Radioactive Barium Ion Trap Based on Metal-Organic Framework for Efficient and Irreversible Removal of Barium from Nuclear Wastewater.

PubMed

Peng, Yaguang; Huang, Hongliang; Liu, Dahuan; Zhong, Chongli

2016-04-06

Highly efficient and irreversible capture of radioactive barium from aqueous media remains a serious task for nuclear waste disposal and environmental protection. To address this task, here we propose a concept of barium ion trap based on metal-organic framework (MOF) with a strong barium-chelating group (sulfate and sulfonic acid group) in the pore structures of MOFs. The functionalized MOF-based ion traps can remove >90% of the barium within the first 5 min, and the removal efficiency reaches 99% after equilibrium. Remarkably, the sulfate-group-functionalized ion trap demonstrates a high barium uptake capacity of 131.1 mg g(-1), which surpasses most of the reported sorbents and can selectively capture barium from nuclear wastewater, whereas the sulfonic-acid-group-functionalized ion trap exhibits ultrafast kinetics with a kinetic rate constant k2 of 27.77 g mg(-1) min(-1), which is 1-3 orders of magnitude higher than existing sorbents. Both of the two MOF-based ion traps can capture barium irreversibly. Our work proposes a new strategy to design barium adsorbent materials and provides a new perspective for removing radioactive barium and other radionuclides from nuclear wastewater for environment remediation. Besides, the concrete mechanisms of barium-sorbent interactions are also demonstrated in this contribution.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, D.P.; Richardson, C.F.

Three mercury measurement techniques were performed on synthesis gas streams before and after an amine-based sulfur removal system. The syngas was sampled using (1) gas impingers containing a nitric acid-hydrogen peroxide solution, (2) coconut-based charcoal sorbent, and (3) an on-line atomic absorption spectrophotometer equipped with a gold amalgamation trap and cold vapor cell. Various impinger solutions were applied upstream of the gold amalgamation trap to remove hydrogen sulfide and isolate oxidized and elemental species of mercury. The results from these three techniques are compared to provide an assessment of these measurement techniques in reducing gas atmospheres.

Sorption vacuum trap

NASA Technical Reports Server (NTRS)

Barrington, A. E.; Caruso, A. J.

1970-01-01

Modified sorption trap for use in high vacuum systems contains provisions for online regeneration of sorbent material. Trap is so constructed that it has a number of encapsulated resistance heaters and a valving and pumping device for removing gases from heated sorbing material. Excessive downtime is eliminated with this trap.

Development of an in-house mixed-mode solid-phase extraction for the determination of 16 basic drugs in urine by High Performance Liquid Chromatography-Ion Trap Mass Spectrometry.

PubMed

Musile, Giacomo; Cenci, Lucia; Piletska, Elena; Gottardo, Rossella; Bossi, Alessandra M; Bortolotti, Federica

2018-07-27

The aim of the present work was to develop a novel in-house mixed-mode SPE sorbent to be used for the HPLC-Ion TrapMS determination of 16 basic drugs in urine. By using a computational modelling, a virtual monomer library was screened identifying three suitable functional monomers, methacrylic acid (MAA), itaconic acid (IA) and 2-acrylamide-2-methylpropane sulfonic acid (AMPSA), respectively. Three different sorbents were then synthetized based on these monomers, and using as cross-linker trimethylolpropane trimethacrylate (TMPTMA). The sorbent characterization analyses brought to the selection of the AMPSA based phase. Using this novel in-house sorbent, a SPE-HPLC-Ion TrapMS method for drug analysis in urine was validated proving to be selective and accurate and showing a sensitivity adequate for toxicological urine analysis. The comparison of the in-house mixed-mode SPE sorbent with two analogous commercial mixed-mode SPE phases showed that the first one was better not only in terms of process efficiency, but also in terms of quality-price rate. To the best of our knowledge, this is the first time in which an in-house SPE procedure has been applied to the toxicological analysis of a complex matrix, such as urine. Copyright © 2018 Elsevier B.V. All rights reserved.

Evaluation of solid sorbents for the determination of fenhexamid, metalaxyl-M, pyrimethanil, malathion and myclobutanil residues in air samples: application to monitoring malathion and fenhexamid dissipation in greenhouse air using C-18 or Supelpak-2 for sampling.

PubMed

Tsiropoulos, Nikolaos G; Bakeas, Evangelos B; Raptis, Vasilios; Batistatou, Stavroula S

2006-07-28

A methodology is described for greenhouse air analysis by sampling fenhexamid, pyrimethanil, malathion, metalaxyl-M and myclobutanil in solid sorbents. Pesticides were determined by gas chromatography with NP Detector. The trapping efficiency of XAD-2, XAD-4, Supelpak-2, Florisil and C-18 at different sampling conditions (rate, time and air humidity) and pesticides concentration levels has been evaluated. No breakthrough was observed in the range of concentration studied (0.10-75 microg of each pesticide). In almost all the cases good stability results were obtained. Personal pumps have been used with selected sorbents (Supelpak-2 and C-18) in order to sample malathion and fenhexamid in air of experimental greenhouse after their application in a tomato crop. The dissipation process of the analytes in various time periods after application has been studied. Malathion concentrations varied between 20.1 microg m(-3) just after application and 1.06 microg m(-3) 3 days later. Fenhexamid concentrations, determined by high performance liquid chromatography with UV detection, fall rapidly; after 12 h post-application being below 0.50 microg m(-3).

CLOSED-LOOP STRIPPING ANALYSIS (CLSA) OF ...

EPA Pesticide Factsheets

Synthetic musk compounds have been found in surface water, fish tissues, and human breast milk. Current techniques for separating these compounds from fish tissues require tedious sample clean-upprocedures A simple method for the deterrnination of these compounds in fish tissues has been developed. Closed-loop stripping of saponified fish tissues in a I -L Wheaton purge-and-trap vessel is used to strip compounds with high vapor pressures such as synthetic musks from the matrix onto a solid sorbent (Abselut Nexus). This technique is useful for screening biological tissues that contain lipids for musk compounds. Analytes are desorbed from the sorbent trap sequentially with polar and nonpolar solvents, concentrated, and directly analyzed by high resolution gas chromatography coupled to a mass spectrometer operating in the selected ion monitoring mode. In this paper, we analyzed two homogenized samples of whole fish tissues with spiked synthetic musk compounds using closed-loop stripping analysis (CLSA) and pressurized liquid extraction (PLE). The analytes were not recovered quantitatively but the extraction yield was sufficiently reproducible for at least semi-quantitative purposes (screening). The method was less expensive to implement and required significantly less sample preparation than the PLE technique. The research focused on in the subtasks is the development and application of state-of the-art technologies to meet the needs of the public, Office of Water,

Multiresidue analytical method using dispersive solid-phase extraction and gas chromatography/ion trap mass spectrometry to determine pharmaceuticals in whole blood.

PubMed

Plössl, Florian; Giera, Martin; Bracher, Franz

2006-11-24

A convenient analytical method for the simultaneous determination of more than 40 pharmaceuticals belonging to various therapeutic categories in whole blood has been developed. Exemplarily, the method was fully validated for eight different pharmaceuticals. The procedure entails addition of acetonitrile, magnesium sulfate and sodium chloride to a small amount of blood, then the mixture is shaken intensively and centrifuged for phase separation. An aliquot of the organic layer is cleaned up by dispersive solid-phase extraction employing bulk sorbents as well as magnesium sulfate for the removal of residual water. This method was based on the QuEChERS approach developed for pesticide residue analysis in food. Gas chromatography/ion trap mass spectrometry (GC/MS) with electron (EI) and chemical (CI) ionisation was then used for qualitative and quantitative determination of the pharmaceuticals. The dispersive SPE with PSA (sorbent functionalized with primary and secondary amines) was found more suitable than aminopropyl and a styrene-divinylbenzene sorbent for sample clean-up before drug level determination in whole blood and plasma, as it was found that most of endogenous matrix components were removed and the analytes were isolated from spiked samples with recoveries above 80%. Variation coefficients of the repeatability typically smaller than 10% have been achieved for a wide range of the investigated substances. The used analytical conditions allowed to separate successively a variety of drugs and poisons with the typical limit of detection at <20 ng mL(-1) levels using 1 microL injection of equivalent blood sample in whole blood. The method is simple, rapid, cheap and very effective for therapeutic drug monitoring and forensic chemistry.

Use of a bisphenol-A imprinted polymer as a selective sorbent for the determination of phenols and phenoxyacids in honey by liquid chromatography with diode array and tandem mass spectrometric detection.

PubMed

Herrero-Hernández, E; Carabias-Martínez, R; Rodríguez-Gonzalo, E

2009-09-21

An extraction-preconcentration procedure based on the use of a molecularly imprinted polymer (MIP) as selective sorbent has been developed for the determination of several phenolic compounds (bisphenol-A, bisphenol-F and 4-nitrophenol) and phenoxyacid herbicides (2,4-D, 2,4,5-T and 2,4,5-TP) in honey samples. Liquid chromatography with diode array detection (LC-DAD) and electrospray ionisation-ion trap mass spectrometry (LC-IT-MS) were used for the separation, identification and quantification of these analytes. The molecularly imprinted polymer was obtained by precipitation polymerisation with bisphenol-A (BPA) as template and 4-vinylpyridine as the functional monomer. The behaviour of this sorbent was compared with those of other materials frequently used in SPE. The selectivity of the BPA-MIP for the target analytes was tested in samples containing other pesticides in common use. The recoveries achieved for all six compounds were in the 81-96% range. By applying the proposed procedure prior to LC-IT-MS, the limits of detection achieved in commercial honey samples were in the 0.1-3.8 ng g(-1) range, with relative standard deviations of 12-24%.

Technetium-99m generator system

DOEpatents

Mirzadeh, Saed; Knapp, Jr., Furn F.; Collins, Emory D.

1998-01-01

A .sup.99 Mo/.sup.99m Tc generator system includes a sorbent column loaded with a composition containing .sup.99 Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating .sup.99m Tc eluted from the sorbent column. A method of preparing a concentrated solution of .sup.99m Tc includes the general steps of: a. providing a sorbent column loaded with a composition containing .sup.99 Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; b. eluting the sorbent column with a salt solution to elute .sup.99m Tc from the sorbent and to trap and concentrate the eluted .sup.99m Tc on the ion-exchange column; and c. eluting the concentrated .sup.99m Tc from the ion-exchange column with a solution comprising a reductive complexing agent.

Technetium-99m generator system

DOEpatents

Mirzadeh, S.; Knapp, F.F. Jr.; Collins, E.D.

1998-06-30

A {sup 99}Mo/{sup 99m}Tc generator system includes a sorbent column loaded with a composition containing {sup 99}Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating {sup 99m}Tc eluted from the sorbent column. A method of preparing a concentrated solution of {sup 99m}Tc includes the general steps of: (a) providing a sorbent column loaded with a composition containing {sup 99}Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; (b) eluting the sorbent column with a salt solution to elute {sup 99m}Tc from the sorbent and to trap and concentrate the eluted {sup 99m}Tc on the ion-exchange column; and (c) eluting the concentrated {sup 99m}Tc from the ion-exchange column with a solution comprising a reductive complexing agent. 1 fig.

Suspension column for recovery and separation of substances using ultrasound-assisted retention of bead sorbents.

PubMed

Spivakov, Boris Ya; Shkinev, Valeriy M; Danilova, Tatiana V; Knyazkov, Nikolai N; Kurochkin, Vladimir E; Karandashev, Vasiliy K

2012-12-15

A novel approach to sorption recovery and separation of different substances is proposed which is based on the use of suspended bead sorbents instead of conventional packed beds of such sorbents. This makes it possible to employ small-sized beads which are trapped in a low-pressure column due to ultrasound-assisted retention, without any frits to hold the sorption material. A flow system including a separation mini-column, named herein a suspension column, has been developed and tested by the studies of solid phase extraction (SPE) of trace metals from bi-distilled water and sea water using a 150-μL column with a silica-based sorbent containing iminodiacetic groups (DIAPAK IDA) and having a grain size of 6 μm. The adsorption properties of DIAPAK IDA suspension (9.5mg) were evaluated through adsorption/desorption experiments, where the effect of solution pH and eluent on the SPE of trace metals were examined by ICP-MS or ICP-AES measurements. When sample solution was adjusted to pH 8.0 and 1 mol L(-1) nitric acid was used as eluent, very good recoveries of more than 90% were obtained for a number of elements in a single-step extraction. To demonstrate the versatility of the approach proposed and to show another advantage of ultrasonic field (acceleration of sorbate/sorbent interaction), a similar system was used for heterogeneous immunoassays of some antigens in ultrasonic field using agarose sorbents modified by corresponding antibodies. It has been shown that immunoglobulins, chlamidia, and brucellos bacteria can be quantitatively adsorbed on 15-μm sorbent (15 particles in 50 μL) and directly determined in a 50-μL mini-chamber using fluorescence detection. Copyright © 2012 Elsevier B.V. All rights reserved.

