science.gov (United States)

    Panjali, Zahra; Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira; Jalilian, Niloofar; Yarahmadi, Rasoul; Shahtaheri, Seyed Jamaleddin

    2016-08-01

    The analysis of heavy metals at trace level is one of the main toxicologists concern, due to their vital rules in human`s life. Cadmium is one of these toxic heavy metals, which released to the environment from various industries. In order to determine Cd (II) ions in various matrices magnetic ion-imprinted polymer (IIP) method has been developed and applied. This nano-sorbent has been synthesized by coating an IIP compound on Fe 3 O 4 nanoparticles core to achieve highest surface area. This polymer has been used to evaluate Cd (II) levels in food, river, and wastewater in Tehran, Iran. Fe 3 O 4 @Cd-IIP was stable up to 300 °C. The various factors such as sample pH (optimized as 7), elution/sorption time (5 min), eluent amount (4 mL HCL), and its concentration (2 mol L -1 ) were optimized. Analysis instrument in all steps was Flame Atomic Abortion Spectrophotometer (FAAS). In this study, the detection limit was determined down to 0.6 μg L -1 . This method was applied successfully for the preconcentration and determination of Cd (II) ions in environmental samples obtained from rivers, various foods and wastewater. In addition, the accuracy of the method was confirmed by analyzing a certified reference material (Seronorm LOT NO2525) and spiked real samples.

  6. Combustion chemical vapor deposited coatings for thermal barrier coating systems

    Energy Technology Data Exchange (ETDEWEB)

    Hampikian, J.M.; Carter, W.B. [Georgia Institute of Technology, Atlanta, GA (United States). School of Materials Science and Engineering

    1995-12-31

    The new deposition process, combustion chemical vapor deposition, shows a great deal of promise in the area of thermal barrier coating systems. This technique produces dense, adherent coatings, and does not require a reaction chamber. Coatings can therefore be applied in the open atmosphere. The process is potentially suitable for producing high quality CVD coatings for use as interlayers between the bond coat and thermal barrier coating, and/or as overlayers, on top of thermal barrier coatings. In this report, the evaluation of alumina and ceria coatings on a nickel-chromium alloy is described.

  7. Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice

    Directory of Open Access Journals (Sweden)

    Dong Kyu Lim

    2018-01-01

    Full Text Available The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC–MS to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043. Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice.

  8. Degradation product emission from historic and modern books by headspace SPME/GC-MS: evaluation of lipid oxidation and cellulose hydrolysis.

    Science.gov (United States)

    Clark, Andrew J; Calvillo, Jesse L; Roosa, Mark S; Green, David B; Ganske, Jane A

    2011-04-01

    Volatile organic compounds emitted from a several decade series of bound periodicals (1859-1939) printed on ground wood paper, as well as historical books dating from the 1500s to early 1800s made from cotton/linen rag, were studied using an improved headspace SPME/GC-MS method. The headspace over the naturally aging books, stored upright in glass chambers, was monitored over a 24-h period, enabling the identification of a wide range of organic compounds emanating from the whole of the book. The detection of particular straight chain aldehydes, as well as characteristic alcohols, alkenes and ketones is correlated with oxidative degradation of the C(18) fatty acid constituency of paper. The relative importance of hydrolytic and oxidative chemistry involved in paper aging in books published between 1560 and 1939 was examined by comparing the relative abundances of furfural (FUR) a known cellulose hydrolysis product, and straight chain aldehydes (SCA) produced from the oxidation of fatty acids in paper. The relative abundance of furfural is shown to increase across the 379-year publication time span. A comparison of relative SCA peak areas across the series of books examined reveals that SCA emission is more important in the cotton/linen rag books than in the ground wood books.

  9. Stable isotope dilution assay (SIDA) and HS-SPME-GCMS quantification of key aroma volatiles for fruit and sap of Australian mango cultivars.

    Science.gov (United States)

    San, Anh T; Joyce, Daryl C; Hofman, Peter J; Macnish, Andrew J; Webb, Richard I; Matovic, Nicolas J; Williams, Craig M; De Voss, James J; Wong, Siew H; Smyth, Heather E

    2017-04-15

    Reported herein is a high throughput method to quantify in a single analysis the key volatiles that contribute to the aroma of commercially significant mango cultivars grown in Australia. The method constitutes stable isotope dilution analysis (SIDA) in conjunction with headspace (HS) solid-phase microextraction (SPME) coupled with gas-chromatography mass spectrometry (GCMS). Deuterium labelled analogues of the target analytes were either purchased commercially or synthesised for use as internal standards. Seven volatiles, hexanal, 3-carene, α-terpinene, p-cymene, limonene, α-terpinolene and ethyl octanoate, were targeted. The resulting calibration functions had determination coefficients (R 2 ) ranging from 0.93775 to 0.99741. High recovery efficiencies for spiked mango samples were also achieved. The method was applied to identify the key aroma volatile compounds produced by 'Kensington Pride' and 'B74' mango fruit and by 'Honey Gold' mango sap. This method represents a marked improvement over current methods for detecting and measuring concentrations of mango fruit and sap volatiles. Copyright © 2016 Elsevier Ltd. All rights reserved.

  10. Investigation of a Quantitative Method for the Analysis of Chiral Monoterpenes in White Wine by HS-SPME-MDGC-MS of Different Wine Matrices.

    Science.gov (United States)

    Song, Mei; Xia, Ying; Tomasino, Elizabeth

    2015-04-22

    A valid quantitative method for the analysis of chiral monoterpenes in white wine using head-space solid phase micro-extraction-MDGC-MS (HS-SPME-MDGC-MS) with stable isotope dilution analysis was established. Fifteen compounds: (S)-(-)-limonene, (R)-(+)-limonene, (+)-(2R,4S)-cis-rose oxide, (-)-(2S,4R)-cis-rose oxide, (-)-(2R,4R)-trans-rose oxide, (+)-(2S,4S)-cis-rose oxide, furanoid (+)-trans-linalool oxide, furanoid (-)-cis-linalool oxide, furanoid (-)-trans-linalool oxide, furanoid (+)-cis-linalool oxide, (-)-linalool, (+)-linalool, (-)-α-terpineol, (+)-α-terpineol and (R)-(+)-β-citronellol were quantified. Two calibration curves were plotted for different wine bases, with varying residual sugar content, and three calibration curves for each wine base were investigated during a single fiber's lifetime. This was needed as both sugar content and fiber life impacted the quantification of the chiral terpenes. The chiral monoterpene content of six Pinot Gris wines and six Riesling wines was then analyzed using the verified method. ANOVA with Tukey multiple comparisons showed significant differences for each of the detected chiral compounds in all 12 wines. PCA score plots showed a clear separation between the Riesling and Pinot Gris wines. Riesling wines had greater number of chiral terpenes in comparison to Pinot Gris wines. Beyond total terpene content it is possible that the differences in chiral terpene content may be driving the aromatic differences in white wines.

  11. Effect of hot air drying on volatile compounds of Flammulina velutipes detected by HS-SPME-GC-MS and electronic nose.

    Science.gov (United States)

    Yang, Wenjian; Yu, Jie; Pei, Fei; Mariga, Alfred Mugambi; Ma, Ning; Fang, Yong; Hu, Qiuhui

    2016-04-01

    Volatile compounds are important factors that affect the flavor quality of Flammulina velutipes, but the changes occurring during hot air drying is still unclear. To clarify the dynamic changes of flavor components during hot air drying, comprehensive flavor characterization and volatile compounds of F. velutipes were evaluated using electronic nose technology and headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS), respectively. Results showed that volatile components in F. velutipes significantly changed during hot air drying according to the principal component analysis and radar fingerprint chart of electronic nose. Volatile compounds of fresh F. velutipes consisted mainly of ketones, aldehydes and alcohols, and 3-octanone was the dominant compound. Drying process could significantly decrease the relative content of ketones and promoted the generation of alcohols, acids, and esters, which became the main volatile compounds of dried F. velutipes. These may provide a theoretical basis for the formation mechanism of flavor substances in dried F. velutipes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  12. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME-GC-MS: newly identified compounds, flavors molecular markers, and terpenic profile.