Large volume preconcentration and determination of nanomolar concentrations of iron in seawater using a renewable cellulose 8-hydroquinoline sorbent microcolumn and universal approach of post-column eluate utilization in a Lab-on-Valve system.

PubMed

Horstkotte, Burkhard; Chocholouš, Petr; Solich, Petr

2016-04-01

We report on a Lab-On-Valve (LOV) configuration for analyte preconcentration from milliliter sample volumes using confluent mixing in the holding coil for in-line addition of loading buffer. The system was applied to the spectrophotometric determination of iron(II) in acidified seawater using 1,10-phenanthroline as color reagent. A cellulose-based chelating sorbent containing 8-hydroxyquinoline was used for the first time in LOV and excellent retention behavior and loading capacity were found. The flow system employs a syringe pump for handling all solutions (sorbent suspension, loading buffer, water, eluent, and color reagent) and a peristaltic pump for sample propulsion and includes a fit-for-purpose 14 cm long detection glass flow cell and a bubble trap for in-line carrier degasification. Advantage was taken of the LOV flow-through port to keep the eluted analytes for re-aspiration for subsequent chromogenic reaction. In effect, a universal analyzer configuration and preconcentration procedure was developed, which is combinable with other analytes, sorbents, and reagents. Among the studied parameters were the compositions, pH, volumes, and flow rates of loading buffer, eluent, and color reagent, as well as the microcolumn size, repeatability, and system stability. Reproducibility of 4.1% RSD over the entire working range, a LOD of down to 5 nmol L(-1), sampling frequency of 12h(-1), and linearity up to 1 µmol L(-1) for 3.3 mL of sample were obtained and applicability to real samples was demonstrated. It was proven that both Fe(III) and Fe(II) were retained and yielded similar recovery and sensitivity values. The method was applied to coastal seawater samples and spiking experiments yielded recovery values close to 100%. Copyright © 2015 Elsevier B.V. All rights reserved.

Performance characteristics of an automated gas chromatograph-ion trap mass spectrometer system used for the 1995 Southern Oxidants Study field investigation in Nashville, Tennessee

NASA Astrophysics Data System (ADS)

Daughtrey, E. Hunter; Adams, Jeffrey R.; Oliver, Karen D.; Kronmiller, Keith G.; McClenny, William A.

1998-09-01

A trailer-deployed automated gas chromatograph-mass spectrometer (autoGC-MS) system capable of making continuous hourly measurements was used to determine volatile organic compounds (VOCs) in ambient air at New Hendersonville, Tennessee, and Research Triangle Park, North Carolina, in 1995. The system configuration, including the autoGC-MS, trailer and transfer line, siting, and sampling plan and schedule, is described. The autoGC-MS system employs a pair of matched sorbent traps to allow simultaneous sampling and desorption. Desorption is followed by Stirling engine cryofocusing and subsequent GC separation and mass spectral identification and quantification. Quality control measurements described include evaluating precision and accuracy of replicate analyses of independently supplied audit and round-robin canisters and determining the completeness of the data sets taken in Tennessee. Data quality objectives for precision (±10%) and accuracy (±20%) of 10- to 20-ppbv audit canisters and a completeness of >75% data capture were met. Quality assurance measures used in reviewing the data set include retention time stability, calibration checks, frequency distribution checks, and checks of the mass spectra. Special procedures and tests were used to minimize sorbent trap artifacts, to verify the quality of a standard prepared in our laboratory, and to prove the integrity of the insulated, heated transfer line. A rigorous determination of total system blank concentration levels using humidified scientific air spiked with ozone allowed estimation of method detection limits, ranging from 0.01 to 1.0 ppb C, for most of the 100 target compounds, which were a composite list of the target compounds for the Photochemical Assessment Monitoring Station network, those for Environmental Protection Agency method TO-14, and selected oxygenated VOCs.

Headspace needle-trap analysis of priority volatile organic compounds from aqueous samples: application to the analysis of natural and waste waters.

PubMed

Alonso, Monica; Cerdan, Laura; Godayol, Anna; Anticó, Enriqueta; Sanchez, Juan M

2011-11-11

Combining headspace (HS) sampling with a needle-trap device (NTD) to determine priority volatile organic compounds (VOCs) in water samples results in improved sensitivity and efficiency when compared to conventional static HS sampling. A 22 gauge stainless steel, 51-mm needle packed with Tenax TA and Carboxen 1000 particles is used as the NTD. Three different HS-NTD sampling methodologies are evaluated and all give limits of detection for the target VOCs in the ng L⁻¹ range. Active (purge-and-trap) HS-NTD sampling is found to give the best sensitivity but requires exhaustive control of the sampling conditions. The use of the NTD to collect the headspace gas sample results in a combined adsorption/desorption mechanism. The testing of different temperatures for the HS thermostating reveals a greater desorption effect when the sample is allowed to diffuse, whether passively or actively, through the sorbent particles. The limits of detection obtained in the simplest sampling methodology, static HS-NTD (5 mL aqueous sample in 20 mL HS vials, thermostating at 50 °C for 30 min with agitation), are sufficiently low as to permit its application to the analysis of 18 priority VOCs in natural and waste waters. In all cases compounds were detected below regulated levels. Copyright © 2011 Elsevier B.V. All rights reserved.

Lunar Sulfur Capture System

NASA Technical Reports Server (NTRS)

Berggren, Mark; Zubrin, Robert; Bostwick-White, Emily

2013-01-01

The Lunar Sulfur Capture System (LSCS) protects in situ resource utilization (ISRU) hardware from corrosion, and reduces contaminant levels in water condensed for electrolysis. The LSCS uses a lunar soil sorbent to trap over 98 percent of sulfur gases and about two-thirds of halide gases evolved during hydrogen reduction of lunar soils. LSCS soil sorbent is based on lunar minerals containing iron and calcium compounds that trap sulfur and halide gas contaminants in a fixed-bed reactor held at temperatures between 250 and 400 C, allowing moisture produced during reduction to pass through in vapor phase. Small amounts of Earth-based polishing sorbents consisting of zinc oxide and sodium aluminate are used to reduce contaminant concentrations to one ppm or less. The preferred LSCS configuration employs lunar soil beneficiation to boost concentrations of reactive sorbent minerals. Lunar soils contain sulfur in concentrations of about 0.1 percent, and halogen compounds including chlorine and fluorine in concentrations of about 0.01 percent. These contaminants are released as gases such as H2S, COS, CS2,HCl, and HF during thermal ISRU processing with hydrogen or other reducing gases. Removal of contaminant gases is required during ISRU processing to prevent hardware corrosion, electrolyzer damage, and catalyst poisoning. The use of Earth-supplied, single-use consumables to entirely remove contaminants at the levels existing in lunar soils would make many ISRU processes unattractive due to the large mass of consumables relative to the mass of oxygen produced. The LSCS concept of using a primary sorbent prepared from lunar soil was identified as a method by which the majority of contaminants could be removed from process gas streams, thereby substantially reducing the required mass of Earth-supplied consumables. The LSCS takes advantage of minerals containing iron and calcium compounds that are present in lunar soil to trap sulfur and halide gases in a fixedbed reactor downstream of an in-ISRU process such as hydrogen reduction. The lunar-soil-sorbent trap is held at a temperature significantly lower than the operating temperature of the hydrogen reduction or other ISRU process in order to maximize capture of contaminants, but is held at a high enough temperature to allow moisture to pass through without condensing. The lunar soil benefits from physical beneficiation to remove ultrafine particles (to reduce pressure drop through a fixed bed reactor) and to upgrade concentrations of iron and/or calcium compounds (to improve reactivity with gaseous contaminants).

CLOSED-LOOP STRIPPING ANALYSIS (CLSA) OF ...

EPA Pesticide Factsheets

Synthetic musk compounds are used as inexpensive fragrance materials for the production of perfumes and as additives to soap, detergent, and shampoo. They have been found in surface water, fish tissues, and human breast milk. The ubiquity of this class of compounds in the environment is attributable to high use and release into the environment. Current techniques for separating these compounds from fish tissues require tedious sample clean-up procedures. To obtain fat-free extracts, gel permeation chromatography (GPC), column chromatography using alumina, and silica gel, and thin layer chromatography (TLC clean-up procedures are frequently employed. Despite the considerable effort and resources devoted to these processes, a fraction of the lipids and lipid-like compounds frequently remains in the extracts. These low-level lipids foul injection liners, contaminate columns, and yield elevated baselines during gas chromatographic analysis of synthetic musk compounds. In this study, a simple method for the determination of synthetic musk compounds in fish tissues has been developed. Closed-loop stripping of saponified fish tissues in a I -L Wheaton purge- and-trap vessel, is used to strip compounds with high vapor pressures such as synthetic musks from the matrix onto a solid sorbent (Abselut Nexus). This technique is useful for screening biological tissues that contain lipids for musk compounds. Analytes are desorbed from the sorbent trap sequentially with polar an

Sulphation of CaO-Based Sorbent Modified in CO2 Looping Cycles

NASA Astrophysics Data System (ADS)

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, <35%, resulting in sulphation conversion of spent samples <30%, significantly lower than for the original sample (45%). These results showed that spent sorbent samples from CO2 looping cycles can be used as sorbents for SO2 retention if significant porosity loss does not occur during CO2 reaction cycles. For spent Kelly Rock and Katowice samples final conversions are determined by the total pore volume available for the bulky CaSO4 product.

Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry.

PubMed

Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel

2016-08-12

A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (β-blockers, β-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75μg/kg and 0.02-62.50μg/kg, respectively. Recoveries for 15 of the target analytes ranged from 71 to 98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples. Copyright © 2016 Elsevier B.V. All rights reserved.

6S Return Samples: Assessment of Air Quality in the International Space Station (ISS) Based on Solid Sorbent Air Sampler (SSAS) and Formaldehyde Monitoring Kit (FMK) Analyses

NASA Technical Reports Server (NTRS)

James, John T.

2004-01-01

The toxicological assessments of SSAS and FMK analytical results are reported. Analytical methods have not changed from earlier reports. Surrogate standard recoveries from the SSAS tubes were 66-76% for 13C-acetone, 85-96% for fluorobenzene, and 73-89% for chlorobenzene. Post-flight flows were far below pre-flight flows and an investigation of the problem revealed that the reduced flow was caused by a leak at the interface of the pump inlet tube and the pump head. This resulted in degradation of pump efficiency. Further investigation showed that the problem occurred before the SSAS was operated on orbit and that use of the post-flight flows yielded consistent and useful results. Recoveries from formaldehyde control badges were 86 to 104%. The two general criteria used to assess air quality are the total-non-methane-volatile organic hydrocarbons (NMVOCs) and the total T-value (minus the CO2 and formaldehyde contributions). The T values will not be reported for these data due to the flow anomaly. Control of atmospheric alcohols is important to the water recovery system engineers, hence total alcohols (including acetone) are also shown for each sample. Octafluoropropane (OFP) is not efficiently trapped by the sorbents used in the SSAS. Because formaldehyde is quantified from sorbent badges, its concentration is also listed separately. These five indices of air quality are summarized.

Application of multiwalled carbon nanotubes as sorbents for the extraction of mycotoxins in water samples and infant milk formula prior to high performance liquid chromatography mass spectrometry analysis.

PubMed

Socas-Rodríguez, Bárbara; González-Sálamo, Javier; Hernández-Borges, Javier; Rodríguez Delgado, Miguel Ángel

2016-05-01

In this work, a simple and environmental friendly methodology has been developed for the analysis of a group of six mycotoxins with estrogenic activity produced by Fusarium species (i.e. zearalanone, zearalenone, α-zearalanol, β-zearalanol, α-zearalenol, and β-zearalenol), using microdispersive SPE the symbol micro should de before dSPE with multiwalled carbon nanotubes as sorbent. Separation, determination, and quantification were achieved by HPLC coupled to ion trap MS with an ESI interface. Parameters affecting the extraction efficiency of µ-dSPE such as pH of the sample, amount of multiwalled carbon nanotubes, and type and volume of elution solvent, were studied and optimized. The methodology was validated for mineral, pond, and wastewater as well as for powdered infant milk using 17β-estradiol-2,4,16,16,17-d5 (17β-E2 -D5 ) as internal standard, obtaining recoveries ranging from 85 to 120% for the three types of water samples and from 77 to 115% for powdered infant milk. RSD values were lower than 10%. The LOQs achieved were in the range 0.05-2.90 μg/L for water samples and 2.02-31.9 μg/L for powdered infant milk samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An insight into the determination of trace levels of benzodiazepines in biometric systems: Use of crab shell powder as an environmentally friendly biosorbent.

PubMed

Samadi, Fatemeh; Sarafraz-Yazdi, Ali; Es'haghi, Zarrin

2018-05-30

A vortex assisted dispersive solid phase extraction approach (VADSPE) based on crab shell powder as biodegradable and biocompatible μ-sorbent was developed for simultaneous analysis of three benzodiazepines (BZPs): Oxazepam, Flurazepamand Diazepam, in biological matrixes included blood, nail, hair and urine samples. The effective parameters in VADSPE process, including the volume of uptake solvent, the dosage of sorbent, extraction time and back extraction time, were optimized using response surface methodology(RSM) based on central composite design(CCD). The suggested technique allows successful trapping of BZPs in a single-step extraction. Under the optimized extraction conditions, the proposed approach was exhibited low limits of detection (0.003-1.2 μg·mL -1 ), an acceptable linearity (0.04-20 μg·mL -1 ). Method performance was assessed by recovery experiments at spiking levels of 10 μg·mL -1 (n = 5) for BZPs in blood, nail, hair and urine samples. Relative recoveries were determined by HPLC, which were between 36%and 95.6%. Copyright © 2018. Published by Elsevier B.V.

Sample Enrichment for Bioanalytical Assessment of Disinfected Drinking Water: Concentrating the Polar, the Volatiles, and the Unknowns.

PubMed

Stalter, Daniel; Peters, Leon I; O'Malley, Elissa; Tang, Janet Yat-Man; Revalor, Marion; Farré, Maria José; Watson, Kalinda; von Gunten, Urs; Escher, Beate I

2016-06-21

Enrichment methods used in sample preparation for the bioanalytical assessment of disinfected drinking water result in the loss of volatile and hydrophilic disinfection byproducts (DBPs) and hence likely tend to underestimate biological effects. We developed and evaluated methods that are compatible with bioassays, for extracting nonvolatile and volatile DBPs from chlorinated and chloraminated drinking water to minimize the loss of analytes. For nonvolatile DBPs, solid-phase extraction (SPE) with TELOS ENV as solid phase performed superior compared to ten other sorbents. SPE yielded >70% recovery of nonpurgeable adsorbable organic halogens (AOX). For volatile DBPs, cryogenic vacuum distillation performed unsatisfactorily. Purge and cold-trap with crushed ice serving as condensation nuclei achieved recoveries of 50-100% for trihalomethanes and haloacetonitriles and approximately 60-90% for purged AOX from tap water. We compared the purgeable versus the nonpurgeable fraction by combining purge-and-trap extraction with SPE. The purgeable DBP fraction enriched with the purge-and-trap method exerted a lower oxidative stress response in mammalian cells than the nonpurgeable DBPs enriched with SPE after purging, while contributions of both fractions to bacterial cytotoxicity was more variable. 37 quantified DBPs explained almost the entire AOX in the purge-and-trap extracts, but <16% in the SPE extracts demonstrating that the nonpurgeable fraction is dominated by unknown DBPs.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Manovic, V.; Anthony, E.J.; Loncarevic, D.

CaO-based looping cycles are promising processes for CO{sub 2} Capture from both syngas and flue gas. The technology is based on cyclical carbonation of CaO and regeneration of CaCO{sub 3} in a dual fluidized-bed reactor to produce a pure CO{sub 2} stream suitable for sequestration. Use of spent sorbent from CO{sub 2} looping cycles for SO{sub 2} capture is investigated. Three limestones were investigated: Kelly Rock (Canada), La Blanca (Spain), and Katowice (Poland, Upper Silesia). Carbonation/calcination cycles were performed in a tube furnace with both the original limestones and samples thermally pretreated for different times (i.e., sintered). The spent sorbentmore » samples were sulfated in a thermogravimetric analyzer (TGA). The changes in the resulting sorbent pore structure were then investigated using mercury porosimetry. It has been shown that the sulfation rates of both thermally pretreated and spent sorbent samples are lower in comparison with those of the original samples. However, final conversions of both spent and pretreated sorbents after longer sulfation time were comparable or higher than those observed for the original sorbents under comparable conditions. Maximum sulfation levels strongly depend on sorbent porosity and pore surface area. The results showed that spent sorbent samples from CO{sub 2} looping cycles can be used as sorbents for SO{sub 2} retention in cases where significant porosity loss does not occur during CO{sub 2} reaction cycles. In the case of spent Kelly Rock and Katowice samples, sorbent particles are practically uniformly sulfated, achieving final conversions that are determined by the total pore volume available for the bulky CaSO{sub 4} product.« less

Needle Trap Device as a New Sampling and Preconcentration Approach for Volatile Organic Compounds of Herbal Medicines and its Application to the Analysis of Volatile Components in Viola tianschanica.

PubMed

Qin, Yan; Pang, Yingming; Cheng, Zhihong

2016-11-01

The needle trap device (NTD) technique is a new microextraction method for sampling and preconcentration of volatile organic compounds (VOCs). Previous NTD studies predominantly focused on analysis of environmental volatile compounds in the gaseous and liquid phases. Little work has been done on its potential application in biological samples and no work has been reported on analysis of bioactive compounds in essential oils from herbal medicines. The main purpose of the present study is to develop a NTD sampling method for profiling VOCs in biological samples using herbal medicines as a case study. A combined method of NTD sample preparation and gas chromatography-mass spectrometry was developed for qualitative analysis of VOCs in Viola tianschanica. A 22-gauge stainless steel, triple-bed needle packed with Tenax, Carbopack X and Carboxen 1000 sorbents was used for analysis of VOCs in the herb. Furthermore, different parameters affecting the extraction efficiency and capacity were studied. The peak capacity obtained by NTDs was 104, more efficient than those of the static headspace (46) and hydrodistillation (93). This NTD method shows potential to trap a wide range of VOCs including the lower and higher volatile components, while the static headspace and hydrodistillation only detects lower volatile components, and semi-volatile and higher volatile components, respectively. The developed NTD sample preparation method is a more rapid, simpler, convenient, and sensitive extraction/desorption technique for analysis of VOCs in herbal medicines than the conventional methods such as static headspace and hydrodistillation. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

SO2 retention by reactivated CaO-based sorbent from multiple CO2 capture cycles.

PubMed

Manovic, Vasilije; Anthony, Edward J

2007-06-15

This paper examines the reactivation of spent sorbent, produced from multiple CO2 capture cycles, for use in SO2 capture. CaO-based sorbent samples were obtained from Kelly Rock limestone using three particle size ranges, each containing different impurities levels. Using a thermogravimetric analyzer (TGA), the sulfation behavior of partially sulfated and unsulfated samples obtained after multiple calcination-carbonation cycles in a tube furnace (TF), following steam reactivation in a pressurized reactor, is examined. In addition, samples calcined/sintered under different conditions after hydration are also examined. The results show that suitably treated spent sorbent has better sulfation characteristics than that of the original sorbent. Thus for example, after 2 h sulfation, > 80% of the CaO was sulfated. In addition, the sorbent showed significant activity even after 4 h when > 95% CaO was sulfated. The results were confirmed by X-ray diffraction (XRD) analysis, which showed that, by the end of the sulfation process, samples contained CaSO4 with only traces of unreacted CaO. The superior behavior of spent reactivated sorbent appears to be due to swelling of the sorbent particles during steam hydration. This enables the development of a more suitable pore surface area and pore volume distribution for sulfation, and this has been confirmed by N2 adsorption-desorption isotherms and the Barrett-Joyner-Halenda (BJH) method. The surface area morphology of sorbent after reactivation was examined by scanning electron microscopy (SEM). Ca(OH)2 crystals were seen, which displayed their regular shape, and their elemental composition was confirmed by energy-dispersive X-ray (EDX) analysis. The improved characteristics of spent reactivated sorbent in comparison to the original and to the sorbent calcined under different conditions and hydrated indicate the beneficial effect of CO2 cycles on sorbent reactivation and subsequent sulfation. These results allow us to propose a new process for the use of CaO-based sorbent in fluidized bed combustion (FBC) systems, which incorporates CO2 capture, sorbent reactivation, and SO2 retention.

Research on using Mineral Sorbents for A Sorption Process in the Environment Contaminated with Petroleum Substances

NASA Astrophysics Data System (ADS)

Pijarowski, Piotr Marek; Tic, Wilhelm Jan

2014-06-01

A research on diatomite sorbents was carried out to investigate their ability to remove hazardous substances from oil spillages. We used two types of sorbents available on the market with differences in material density and particles size of composition. As sorbents we used Ekoterm oil and unleaded petrol 95 coming from refinery PKN Orlen S.A. Two types of sorbents with similar chemical composition but different granulometric composition were used. They are marked as D1 and C1 samples. The fastest absorbent was C1, but D1 sample was the most absorptive.

Tank vapor characterization project. Headspace vapor characterization of Hanford waste tank 241-BY-108: Second comparison study results from samples collected on 3/28/96

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas, B.L.; Pool, K.H.; Evans, J.C.

1997-01-01

This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H{sub 2}O) and ammonia (NH{sub 3}), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA{trademark} canisters and on triple sorbent traps (TSTs).more » Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC.« less

Time-Dependent CO[subscript 2] Sorption Hysteresis in a One-Dimensional Microporous Octahedral Molecular Sieve

DOE Office of Scientific and Technical Information (OSTI.GOV)

Espinal, Laura; Wong-Ng, Winnie; Kaduk, James A.

2014-09-24

The development of sorbents for next-generation CO{sub 2} mitigation technologies will require better understanding of CO{sub 2}/sorbent interactions. Among the sorbents under consideration are shape-selective microporous molecular sieves with hierarchical pore morphologies of reduced dimensionality. We have characterized the non-equilibrium CO{sub 2} sorption of OMS-2, a well-known one-dimensional microporous octahedral molecular sieve with manganese oxide framework. Remarkably, we find that the degree of CO{sub 2} sorption hysteresis increases when the gas/sorbent system is allowed to equilibrate for longer times at each pressure step. Density functional theory calculations indicate a 'gate-keeping' role of the cation in the tunnel, only allowing CO{submore » 2} molecules to enter fully into the tunnel via a highly unstable transient state when CO{sub 2} loadings exceed 0.75 mmol/g. The energy barrier associated with the gate-keeping effect suggests an adsorption mechanism in which kinetic trapping of CO{sub 2} is responsible for the observed hysteretic behavior.« less

Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

PubMed

Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

2014-05-21

In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

40 CFR 75.84 - Recordkeeping and reporting.

Code of Federal Regulations, 2010 CFR

2010-07-01

... (CONTINUED) CONTINUOUS EMISSION MONITORING Hg Mass Emission Provisions § 75.84 Recordkeeping and reporting... Federal Hg mass emission reduction program”; (2) The information required in § 75.58(b)(3), for units with... or sorbent trap monitoring systems, for each hour when the unit is operating, record the Hg mass...

Facility monitoring of chemical warfare agent simulants in air using an automated, field-deployable, miniature mass spectrometer.

PubMed

Smith, Jonell N; Noll, Robert J; Cooks, R Graham

2011-05-30

Vapors of four chemical warfare agent (CWA) stimulants, 2-chloroethyl ethyl sulfide (CEES), diethyl malonate (DEM), dimethyl methylphosphonate (DMMP), and methyl salicylate (MeS), were detected, identified, and quantitated using a fully automated, field-deployable, miniature mass spectrometer. Samples were ionized using a glow discharge electron ionization (GDEI) source, and ions were mass analyzed with a cylindrical ion trap (CIT) mass analyzer. A dual-tube thermal desorption system was used to trap compounds on 50:50 Tenax TA/Carboxen 569 sorbent before their thermal release. The sample concentrations ranged from low parts per billion [ppb] to two parts per million [ppm]. Limits of detection (LODs) ranged from 0.26 to 5.0 ppb. Receiver operating characteristic (ROC) curves are presented for each analyte. A sample of CEES at low ppb concentration was combined separately with two interferents, bleach (saturated vapor) and diesel fuel exhaust (1%), as a way to explore the capability of detecting the simulant in an environmental matrix. Also investigated was a mixture of the four CWA simulants (at concentrations in air ranging from 270 to 380 ppb). Tandem mass (MS/MS) spectral data were used to identify and quantify the individual components. Copyright © 2011 John Wiley & Sons, Ltd.