    Science.gov (United States)

    Cecchi, Teresa; Alfei, Barbara

    2013-12-01

    This study aims to contribute to the knowledge of the commercial, sensory, and analytical characteristics of extra virgin olive oil (EVOO) from Italy (Marche region), renowned since ancient times. Headspace solid-phase micro-extraction (HS-SPME) was applied for the very first time to the sampling of volatile compounds of eleven typical Italian monocultivar EVOOs. Forty-eight compounds were characterised by GC-MS, some of them were only occasionally found in other EVOOs and some other were never detected before in any EVOO. Compounds belonging mainly to alcohols, esters, aldehydes, ketones and hydrocarbons chemical classes characterised the volatile profiles. The main volatile compounds detected in the EVOOs were the C6 compounds derived from polyunsaturated fatty acids, through the lipoxygenase pathway, in different proportion according to the specific cultivar. The results suggest that genetic factors strongly influence volatile formation and terpene hydrocarbons are claimed to be suitable markers of the geographic origin and genotype of the EVOO. Correlations among sensory attributes evaluated by a panel test and the presence of specific volatile compounds were highlighted for the very first time. The significance of the presence of some newly identified volatile compounds was discussed. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Characterization of volatile profile from ten different varieties of Chinese jujubes by HS-SPME/GC-MS coupled with E-nose.

    Science.gov (United States)

    Chen, Qinqin; Song, Jianxin; Bi, Jinfeng; Meng, Xianjun; Wu, Xinye

    2018-03-01

    Volatile profile of ten different varieties of fresh jujubes was characterized by HS-SPME/GC-MS (headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry) and E-nose (electronic nose). GC-MS results showed that a total of 51 aroma compounds were identified in jujubes, hexanoic acid, hexanal, (E)-2-hexenal, (Z)-2-heptenal, benzaldehyde and (E)-2-nonenal were the main aroma components with contributions that over 70%. Differentiation of jujube varieties was conducted by cluster analysis of GC-MS data and principal component analysis & linear discriminant analysis of E-nose data. Both results showed that jujubes could be mainly divided into two groups: group A (JZ, PDDZ, JSXZ and LWZZ) and group B (BZ, YZ, MZ, XZ and DZ). There were significant differences in contents of alcohols, acids and aromatic compounds between group A and B. GC-MS coupled with E-nose could be a fast and accurate method to identify the general flavor difference in different varieties of jujubes. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Raman spectroscopy, electronic microscopy and SPME-GC-MS to elucidate the mode of action of a new antimicrobial food packaging material.

    Science.gov (United States)

    Clemente, Isabel; Aznar, Margarita; Salafranca, Jesús; Nerín, Cristina

    2017-02-01

    One critical challenge when developing a new antimicrobial packaging material is to demonstrate the mode of action of the antimicrobials incorporated into the packaging. For this task, several analytical techniques as well as microbiology are required. In this work, the antimicrobial properties of benzyl isothiocyanate, allyl isothiocyanate and essential oils of cinnamon and oregano against several moulds and bacteria have been evaluated. Benzyl isothiocyanate showed the highest antimicrobial activity and it was selected for developing the new active packaging material. Scanning electron microscopy and Raman spectroscopy were successfully used to demonstrate the mode of action of benzyl isothiocyanate on Escherichia coli. Bacteria exhibited external modifications such as oval shape and the presence of septum surface, but they did not show any disruption or membrane damage. To provide data on the in vitro action of benzyl isothiocyanate and the presence of inhibition halos, the transfer mechanism to the cells was assessed using solid-phase microextraction-gas chromatography-mass spectrometry. Based on the transfer system, action mechanism and its stronger antimicrobial activity, benzyl isothiocyanate was incorporated to two kinds of antimicrobial labels. The labels were stable and active for 140 days against two mould producers of ochratoxin A; Penicillium verrucosum is more sensitive than Aspergillus ochraceus. Details about the analytical techniques and the results obtained are shown and discussed. Graphical Abstract Antimicrobial evaluation of pure compounds, incorporation in the packaging and study for mode of action on S. coli by Raman, SEM and SPME-GC-MS.