Development of Carbotrap B-packed needle trap device for determination of volatile organic compounds in air.

PubMed

Poormohammadi, Ali; Bahrami, Abdulrahman; Farhadian, Maryam; Ghorbani Shahna, Farshid; Ghiasvand, Alireza

2017-12-08

Carbotrap B as a highly pure surface sorbent with excellent adsorption/desorption properties was packed into a stainless steel needle to develop a new needle trap device (NTD). The performance of the prepared NTD was investigated for sampling, pre-concentration and injection of benzene, toluene, ethyl benzene, o-xylene, and p-xylene (BTEX) into the column of gas chromatography-mass spectrometry (GC-MS) device. Response surface methodology (RSM) with central composite design (CCD) was also employed in two separate consecutive steps to optimize the sampling and device parameters. First, the sampling parameters such as sampling temperature and relative humidity were optimized. Afterwards, the RSM was used for optimizing the desorption parameters including desorption temperature and time. The results indicated that the peak area responses of the analytes of interest decreased with increasing sampling temperature and relative humidity. The optimum values of desorption temperature were in the range 265-273°C, and desorption time were in the range 3.4-3.8min. The limits of detection (LODs) and limits of quantitation (LOQs) of the studied analytes were found over the range of 0.03-0.04ng/mL, and 0.1-0.13ng/mL, respectively. These results demonstrated that the NTD packed with Carbotrap B offers a high sensitive procedure for sampling and analysis of BTEX in concentration range of 0.03-25ng/mL in air. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of carrier properties on surface characteristics of sorbents modified with acetylacetonates Ni (II), Cu (II)

NASA Astrophysics Data System (ADS)

Faustova, Zhanna; Matveeva, Tatiana; Slizhov, Yuriy

2017-11-01

Sorbents based on Chromaton N-AW with layers of mesoporous silica gel modified with acetylacetonate nickel (II) and copper (II) were obtained. The porous structure of sorbents based on synthesized silica gel and industrial samples of Chromaton N, Silipore 075, Silochrom C-120 was studied. All studied samples are mesoporous. For sorbents based on commercially available Chromaton N, Silipore 075, and Silochrome 120, the mesopore dimensions vary in a wide range from 10 to 50 nm. For synthesized silica gel and chelate-containing sorbents, a narrower pore distribution is observed in the range of 5-15 nm, which indicates the uniformity of its surface. A comparative analysis of the effect of carrier properties on the acid-base properties of the surface of chelate-containing sorbents is carried out. The acid-base nature of the modifier is more pronounced in the case of synthesized silica gel by the sol-gel method.

Efficient sample preparation method based on solvent-assisted dispersive solid-phase extraction for the trace detection of butachlor in urine and waste water samples.

PubMed

Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

2016-10-01

In this work, an efficient sample preparation method termed solvent-assisted dispersive solid-phase extraction was applied. The used sample preparation method was based on the dispersion of the sorbent (benzophenone) into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was achieved by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the butachlor, the cloudy solution was centrifuged and butachlor in the sediment phase dissolved in ethanol and determined by gas chromatography with flame ionization detection. Under the optimized conditions (solution pH = 7.0, sorbent: benzophenone, 2%, disperser solvent: ethanol, 500 μL, centrifuged at 4000 rpm for 3 min), the method detection limit for butachlor was 2, 3 and 3 μg/L for distilled water, waste water, and urine sample, respectively. Furthermore, the preconcentration factor was 198.8, 175.0, and 174.2 in distilled water, waste water, and urine sample, respectively. Solvent-assisted dispersive solid-phase extraction was successfully used for the trace monitoring of butachlor in urine and waste water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Low acetaldehyde collection efficiencies for 24-hour sampling with 2,4-dinitrophenylhydrazine (DNPH)-coated solid sorbents.

PubMed

Herrington, Jason S; Fan, Zhi-Hua Tina; Lioy, Paul J; Zhang, Junfeng Jim

2007-01-15

Airborne aldehyde and ketone (carbonyl) sampling methodologies based on derivatization with 2,4-dinitrophenylhydrazine (DNPH)-coated solid sorbents could unequivocally be considered the "gold" standard. Originally developed in the late 1970s, these methods have been extensively evaluated and developed up to the present day. However, these methods have been inadequately evaluated for the long-term (i.e., 24 h or greater) sampling collection efficiency (CE) of carbonyls other than formaldehyde. The current body of literature fails to demonstrate that DNPH-coated solid sorbent sampling methods have acceptable CEs for the long-term sampling of carbonyls other than formaldehyde. Despite this, such methods are widely used to report the concentrations of multiple carbonyls from long-term sampling, assuming approximately 100% CEs. Laboratory experiments were conducted in this study to evaluate the long-term formaldehyde and acetaldehyde sampling CEs for several commonly used DNPH-coated solid sorbents. Results from sampling known concentrations of formaldehyde and acetaldehyde generated in a dynamic atmosphere generation system demonstrate that the 24-hour formaldehyde sampling CEs ranged from 83 to 133%, confirming the findings made in previous studies. However, the 24-hour acetaldehyde sampling CEs ranged from 1 to 62%. Attempts to increase the acetaldehyde CEs by adding acid to the samples post sampling were unsuccessful. These results indicate that assuming approximately 100% CEs for 24-hour acetaldehyde sampling, as commonly done with DNPH-coated solid sorbent methods, would substantially under estimate acetaldehyde concentrations.

Application of ultradisperse magnetic adsorbents for removal of small concentrations of pollutants from large volumes of water

NASA Astrophysics Data System (ADS)

Nechitailo, Galina S.; Kuznetsov, Anatoli; Kuznetsov, Oleg

2016-07-01

Pollution of natural bodies of water (rivers, lakes, ground water, etc) is unfortunately very common, both from natural sources like volcanic activity; and, even more importantly, from human activity, including disposal of industrial and municipal waste, mining, etc. Many toxic substances are harmful for humans and other organisms even in very low concentrations (e.g., less than 1 µg/L of cadmium is harmful, for Hg it is 0.5 µg/L, for phenol - 1 µg/L), and can remain in water for decades or longer. Cleaning large volumes of water even from low concentrations of pollutants is a challenging technological task and is very expensive. We propose to use suspension of ultradisperse magnetic adsorbents, for example, nanostructured ferro-carbon particles, produced by plasmachemical technique, for removing small concentrations of pollutants from large volumes of water. The suspension is introduced into the water. Due to their small sizes and densities similar to water (we measured the density of FC-4 ferro-carbon to be about 1 g/cm3; presumably due to porosity) the particles do not sediment for a long time (hours, days or longer), move due to Brownian motion and adsorb a variety of substances from the water. The particle surface can be modified to provide selectivity of the adsorption. Sorption capacities of ferro-carbon adsorbents is in dozens of percent. Therefore, to collect 1 kg of a pollutant, 2 to 20 kg of the adsorbents is required. Then the particles with the adsorbed contaminant can be collected (e.g., downstream of the river) using a variety of magnetic traps. The traps can consist of ferromagnetic wires and permanent magnets, a variety of simple and inexpensive designs are available. As a model system, the kinetics of adsorption of a highly diluted (0.002 mg/ml) aqueous solution of a low molecular weight compound (toluidine blue) by a small concentration of a ferro-carbon powder (FC-4) was studied by spectrophotometry. Before each measurement, the particles with the adsorbed toluidine blue were removed from the solution by magnetic separation. The sorbent was proven to have high sorption capacity and rapid adsorption kinetics for toluidine blue. These experiments demonstrated the validity of the method, where a small concentration of a pollutant was successfully collected from a large volume of water. By varying the ratio of the sorbent/pollutant, it is possible to optimize the sorbent use and the time required to adsorb all pollutant present in the treated water. A variety of magnetically controlled sorbents can be designed and used in this method, from broad-spectrum adsorbing sorbents to sorbents specifically targeting a particular pollutant. These sorbents can be used either individually or as mixtures of sorbents with different properties, depending on the desired purification goals. Simplicity and scalability of this method allow a variety of ecological applications, as well as industrial ones, from process water purification to wastewater treatment.

Poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles as sorbents for the analysis of sodium benzoate in beverages.

PubMed

Ji, Shilei; Li, Nan; Qi, Li; Wang, Minglin

2017-01-01

In this study, poly(styrene-co-N-methacryloyl-l-phenylalanine methyl ester)-functionalized magnetic nanoparticles were constructed and used as magnetic solid-phase extraction sorbents for analysis of food preservatives in beverages. To prepare the poly(amino acid)-based sorbents, N-methacryloyl-l-phenylalanine methyl ester, and styrene served as the functional monomers and modified onto the magnetic nanoparticles via free radical polymerization. Interestingly, compared with propylparaben and potassium sorbate, the proposed poly(amino acid)-based sorbents showed a good selectivity to sodium benzoate. The adsorption capacity of the sorbents to sodium benzoate was 6.08 ± 0.31 mg/g. Moreover, the fast adsorption equilibrium could be reached within 5 min. Further, the resultant poly(amino acid)-based sorbents were applied in the analysis of sodium benzoate in real beverage samples. The results proved that the proposed magnetic solid-phase extraction sorbents have a great potential for the analysis of preservatives in food samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

REDUCTION OF COAL-BASED METAL EMISSIONS BY FURNACE SORBENT INJECTION

EPA Science Inventory

The ability of sorbent injection technology to reduce the potential for trace metal emissions from coal combustion was researched. Pilot scale tests of high-temperature furnace sorbent injection were accompanied by stack sampling for coal-based, metallic air toxics. Tested sorben...

Noninvasive analysis of volatile biomarkers in human emanations for health and early disease diagnosis.

PubMed

Kataoka, Hiroyuki; Saito, Keita; Kato, Hisato; Masuda, Kazufumi

2013-06-01

Early disease diagnosis is crucial for human healthcare and successful therapy. Since any changes in homeostatic balance can alter human emanations, the components of breath exhalations and skin emissions may be diagnostic biomarkers for various diseases and metabolic disorders. Since hundreds of endogenous and exogenous volatile organic compounds (VOCs) are released from the human body, analysis of these VOCs may be a noninvasive, painless, and easy diagnostic tool. Sampling and preconcentration by sorbent tubes/traps and solid-phase microextraction, in combination with GC or GC-MS, are usually used to analyze VOCs. In addition, GC-MS-olfactometry is useful for simultaneous analysis of odorants and odor quality. Direct MS techniques are also useful for the online real-time detection of VOCs. This review focuses on recent developments in sampling and analysis of volatile biomarkers in human odors and/or emanations, and discusses future use of VOC analysis.

40 CFR 63.10009 - May I use emissions averaging to comply with this subpart?

Code of Federal Regulations, 2014 CFR

2014-07-01

... performance test must not be less than the design efficiency of the emissions control technology employed 180... properties, belonging to a single major industrial grouping, which are under common control of the same person (or persons under common control); and (ii) You use CEMS (or sorbent trap monitoring systems for...

40 CFR 63.10009 - May I use emissions averaging to comply with this subpart?

Code of Federal Regulations, 2012 CFR

2012-07-01

... performance test must not be less than the design efficiency of the emissions control technology employed 180... properties, belonging to a single major industrial grouping, which are under common control of the same person (or persons under common control); and (ii) You use CEMS (or sorbent trap monitoring systems for...

In situ trapping of As, Sb and Se hydrides on nanometer-sized ceria-coated iron oxide-silica and slurry suspension introduction to ICP-OES.

PubMed

Dados, A; Kartsiouli, E; Chatzimitakos, Th; Papastephanou, C; Stalikas, C D

2014-12-01

A procedure is developed for the analysis of sub-μg L(-1) levels of arsenic, antimony and selenium after preconcentration of their hydrides. The study highlights the capability of an aqueous suspension of a nanometer-sized magnetic ceria, in the presence of iodide, to function as a sorbent for the in situ trapping and preconcentration of the hydrides of certain metalloids. After extraction, the material is magnetically separated from the trapping solution and analyzed. A slurry suspension sampling approach with inductively coupled plasma-optical emission spectrometry (ICP-OES) is employed for measurements, as the quantitative elution of the adsorbed metalloids is not feasible. The whole analytical procedure consists of five steps: (i) pre-reduction of As, Sb and Se, (ii) generation of the hydrides AsH3, SbH3 and SeH2, (iii) in situ collection in the trapping suspension of magnetic ceria, (iv) isolation of the particles by applying a magnetic field, and (v) measurement of As, Sb and Se concentrations using ICP-OES. Under the established experimental conditions, the efficiency of trapping accounted for 94 ± 2%, 89 ± 2% and 98 ± 3% for As, Sb and Se, respectively, signifying the effective implementation of the overall procedure. The applicability of the procedure has been demonstrated by analyzing tap and lake water and a reference material (soft drinking water). The obtained analytical figures of merit were satisfactory for the analysis of the above metalloids in natural waters by ICP-OES. Copyright © 2014 Elsevier B.V. All rights reserved.

Chemical analysis of whale breath volatiles: a case study for non-invasive field health diagnostics of marine mammals.

PubMed

Cumeras, Raquel; Cheung, William H K; Gulland, Frances; Goley, Dawn; Davis, Cristina E

2014-09-12

We explored the feasibility of collecting exhaled breath from a moribund gray whale (Eschrichtius robustus) for potential non-invasive health monitoring of marine mammals. Biogenic volatile organic compound (VOC) profiling is a relatively new field of research, in which the chemical composition of breath is used to non-invasively assess the health and physiological processes on-going within an animal or human. In this study, two telescopic sampling poles were designed and tested with the primary aim of collecting whale breath exhalations (WBEs). Once the WBEs were successfully collected, they were immediately transferred onto a stable matrix sorbent through a custom manifold system. A total of two large volume WBEs were successfully captured and pre-concentrated onto two Tenax®-TA traps (one exhalation per trap). The samples were then returned to the laboratory where they were analyzed using solid phase micro extraction (SPME) and gas chromatography/mass spectrometry (GC/MS). A total of 70 chemicals were identified (58 positively identified) in the whale breath samples. These chemicals were also matched against a database of VOCs found in humans, and 44% of chemicals found in the whale breath are also released by healthy humans. The exhaled gray whale breath showed a rich diversity of chemicals, indicating the analysis of whale breath exhalations is a promising new field of research.

Determination of decamethylcyclopentasiloxane in air using commercial solid phase extraction cartridges.

PubMed

Kierkegaard, Amelie; McLachlan, Michael S

2010-05-21

Decamethylcyclopentasiloxane (D(5)), a high production volume chemical used in personal care products, has been designated for regulation in Canada and is under review in the EU because of concerns about its persistence and potential for bioaccumulation in the environment. D(5) is a volatile compound expected to be found primarily in air, but there is little information on atmospheric concentrations due to the lack of sensitive analytical methods. Here a simple and sensitive method to determine D(5) in ambient air is presented. The challenge in the environmental analysis of D(5) is avoiding contamination. Our method is based on the high trapping efficiency of the sorbent Isolute ENV+, combined with a comparably high sampling rate. A small amount of sorbent (10 mg) is eluted in a small volume of n-hexane (0.1-0.6 mL), which is injected onto a GC/MS system without further processing. The simplicity of the method enables the use of a field blank for every sample to trace contamination. The method provides low limits of quantification (approximately 0.3 ng/m(3)), good repeatability and limited breakthrough (approximately 1%). By lowering the limit of quantification compared to published work by almost two orders of magnitude, it became possible to quantify D(5) in ambient air at locations remote from strong point sources. The concentrations at a rural Swedish site ranged from 0.7 to 8 ng/m(3) over a period of 4 months. 2010 Elsevier B.V. All rights reserved.

Novel sample preparation technique with needle-type micro-extraction device for volatile organic compounds in indoor air samples.

PubMed

Ueta, Ikuo; Mizuguchi, Ayako; Fujimura, Koji; Kawakubo, Susumu; Saito, Yoshihiro

2012-10-09

A novel needle-type sample preparation device was developed for the effective preconcentration of volatile organic compounds (VOCs) in indoor air before gas chromatography-mass spectrometry (GC-MS) analysis. To develop a device for extracting a wide range of VOCs typically found in indoor air, several types of particulate sorbents were tested as the extraction medium in the needle-type extraction device. To determine the content of these VOCs, air samples were collected for 30min with the packed sorbent(s) in the extraction needle, and the extracted VOCs were thermally desorbed in a GC injection port by the direct insertion of the needle. A double-bed sorbent consisting of a needle packed with divinylbenzene and activated carbon particles exhibited excellent extraction and desorption performance and adequate extraction capacity for all the investigated VOCs. The results also clearly demonstrated that the proposed sample preparation method is a more rapid, simpler extraction/desorption technique than traditional sample preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Evaluation of a portable gas chromatograph with photoionization detector under variations of VOC concentration, temperature, and relative humidity.

PubMed

Soo, Jhy-Charm; Lee, Eun Gyung; LeBouf, Ryan F; Kashon, Michael L; Chisholm, William; Harper, Martin

2018-04-01

The objective of this present study was to evaluate the performance of a portable gas chromatograph-photoionization detector (GC-PID), under various test conditions to determine if it could be used in occupational settings. A mixture of 7 volatile organic compounds (VOCs)-acetone, ethylbenzene, methyl isobutyl ketone, toluene, m-xylene, p-xylene, and o-xylene-was selected because its components are commonly present in paint manufacturing industries. A full-factorial combination of 4 concentration levels (exposure scenarios) of VOC mixtures, 3 different temperatures (25°C, 30°C, and 35°C), and 3 relative humidities (RHs; 25%, 50%, and 75%) was conducted in a full-size controlled environmental chamber. Three repetitions were conducted for each test condition allowing for estimation of accuracy. Time-weighted average exposure data were collected using solid sorbent tubes (Anasorb 747, SKC Inc.) as the reference sampling medium. Calibration curves of Frog-4000 using the dry gases showed R 2 > 0.99 for all analytes except for toluene (R 2 = 0.97). Frog-4000 estimates within a test condition showed good consistency for the performance of repeated measurement. However, there was ∼41-64% reduction in the analysis of polar acetone with 75% RH relative to collection at 25% RH. Although Frog-4000 results correlated well with solid sorbent tubes (r = 0.808-0.993, except for toluene) most of the combinations regardless of analyte did not meet the <25% accuracy criterion recommended by NIOSH. The effect of chromatographic co-elution can be seen with m, p-xylene when the results are compared to the sorbent tube sampling technique with GC-flame ionization detector. The results indicated an effect of humidity on the quantification of the polar compounds that might be attributed to the pre-concentrator placed in the selected GC-PID. Further investigation may resolve the humidity effect on sorbent trap with micro GC pre-concentrator when water vapor is present. Although this instrument does not fulfill the accuracy criterion specified in the NIOSH technical report No. 2012-162, it can be used as a screening tool for range finding monitoring with dry gases calibration in the occupational setting rather than compliance monitoring.

Molecularly imprinted polymer online solid-phase extraction coupled with high-performance liquid chromatography-UV for the determination of three sulfonamides in pork and chicken.

PubMed

He, Jinxing; Wang, Shuo; Fang, Guozhen; Zhu, Huaping; Zhang, Yan

2008-05-14

A selective imprinted amino-functionalized silica gel sorbent was prepared by combining a surface molecular imprinting technique with a sol-gel process for online solid-phase extraction-HPLC determination of three trace sulfonamides in pork and chicken muscle. The imprinted functionalized silica gel sorbent exhibited selectivity and fast kinetics for the adsorption and desorption of sulfonamides. With a sample loading flow rate of 4 mL min (-1) for 12.5 min, enhancement factors and detection limits for three sulfonamides ( S/ N = 3) were achieved. The precision (RSD) for nine replicate online sorbent extractions of 5 microg L (-1) sulfonamides was less than 4.5%. The sorbent also offered good linearity ( r (2) > 0.99) for online solid-phase extraction of trace levels of sulfonamides. The method was applied to the determination of sulfonamides in pork and chicken muscle samples. The prepared polymer sorbent shows promise for online solid-phase extraction for HPLC determination of trace levels of sulfonamides in pork and chicken samples.

Outdoor air 1,3-butadiene monitoring: Comparison of performance of Radiello® passive samplers and active multi-sorbent bed tubes

NASA Astrophysics Data System (ADS)

Gallego, Eva; Teixidor, Pilar; Roca, Francisco Javier; Perales, José Francisco; Gadea, Enrique

2018-06-01

A comparison was made between the relative performance of active and passive sampling methods for the analysis of 1,3-butadiene in outdoor air. Active and passive sampling was conducted using multi-sorbent bed tubes (Carbotrap, Carbopack X, Carboxen 569) and RAD141 Radiello® diffusive samplers (filled with Carbopack X), respectively. Daily duplicate samples of multi-sorbent bed tubes were taken over a period of 14 days (9 + 5 days) at El Morell (Tarragona, Spain), near the petrochemical area. As 1,3-butadiene is a reactive pollutant and can be rapidly oxidized, half of the samplers were equipped with ozone scrubbers. Samples consisted in two tubes connected in series (front and back) to allow the determination of breakthrough. Quadruplicate samples of Radiello® tubes were taken over a period of 14 days (9 days and 5 days), too. During those days, ozone concentration was measured using RAD172 Radiello® samplers. In addition to this, daily duplicate samples of multi-sorbent bed tubes were taken in the city of Barcelona over a period of 8 days. Simultaneously, 4 samples of Radiello® tubes were exposed to outdoor air. Sampling was done throughout June and July 2017. Analysis was performed by thermal desorption coupled with gas chromatography/mass spectrometry. Analytical performance of the two sampling methods was evaluated by describing several quality assurance parameters, with results showing that performances are quite similar. They display low detection limits, good precision, linearity and desorption efficiency, low levels of blank values, and low breakthrough for multi-sorbent bed tubes. However, Radiello® samplers were not able to uptake episodic 1,3-butadiene high concentrations, leading to underestimation of real values. Hence, we can conclude that Radiello® samplers can be used for baseline 1,3-butadiene levels whereas multi-sorbent bed tubes would be advisable when relevant episodes are expected.

‘Fuji’ apple (Malus domestica Borkh) volatile production during high pCO2 controlled atmosphere storage

USDA-ARS?s Scientific Manuscript database

‘Fuji’apple [Malus sylvestris var. domestica (Borkh.) Mansf.] volatile compound dynamics were characterized during cold storage in air or at low pO2 controlled atmosphere (CA) with up to 5 kPa CO2. Volatile compounds in storage chambers were adsorbed onto solid sorbent traps and analyzed by GC-MS....

Development of magnetic micro-solid phase extraction for analysis of phthalate esters in packaged food.

PubMed

Makkliang, Fonthip; Kanatharana, Proespichaya; Thavarungkul, Panote; Thammakhet, Chongdee

2015-01-01

A novel, simple and low cost magnetic multi-walled carbon nanotubes-poly (vinyl alcohol) cryogel-micro-solid phase extraction (magnetic-MWCNTs-PVA cryogel-μ-SPE) sorbent was synthesized by incorporating magnetic particles and MWCNTs into a PVA cryogel. The magnetic-MWCNTs-PVA cryogel-μ-SPE sorbent developed, with a large surface area and macro-porous structure, provided good sorbent-to-sorbent reproducibility (%RSD<8) and each sorbent could be used up to 30 times (%RSD<6). This sorbent was applied for the extraction of dibutyl phthalate (DBP) and di-2-(ethylhexyl) phthalate (DEHP) in packaged food prior to analysis by gas chromatograph coupled with flame ionisation detector (GC-FID). The concentration of DBP and DEHP in hot-water samples from plastic bags were found in the range 0.04-0.15 μg mL(-1) and 0.03-0.20 μg mL(-1), respectively, but only DEHP was found in clear chicken soup samples in the range 0.02-0.07 μg mL(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

[Optimization of solid-phase extraction for enrichment of toxic organic compounds in water samples].

PubMed

Zhang, Ming-quan; Li, Feng-min; Wu, Qian-yuan; Hu, Hong-ying

2013-05-01

A concentration method for enrichment of toxic organic compounds in water samples has been developed based on combined solid-phase extraction (SPE) to reduce impurities and improve recoveries of target compounds. This SPE method was evaluated in every stage to identify the source of impurities. Based on the analysis of Waters Oasis HLB without water samples, the eluent of SPE sorbent after dichloromethane and acetone contributed 85% of impurities during SPE process. In order to reduce the impurities from SPE sorbent, soxhlet extraction of dichloromethane followed by acetone and lastly methanol was applied to the sorbents for 24 hours and the results had proven that impurities were reduced significantly. In addition to soxhlet extraction, six types of prevalent SPE sorbents were used to absorb 40 target compounds, the lgK(ow) values of which were within the range of 1.46 and 8.1, and recovery rates were compared. It was noticed and confirmed that Waters Oasis HLB had shown the best recovery results for most of the common testing samples among all three styrenedivinylbenzene (SDB) polymer sorbents, which were 77% on average. Furthermore, Waters SepPak AC-2 provided good recovery results for pesticides among three types of activated carbon sorbents and the average recovery rates reached 74%. Therefore, Waters Oasis HLB and Waters SepPak AC-2 were combined to obtain a better recovery and the average recovery rate for the tested 40 compounds of this new SPE method was 87%.