  15. Determination of Hazardous VOCs and Nicotine Released from Mainstream Smoke by the Combination of the SPME and GC-MS Methods

    Directory of Open Access Journals (Sweden)

    Sudhir Kumar Pandey

    2010-01-01

    Full Text Available In this study, the contents of nicotine and volatile organic compounds (VOCs in mainstream smoke (MSS were analyzed using samples of four cigarette types consisting of two common brands (R and E with full (F and light (L flavor, coded with R-F, R-L, E-F, and E-L. These cigarettes were also analyzed after removing the filter portions with the assignment of a new sample code of (N as the third letter (e.g., R-L-N. A total of 44 VOCs (including nicotine were quantified by the combination of the SPME and GC-MS methods. Out of the 44 VOCs, 10 were identified as hazardous air pollutants listed by the U.S. EPA, while their concentrations exceeded the reference exposure limits set by various agencies. A clear distinction was apparent in the concentration levels of VOCs between different brands or between full and light flavors. Nicotine concentrations varied greatly between different cigarettes types of the R brand, whereas such changes were insignificant in the counterpart E brand. This thus suggests that light-flavor cigarettes do not necessarily guarantee low doses of carcinogens (and tar than regular cigarettes, as their differences can be balanced by the inhaling behavior of the smoker.

  16. Optimizing the Costs of Solid Sorbent-Based CO2 Capture Process Through Heat Integration

    Energy Technology Data Exchange (ETDEWEB)

    Sjostrom, Sharon [Ada-Es, Inc., Highlands Ranch, CO (United States)

    2016-03-18

    The focus of this project was the ADAsorb™ CO2 Capture Process, a temperature-swing adsorption process that incorporates a three-stage fluidized bed as the adsorber and a single-stage fluidized bed as the regenerator. ADAsorb™ system was designed, fabricated, and tested under DOE award DEFE0004343. Two amine-based sorbents were evaluated in conjunction with the ADAsorb™ process: “BN”, an ion-exchange resin; and “OJ”, a metal organic framework (MOF) sorbent. Two cross heat exchanger designs were evaluated for use between the adsorber and regenerator: moving bed and fluidized bed. The fluidized bed approach was rejected fairly early in the project because the additional electrical load to power blowers or fans to overcome the pressure drop required for fluidization was estimated to be nominally three times the electrical power that could be generated from the steam saved through the use of the cross heat exchanger. The Energy Research Center at Lehigh University built and utilized a process model of the ADAsorb™ capture process and integrated this model into an existing model of a supercritical PC power plant. The Lehigh models verified that, for the ADAsorb™ system, the largest contributor to parasitic power was lost electrical generation, which was primarily electric power which the host plant could not generate due to the extraction of low pressure (LP) steam for sorbent heating, followed by power for the CO2 compressor and the blower or fan power required to fluidize the adsorber and regenerator. Sorbent characteristics such as the impacts of moisture uptake, optimized adsorption and regeneration temperature, and sensitivity to changes in pressure were also included in the modeling study. Results indicate that sorbents which adsorb more than 1-2% moisture by weight are unlikely to be cost competitive unless they have an extremely high CO2 working capacity that well exceeds 15% by weight. Modeling also revealed

  17. Rock-hard coatings

    OpenAIRE

    Muller, M.

    2007-01-01

    Aircraft jet engines have to be able to withstand infernal conditions. Extreme heat and bitter cold tax coatings to the limit. Materials expert Dr Ir. Wim Sloof fits atoms together to develop rock-hard coatings. The latest invention in this field is known as ceramic matrix composites. Sloof has signed an agreement wit