Comparison of methods for the measurement of mist and vapor from light mineral oil-based metalworking fluids.

PubMed

Simpson, Andrew T

2003-11-01

The measurement of oil mist derived from metalworking fluids formulated with light mineral oils can be highly inaccurate when using traditional filter sampling. This is due to evaporation of oil from the filter. In this work the practicability of an alternative approach measuring total oil mist and vapor was investigated. Combinations of inhalable particle samplers with backup sorbent vapor traps and standard vapor sampling on pumped and diffusive sorbent tubes were evaluated with gravimetric, infrared spectroscopic, and gas chromatographic analytical methods against the performance requirements of European Standard EN 482. An artificial aerosol was used to compare the methods against a reference method of filter sampler in series with three impingers. Multi-orifice samplers were used with standard 8-mm diameter charcoal tubes at 2 L/min without any signs of channelling or significant breakthrough, as were conical inhalable samplers with XAD-2 tubes at 1 L/min. Most combinations of samplers had a bias of less than 3 percent, but solitary pumped charcoal tubes underestimated total oil by 13 percent. Diffusive sampling was affected by impaction of mist particles and condensation of oil vapor. Gravimetric analysis of filters revealed significant potential sample loss during storage, with 4 percent being lost after one day when stored at room temperature and 2 percent when refrigerated. Samples left overnight in the balance room to equilibrate lost 24 percent. Infrared spectroscopy gave more precise results for vapor than gas chromatography (p = 0.002). Gas chromatography was less susceptible to bias from contaminating solvent vapors than infrared spectroscopy, but was still vulnerable to petroleum distillates. Under the specific test conditions (one oil type and mist particle size), all combinations of methods examined complied with the requirements of European Standard EN 484. Total airborne oil can be measured accurately; however, care must be taken to avoid contamination by hydrocarbon solvent vapors during sampling.

Single-step reinforced microextraction of polycyclic aromatic hydrocarbons from soil samples using an inside needle capillary adsorption trap with electropolymerized aniline/multi-walled carbon nanotube sorbent.

PubMed

Ghiasvand, Ali Reza; Yazdankhah, Fatemeh

2017-03-03

A polyaniline/multi-wall carbon nanotubes (PANI/MWCNT) composite was electrodeposited on the interior surface of a platinized stainless steel capillary needle and used to prepare an inside needle capillary adsorption trap (INCAT) device. The platinization expanded the interior adsorbing surface of the needle and made it more porous and cohesive for nanocomposite film. The nanocomposite was characterized using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). The fabricated INCAT was fixed into a cooling capsule to fabricate a cooling-assisted INCAT (CA-INCAT) system. The CA-INCAT device was used to extract polycyclic aromatic hydrocarbons (PAHs) from solid samples followed by gas chromatography-flame ionization detection (GC-FID) determination. To obtain the best extraction efficiency, the important experimental variables were studied and optimized. Under the optimal conditions, the limits of detection (LODs) for the studied PAHs were in the range of 0.002-0.02ngg -1 . Linear dynamic ranges (LDRs) for the calibration curves were found to be 0.1-30,000ngg -1 . Relative standard deviations (RSDs%) for six replicated analysis of 1ngg -1 PAHs were obtained 7.7-11%. The CA-INCAT-GC-FID method was successfully applied for the extraction and determination of PAHs in contaminated soil samples. The results were in agreement with those obtained by a validated ultrasound-assisted solvent extraction (UA-SE) method. Copyright © 2017 Elsevier B.V. All rights reserved.

Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

PubMed

Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

2016-06-01

Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microtrap assembly for greenhouse gas and air pollution monitoring

DOEpatents

Mitra, Somenath; Saridara, Chutarat

2015-08-25

A microtrap assembly includes a carbon nanotube sorbent. The microtrap assembly may be employed as a preconcentrator operable to deliver a sample to an analytical device to measure the concentrations of greenhouse gases. A system includes a microtrap having a carbon nanotube sorbent for measuring the concentrations of greenhouse gases in a sample.

Evaluation of layered double hydroxide/graphene hybrid as a sorbent in membrane-protected stir-bar supported micro-solid-phase extraction for determination of organochlorine pesticides in urine samples.

PubMed

Sajid, Muhammad; Basheer, Chanbasha; Daud, Muhammad; Alsharaa, Abdulnaser

2017-03-17

In this work, the potential of layered double hydroxide/graphene (LDH-G) hybrid as a sorbent for extraction and preconcentration of fifteen organochlorine pesticides (OCPs) in urine samples was evaluated. The LDH-G hybrid was synthesized by co-precipitation method and it was then characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The sorbent was then employed in membrane-protected stir-bar supported micro-solid-phase extraction (SB-μ-SPE) of OCPs in urine samples. This extraction approach is highly suitable for the samples representing matrix complexity such as urine because the sorbent is effectively protected inside the membrane. The extracted samples were analyzed by gas chromatography mass spectrometry. The factors that affect the performance of SB-μ-SPE were suitably optimized. This method demonstrated good linearity with coefficients of determination up to 0.9996. The limits of detection ranged between 0.22 and 1.38ngmL -1 . The RSD values for intra and inter-day precision were also in a satisfactory range (2.7-9.5%). Copyright © 2017 Elsevier B.V. All rights reserved.

Enantioseparation of Mandelic Acid Enantiomers With Magnetic Nano-Sorbent Modified by a Chiral Selector.

PubMed

Tarhan, Tuba; Tural, Bilsen; Tural, Servet; Topal, Giray

2015-11-01

In this study, R(+)-α-methylbenzylamine-modified magnetic chiral sorbent was synthesized and assessed as a new enantioselective solid phase sorbent for separation of mandelic acid enantiomers from aqueous solutions. The chemical structures and magnetic properties of the new sorbent were characterized by vibrating sample magnetometry, transmission electron microscopy, Fourier transform infrared spectroscopy, and dynamic light scattering. The effects of different variables such as the initial concentration of racemic mandelic acid, dosage of sorbent, and contact time upon sorption characteristics of mandelic acid enantiomers on magnetic chiral sorbent were investigated. The sorption of mandelic acid enantiomers followed a pseudo-second-order reaction and equilibrium experiments were well fitted to a Langmuir isotherm model. The maximum adsorption capacity of racemic mandelic acid on to the magnetic chiral sorbent was found to be 405 mg g(-1). The magnetic chiral sorbent has a greater affinity for (S)-(+)-mandelic acid compared to (R)-(-)-mandelic acid. The optimum resolution was achieved with 10 mL 30 mM of racemic mandelic acid and 110 mg of magnetic chiral sorbent. The best percent enantiomeric excess values (up to 64%) were obtained by use of a chiralpak AD-H column. © 2015 Wiley Periodicals, Inc.

Jet Engine Exhaust Analysis by Subtractive Chromatography

DTIC Science & Technology

1978-12-01

FID B response = oxygenates + aromatics. Oxygenated compounds with 8 Tenax GC Carbosieve B Glass Wool Glass wool Glass Wool Sample Flow Desoption...sorbent samplinq. During the process of compiling this information a new series of sorbent materials that show promising sorbent characteristics was...produced by a process which "carbonizes" a porous polymer material. The pro- duct is a hard, shiny, black-beaded material. The promotional literature

Proton-transfer reaction mass spectrometry (PTRMS) in combination with thermal desorption (TD) for sensitive off-line analysis of volatiles.

PubMed

Crespo, Elena; Devasena, Samudrala; Sikkens, Cor; Centeno, Raymund; Cristescu, Simona M; Harren, Frans J M

2012-04-30

When performing trace gas analysis, it is not always possible to bring the source of volatiles and the gas analyzer together. In these cases, volatile storage containers, such as thermal desorption (TD) tubes, can be used for off-line measurement. TD is routinely combined with gas chromatography/mass spectrometry (GC/MS), but so far not with proton-transfer reaction mass spectrometry (PTRMS), which has a faster response. A PTR-quadrupole-MS instrument and a PTR-ion-trap-MS instrument were separately coupled to a TD unit for off-line analysis of trace volatiles in air. Carbograph 1TD/Carbopack X sorbent tubes were filled with different concentrations of a trace gas mixture containing low molecular weight volatiles (32 g/mol up to 136 g/mol) and measured with the above-mentioned combinations. The carrier gas in the TD unit was changed from helium to nitrogen to be able to combine this instrument with the mass spectrometer. Good linearity and reproducibility with the amount of gas stored were obtained. The storage capacity over time (up to 14 days) showed larger variability (<11% for all compounds, except for acetone 27%). Several tubes were filled with breath of different persons, and the breath of a smoker showed increased levels of acetonitrile and benzene. The combination of the PTR ion-trap instrument with the TD unit was also investigated. Due to its higher sampling rate, the ion-trap system showed higher throughput capabilities than the quadrupole system. The combination of TD with PTRMS using both a quadrupole and an ion trap for off-line volatile analysis has been validated. TD tubes can be a robust and compact volatile storage method when the mass spectrometry and the sampling cannot be performed in the same place, for example in large screening studies. In addition, a higher measurement throughput than with GC/MS could be obtained. Copyright © 2012 John Wiley & Sons, Ltd.

Advances in organic-inorganic hybrid sorbents for the extraction of organic and inorganic pollutants in different types of food and environmental samples.

PubMed

Ng, Nyuk-Ting; Kamaruddin, Amirah Farhan; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Abdul Keyon, Aemi S

2018-01-01

The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of active sampling strategies for the determination of 1,3-butadiene in air

NASA Astrophysics Data System (ADS)

Vallecillos, Laura; Maceira, Alba; Marcé, Rosa Maria; Borrull, Francesc

2018-03-01

Two analytical methods for determining levels of 1,3-butadiene in urban and industrial atmospheres were evaluated in this study. Both methods are extensively used for determining the concentration of volatile organic compounds in the atmosphere and involve collecting samples by active adsorptive enrichment on solid sorbents. The first method uses activated charcoal as the sorbent and involves liquid desorption with carbon disulfide. The second involves the use of a multi-sorbent bed with two graphitised carbons and a carbon molecular sieve as the sorbent, with thermal desorption. Special attention was paid to the optimization of the sampling procedure through the study of sample volume, the stability of 1,3-butadiene once inside the sampling tube and the humidity effect. In the end, the thermal desorption method showed better repeatability and limits of detection and quantification for 1,3-butadiene than the liquid desorption method, which makes the thermal desorption method more suitable for analysing air samples from both industrial and urban atmospheres. However, sampling must be performed with a pre-tube filled with a drying agent to prevent the loss of the adsorption capacity of the solid adsorbent caused by water vapour. The thermal desorption method has successfully been applied to determine of 1,3-butadiene inside a 1,3-butadiene production plant and at three locations in the vicinity of the same plant.

Nonhydrolytic sol-gel approach to facile creation of surface-bonded zirconia organic-inorganic hybrid coatings for sample preparation. Ι. Capillary microextraction of catecholamine neurotransmitters.

PubMed

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.

Determination of trichloroanisole and trichlorophenol in wineries' ambient air by passive sampling and thermal desorption-gas chromatography coupled to tandem mass spectrometry.

PubMed

Camino-Sánchez, F J; Bermúdez-Peinado, R; Zafra-Gómez, A; Ruíz-García, J; Vílchez-Quero, J L

2015-02-06

The present paper describes the calibration of selected passive samplers used in the quantitation of trichlorophenol and trichloroanisole in wineries' ambient air, by calculating the corresponding sampling rates. The method is based on passive sampling with sorbent tubes and involves thermal desorption-gas chromatography-triple quadrupole mass spectrometry analysis. Three commercially available sorbents were tested using sampling cartridges with a radial design instead of axial ones. The best results were found for Tenax TA™. Sampling rates (R-values) for the selected sorbents were determined. Passive sampling was also used for accurately determining the amount of compounds present in the air. Adequate correlation coefficients between the mass of the target analytes and exposure time were obtained. The proposed validated method is a useful tool for the early detection of trichloroanisole and its precursor trichlorophenol in wineries' ambient air while avoiding contamination of wine or winery facilities. Copyright © 2015 Elsevier B.V. All rights reserved.

Ionic liquids: solvents and sorbents in sample preparation.

PubMed

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.

Application of a dispersive solid-phase extraction method using an amino-based silica-coated nanomagnetic sorbent for the trace quantification of chlorophenoxyacetic acids in water samples.

PubMed

Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali; Sobhi, Hamid Reza

2017-09-01

Herein, an amino-based silica-coated nanomagnetic sorbent was applied for the effective extraction of two chlorophenoxyacetic acids (2-methyl-4-chlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid) from various water samples. The sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy. The analytes were extracted by the sorbent mainly through ionic interactions. Once the extraction of analytes was completed, they were desorbed from the sorbent and detected by high-performance liquid chromatography with ultraviolet detection. A number of factors affecting the extraction and desorption of the analytes were investigated in detail and the optimum conditions were established. Under the optimum conditions, the calibration curves were linear over the concentration range of 1-250, and based on a signal-to-noise ratio of 3, the method detection limits were determined to be 0.5 μg/L for both analytes. Additionally, a preconcentration factor of 314 was achieved for the analytes. The average relative recoveries obtained from the fortified water samples varied in the range of 91-108% with relative standard deviations of 2.9-8.3%. Finally, the method was determined to be robust and effective for environmental water analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The development and testing of a volatile organics concentrator for use in monitoring Space Station water quality

NASA Technical Reports Server (NTRS)

Bodek, Itamar; Ehntholt, Daniel J.; Stolki, Thomas J.; Trabanino, Rudy; Hinsdale, Lloyd; Webb, Johanna; Sauer, Richard L.

1992-01-01

The Volatile Organics Concentrator (VOC) system, designed to attach to a gas chromatograph/mass spectrometer (GC/MS) for the analyses of volatile organic compounds in water on Space Station Freedom, is described. Organic volatiles are collected and concentrated in the VOC by means of two primary solid sorbent tubes and desorbed into the GC/MS system. The paper describes the results of testing the VOC breadboard using a GC/MS system. Evaluations performed on 39 organic compounds recovered from water samples were compared with data for these compounds using direct injection/GC/MS and purge and trap/GC/MS procedures. The results demonstrate that the VOC/GC/MS system's detection limits for the 39 compounds analyzed are comparable to those of the EPA Method 524.2, and for many compounds reaching a factor of 5 lower.

SOA precursors at the T0 site during the 2010 CARES campaign

NASA Astrophysics Data System (ADS)

Wallace, H. W.; Jobson, B. T.; Erickson, M. H.

2010-12-01

Continuous measurements of C5 to C12 Volatile Organic Compounds (VOC) have been made using the Washington State University Mobile Atmospheric Chemistry Laboratory (MACL), at the T0 site during the month of June 2010 Carbonaceous Aerosol Carbonaceous Aerosols and Radiative Effects Study (CARES). These measurements were made to better understand aerosol formation and growth in Sacramento, CA and the surrounding areas. Using a sorbent based preconcentration sampling technique for our quadrupole ion trap gas chromatography mass spectrometer (GCMS), we have measured anthropogenic and biogenic secondary organic aerosol (SOA) precursors. Major biogenic VOCs identified include: α-pinene, limonene, isoprene, phellanderene and β-pinene. Diurnal profiles of the concentrations will be presented. Monoterpenes were highest in the mornings while isoprene was highest in the afternoon. In addition to understanding the diurnal profiles the SOA precursors at the T0 site, the relative contributions of biogenic and anthropogenic compounds to SOA formation will be presented.

Magnetically responsive polycaprolactone nanoparticles for progesterone screening in biological and environmental samples using gas chromatography.

PubMed

Es'haghi, Zarrin; Nezhadali, Azizollah; Khatibi, Aram-Dokht

2016-08-01

A new Fe3O4/poly(є-caprolactone) (PCL) magnetite nanocomposite was fabricated and used as a sorbent for magnetically mediated PCL microspheres solid-phase extraction (MM-PCL-SPE) followed by gas chromatography-flame ionization detection (GC-FID) for monitoring of progesterone (PGN) hormone in biological and environmental matrices, namely blood serum, tap water, urine, and hospital wastewater. The nanomagnetite core of the sorbent was synthesized by a co-precipitation method. Magnetic nanoparticles (MNPs) were then microencapsulated with PCL microspheres using emulsion polymerization. The nanocomposite was characterized by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The magnetite sorbent can be effectively dispersed in aqueous solution and attracted to an external magnetic field. The MM-PCL-SPE process for PGN assay involved (a) dispersion of the sorbent in the donor phase aqueous solution with sonication, (b) exposure to a magnetic field to collect sorbent that had adsorbed the analyte, and (c) solvent desorption of extracted PGN for GC-FID analysis. The work demonstrates the usefulness of MM-PCL-SPE in the rapid and sensitive monitoring of trace amounts of PGN in real samples. The limit of detection (LOD) and limit of quantification (LOQ) were 1.00 and 3.30 ng/mL, respectively. The relative recoveries in real samples were adequate. Linearity was observed over a wide range of 2.2-10,000.0 ng/mL in aqueous media and urine and 0.01-70.0 μg/mL in blood serum. Graphical Abstract In this research new Fe3O4/poly(є-caprolactone) (PCL) magnetite microspheres were developed as an efficient sorbent for solid-phase extraction of progesterone hormone in biological and environmental matrices.

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

PubMed

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

2018-04-13

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 rights reserved.

PERMEABILITY PROPERTIES OF FLY ASH FORM FURNACE SORBENT INJECTION PROCESS

EPA Science Inventory

The paper discusses tests of the applicability of furnace sorbent injection (FSI) waste solids for use as synthetic waste landfill liners by measuring the mechanical strength and permeability of moisture-cured samples. SI waste solids were received from the EPA-sponsored demonstr...

Simultaneous extraction and preconcentration of uranium and thorium in aqueous samples by new modified mesoporous silica prior to inductively coupled plasma optical emission spectrometry determination.

PubMed

Yousefi, Seyed Reza; Ahmadi, Seyed Javad; Shemirani, Farzaneh; Jamali, Mohammad Reza; Salavati-Niasari, Masoud

2009-11-15

A new synthesized modified mesoporous silica (MCM-41) using 5-nitro-2-furaldehyde (fural) was applied as an effective sorbent for the solid phase extraction of uranium(VI) and thorium(IV) ions from aqueous solution for the measurement by inductively coupled plasma optical emission spectrometry (ICP OES). The influences of some analytical parameters on the quantitative recoveries of the analyte ions were investigated in batch method. Under optimal conditions, the analyte ions were sorbed by the sorbent at pH 5.5 and then eluted with 1.0 mL of 1.0 mol L(-1) HNO(3). The preconcentration factor was 100 for a 100mL sample volume. The limits of detection (LOD) obtained for uranium(VI) and thorium(IV) were 0.3 microg L(-1). The maximum sorption capacity of the modified MCM-41 was found to be 47 and 49 mg g(-1) for uranium(VI) and thorium(IV), respectively. The sorbent exhibited good stability, reusability, high adsorption capacity and fast rate of equilibrium for sorption/desorption of uranium and thorium ions. The applicability of the synthesized sorbent was examined using CRM and real water samples.

Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

PubMed

Yu, Honglian; Merib, Josias; Anderson, Jared L

2016-03-18

Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Effects of sorbent attrition on utilization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Keener, T.C.; Khang, Soon-Jai; Lee, S.K.

1992-03-01

Attrition of surface product levers of sulfite/sulfate may be the key to substantially increasing sorbent utilization in new dry scrubbing processes. This conclusion has been reached from research results obtained from new gas/solid contacting methods such as the Circulating Fluidized Bed Absorber and the Limestone Emission Control method. An additional savings may be reduced by the use of large initial sorbent, particle sizes which greatly reduces the cost of grinding and sorbent preparation. The objectives of project 1.7 were then to study attrition of sorbent particles in a systematic fashion in order to determine how to use attrition to increasemore » sorbent utilization. This was to be carried out by the construction of a bench scale fluidized bed where a series of experiments were to be conducted to measure attrition of lime and limestone samples. This has been accomplished and the project proceeded as anticipated. The results indicate that attrition differs for wet and dry conditions for certain sorbents and that these differences are substantial. Under dry conditions, the results of attrition tests on carefully characterized lime samples indicate that mechanical abrasion is the primary attrition mechanism. The rate of attrition is seen to be similar to a first order chemical reaction where the bed mass (or total surface area) is analagous to reactant concentration. A model for mechanical attrition is presented which expresses the rate constant in an Arrhenius type form proportional to a pseudo attrition activation energy and excess gas energy above a minimum level. The value of this pseudo attrition activation energy for lime has been found to be 106 KJ/KG. For the attrition of wetted lime particles in a fluidized bed. the attrition rate has been found to be directly related to the volumetric flow rate of injected water.« less

Odor analysis of decomposing buried human remains

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vass, Arpad Alexander; Smith, Rob R; Thompson, Cyril V

2008-01-01

This study, conducted at the University of Tennessee's Anthropological Research Facility (ARF), lists and ranks the primary chemical constituents which define the odor of decomposition of human remains as detected at the soil surface of shallow burial sites. Triple sorbent traps were used to collect air samples in the field and revealed eight major classes of chemicals which now contain 478 specific volatile compounds associated with burial decomposition. Samples were analyzed using gas chromatography-mass spectrometry (GC-MS) and were collected below and above the body, and at the soil surface of 1.5-3.5 ft. (0.46-1.07 m) deep burial sites of four individualsmore » over a 4-year time span. New data were incorporated into the previously established Decompositional Odor Analysis (DOA) Database providing identification, chemical trends, and semi-quantitation of chemicals for evaluation. This research identifies the 'odor signatures' unique to the decomposition of buried human remains with projected ramifications on human remains detection canine training procedures and in the development of field portable analytical instruments which can be used to locate human remains in shallow burial sites.« less

Quantification of Alkyl Nitrates in Ambient Air by Thermal Dissociation Cavity Ring-Down Spectroscopy with Preconcentration

NASA Astrophysics Data System (ADS)

Ye, C. Z.; Osthoff, H. D.; Taha, Y. M.; Pak, J. K.; Saowapon, M. T.

2015-12-01

Alkyl nitrates (AN, molecular formula RONO2) play a crucial role in the troposphere as temporary reservoirs of nitrogen oxides (NOx =NO +NO2) and by acting as chain terminators in the photochemical production of ozone. Mixing ratios of AN in ambient air are commonly quantified by gas chromatography with electron capture or mass spectrometric detection (GC-ECD or GC-MS) coupled to purge-and-trap preconcentration, usually on Tenax sorbent, to improve the detection limits. The analysis, however, is quite laborious as there are many alkyl nitrates that are low in individual abundance (often less than 1 parts-per-trillion by volume, pptv) and that exhibit different instrumental response factors. An alternative method is to determine alkyl nitrates as a sum (ΣAN) by thermal dissociation (TD) to a common fragment (NO2), which can then be quantified with a uniform response factor by optical absorption, for example by cavity ring-down spectroscopy (CRDS). However, the determination of ΣAN by TD-CRDS is hampered by its relatively high detection limits (several 100 pptv) and secondary chemistry following TD that results in both negative and positive interferences and depends on the composition of the ambient air sampled. In this work, a TD-CRDS equipped with a Tenax preconcentration unit is described. Matrix effects are minimized by desorbing the samples from the Tenax in a background of nitrogen. The performance of the instrument, in particular the recovery from the Tenax sorbent, was evaluated by sampling laboratory-generated mixtures of alkyl and peroxyacyl nitrates. Field data from a coastal site collected during the Ozone-depleting reactions in a coastal atmosphere (ORCA) campaign, which took place at the Amphitrite Point Observatory in Ucluelet, BC, from July 6 - 31, 2015, are presented. Advantages and disadvantages of the new method are discussed.

Analysis of trace contamination of phthalate esters in ultrapure water using a modified solid-phase extraction procedure and automated thermal desorption-gas chromatography/mass spectrometry.

PubMed

Liu, Hsu-Chuan; Den, Walter; Chan, Shu-Fei; Kin, Kuan Tzu

2008-04-25

The present study was aimed to develop a procedure modified from the conventional solid-phase extraction (SPE) method for the analysis of trace concentration of phthalate esters in industrial ultrapure water (UPW). The proposed procedure allows UPW sample to be drawn through a sampling tube containing hydrophobic sorbent (Tenax TA) to concentrate the aqueous phthalate esters. The solid trap was then demoisturized by two-stage gas drying before subjecting to thermal desorption and analysis by gas chromatography-mass spectrometry. This process removes the solvent extraction procedure necessary for the conventional SPE method, and permits automation of the analytical procedure for high-volume analyses. Several important parameters, including desorption temperature and duration, packing quantity and demoisturizing procedure, were optimized in this study based on the analytical sensitivity for a standard mixture containing five different phthalate esters. The method detection limits for the five phthalate esters were between 36 ng l(-1) and 95 ng l(-1) and recovery rates between 15% and 101%. Dioctyl phthalate (DOP) was not recovered adequately because the compound was both poorly adsorbed and desorbed on and off Tenax TA sorbents. Furthermore, analyses of material leaching from poly(vinyl chloride) (PVC) tubes as well as the actual water samples showed that di-n-butyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) were the common contaminants detected from PVC contaminated UPW and the actual UPW, as well as in tap water. The reduction of DEHP in the production processes of actual UPW was clearly observed, however a DEHP concentration of 0.20 microg l(-1) at the point of use was still being quantified, suggesting that the contamination of phthalate esters could present a barrier to the future cleanliness requirement of UPW. The work demonstrated that the proposed modified SPE procedure provided an effective method for rapid analysis and contamination identification in UPW production lines.

Selective Solid-Phase Extraction of Zinc(II) from Environmental Water Samples Using Ion Imprinted Activated Carbon.

PubMed

Moniri, Elham; Panahi, Homayon Ahmad; Aghdam, Khaledeh; Sharif, Amir Abdollah Mehrdad

2015-01-01

A simple ion imprinted amino-functionalized sorbent was synthesized by coupling activated carbon with iminodiacetic acid, a functional compound for metal chelating, through cyanoric chloride spacer. The resulting sorbent has been characterized using FTIR spectroscopy, elemental analysis, and thermogravimetric analysis and evaluated for the preconcentration and determination of trace Zn(II) in environmental water samples. The optimum pH value for sorption of the metal ion was 6-7.5. The sorption capacity of the functionalized sorbent was 66.6 mg/g. The chelating sorbent can be reused for 10 cycles of sorption-desorption without any significant change in sorption capacity. A recovery of 100% was obtained for the metal ion with 0.5 M nitric acid as the eluent. Compared with nonimprinted polymer particles, the prepared Zn-imprinted sorbent showed high adsorption capacity, significant selectivity, and good site accessibility for Zn(II). Scatchard analysis revealed that the homogeneous binding sites were formed in the polymer. The equilibrium sorption data of Zn(II) by modified resin were analyzed by Langmuir, Freundlich, Temkin, and Redlich-Peterson models. Based on equilibrium adsorption data, the Langmuir, Freundlich, and Temkin constants were determined as 0.139, 12.82, and 2.34, respectively, at 25°C.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Ultrathin-shell boron nitride hollow spheres as sorbent for dispersive solid-phase extraction of polychlorinated biphenyls from environmental water samples.

PubMed

Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Chen, Fan; Wu, Chi-Man Lawrence; Zhao, Rusong; Cheng, Chuange

2014-11-21

Boron nitride hollow spheres with ultrathin-shells were synthesized and used as sorbents for dispersive solid-phase extraction of aromatic pollutants at trace levels from environmental water samples. Polychlorinated biphenyls (PCBs) were selected as target compounds. Sample quantification and detection were performed by gas chromatography-tandem mass spectrometry. Extraction parameters influencing the extraction efficiency were optimized through response surface methodology using the Box-Behnken design. The proposed method achieved good linearity within the concentration range of 0.15-250 ng L(-1) PCBs, low limits of detection (0.04-0.09 ng L(-1), S/N=3:1), good repeatability of the extractions (relative standard deviation, <12%, n=6), and satisfactory recoveries between 84.9% and 101.0% under optimal conditions. Real environmental samples collected from rivers, local lakes, rain and spring waters were analyzed using the developed method. Results demonstrated that the hexagonal boron nitride-based material has significant potential as a sorbent for organic pollutant extraction from environmental water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel nanoporous sorbent for solid-phase extraction in petroleum fingerprinting

NASA Astrophysics Data System (ADS)

Alayande, S. Oluwagbemiga; Hlengilizwe, Nyoni; Dare, E. Olugbenga; Msagati, Titus A. M.; Akinlabi, A. Kehinde; Aiyedun, P. O.

2016-04-01

Sample preparation is crucial in the analysis of petroleum and its derivatives. In this study, developing affordable sorbent for petroleum fingerprinting analysis using polymer waste such expanded polystyrene was explored. The potential of electrospun expanded polystyrene (EPS) as a sorbent for the solid-phase extraction (SPE) technique was investigated, and its efficiency was compared with commercial cartridges such as alumina, silica and alumina/silica hybrid commercial for petroleum fingerprinting analysis. The chromatograms showed that the packed electrospun EPS fibre demonstrated excellent properties for SPE applications relative to the hybrid cartridges.

Evaluation of ultrasound-assisted in situ sorbent formation solid-phase extraction method for determination of arsenic in water, food and biological samples.

PubMed

Ezoddin, Maryam; Majidi, Behrooz; Abdi, Khosrou

2015-01-01

A simple and rapid ultrasound-assisted in situ sorbent formation solid-phase extraction (UAISFSPE) coupled with electrothermal atomic absorption spectrometry detection (ET-AAS) was developed for preconcentration and determination of arsenic (As) in various samples. A small amount of cationic surfactant is dissolved in the aqueous sample containing As ions, which were complexed by ammonium pyrrolidinedithiocarbamate After shaking, a little volume of hexafluorophosphate (NaPF6) as an ion-pairing agent was added into the solution by a microsyringe. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed. The alkyl groups of the surfactant in the solid particles strongly interact with the hydrophobic groups of analytes and become bound. Sonication aids the dispersion of the sorbent into the sample solution and mass transfer of the analyte into the sorbent, thus reducing the extraction time. The solid particles are centrifuged, and the sedimented particles can be dissolved in an appropriate solvent to recover the absorbed analyte. After separation, total arsenic (As(III) and As(V)) was determined by ET-AAS. Several experimental parameters were investigated and optimized. A detection limit of 7 ng L(-1) with preconcentration factor of 100 and relative standard deviation for 10 replicate determinations of 0.1 µg L(-1) As(III) were 4.5% achieved. Consequently, the method was applied to the determination of arsenic in certified reference materials, water, food and biological samples with satisfactory results.

Sol-gel-graphene-based fabric-phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection.

PubMed

Samanidou, Victoria; Filippou, Olga; Marinou, Eirini; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric-phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent-based sorptive microextraction techniques, using hybrid organic-inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol-gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol-gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tank Vapor Characterization Project: Tank 241-S-102 fourth temporal study: Headspace gas and vapor characterization results from samples collected on December 19, 1996

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pool, K.H.; Evans, J.C.; Olsen, K.B.

1997-08-01

This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis planmore » (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.410% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.« less

An ion-imprinted silica-supported organic-inorganic hybrid sorbent prepared by a surface imprinting technique combined with a polysaccharide incorporated sol-gel process for selective separation of cadmium(II) from aqueous solution.

PubMed

Li, Feng; Jiang, Hongquan; Zhang, Shusheng

2007-03-15

Ion-imprinting concept and polysaccharide incorporated sol-gel process were applied to the preparation of a new silica-supported organic-inorganic hybrid sorbent for selective separation of Cd(II) from aqueous solution. In the prepared shell/core composite sorbent, covalently surface coating on the supporting silica gel was achieved by using a Cd(II)-imprinting sol-gel process starting from an inorganic precursor, gamma-glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS). The sorbent was prepared through self-hydrolysis of GPTMS, self-condensation and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, in combination with in situ covalent cross-linking of CS with partial amine shielded by Cd(II) complexation. Extraction of the imprinting molecules left a predetermined arrangement of ligands and tailored binding pockets for Cd(II). The prepared sorbent was characterized by using X-ray energy dispersion spectroscopy (EDX), X-ray diffraction (XRD), and scanning electron microscopy (SEM). Batch experiments were conducted to study the sorption performance by removal of Cd(II) when present singly or in binary system, an aqueous Cd(II) and Zn(II) mixture. The ion-imprinted composite sorbent offered a fast kinetics for the sorption of Cd(II) and the maximum capacity was 1.14mmolg(-1). The uptake capacity of the imprinted sorbent and the selectivity coefficient were much higher than that of the non-imprinted sorbent. The imprinted sorbent exhibited high reusability. The prepared functional sorbent was shown to be promising for the preconcentration of cadmium in environmental and biological samples.

Imprint-coating synthesis of selective functionalized ordered mesoporous sorbents for separation and sensors

DOEpatents

Dai, Sheng; Burleigh, Mark C.; Shin, Yongsoon

2001-01-01

The present invention relates generally to mesoporous sorbent materials having high capacity, high selectivity, fast kinetics, and molecular recognition capability. The invention also relates to a process for preparing these mesoporous substrates through molecular imprinting techniques which differ from convention techniques in that a template molecule is bound to one end of bifunctional ligands to form a complex prior to binding of the bifunctional ligands to the substrate. The present invention also relates to methods of using the mesoporous sorbent materials, for example, in the separation of toxic metals from process effluents, paints, and other samples; detection of target molecules, such as amino acids, drugs, herbicides, fertilizers, and TNT, in samples; separation and/or detection of substances using chromatography; imaging agents; sensors; coatings; and composites.

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

PubMed Central

Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Strzemski, Maciej; Sawicki, Jan; Staniak, Michał; Dresler, Sławomir; Szwerc, Wojciech; Mołdoch, Jarosław; Latalski, Michał

2018-01-01

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. PMID:29565297

Vortex assisted solid-phase extraction of lead(II) using orthorhombic nanosized Bi2WO6 as a sorbent.

PubMed

Baghban, Neda; Yilmaz, Erkan; Soylak, Mustafa

2017-12-07

Nanosized single crystal orthorhombic Bi 2 WO 6 was synthesized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The crystal and molecular structure of the sorbent was examined using XRD, Raman, SEM and SEM-EDX analysis. Various parameters affecting extraction efficiency were optimized by using multivariate design. The effect of diverse ions on the extraction also was studied. Lead was quantified by flame atomic absorption spectrometry (FAAS). The recoveries of lead(II) from spiked samples (at a typical spiking level of 200-400 ng·mL -1 ) are >95%. Other figures of merit includes (a) a detection limit of 6 ng·mL -1 , (b) a preconcentration factor of 50, (c) a relative standard deviation of 1.6%, and (d) and adsorption capacity of 6.6 mg·g -1 . The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples. Graphical abstract Nanosized single crystal orthorhombic Bi 2 WO 6 was synthesized and characterized by a hydrothermal method and used as a sorbent for vortex assisted solid phase extraction of lead(II). The procedure was successfully applied to accurate determination of lead in (spiked) pomegranate and water samples.

Removal of metals from industrial wastewater and urban runoff by mineral and bio-based sorbents.

PubMed

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.

Sensitive determination of polycyclic aromatic hydrocarbons in water samples by HPLC coupled with SPE based on graphene functionalized with triethoxysilane.

PubMed

Huang, Ke-Jing; Li, Jing; Liu, Yan-Ming; Wang, Lan

2013-02-01

The graphene functionalized with (3-aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1-100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029-0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Glufosinate ammonium clean-up procedure from water samples using SPE

NASA Astrophysics Data System (ADS)

Tayeb M., A.; Ismail B., S.; Mardiana-Jansar, K.; Ta, Goh Choo; Agustar, Hani Kartini

2015-09-01

For the determination of glufosinate ammonium residue in soil and water samples, different solid phase extraction (SPE) sorbent efficiency was studied. Four different SPE sorbents i.e.: CROMABOND PS-H+, CROMABOND PS-OH-, ISOLUTE ENV+, Water Sep-Pak and OASIS HLB were used. Sample clean-up performance was evaluated using high performance liquid chromatography (Agilent 1220 infinity LC) with fluorescence detector. Detection of FMO-derivatives was done at λ ex = 260 nm and λ em= 310 nm. OASIS HLB column was the most suitable for the clean-up in view of the overall feasibility of the analysis.

Air Quality Inside Police Drug Safes and Drug Storage Areas.

PubMed

Doran, Gregory S; Deans, Ralph; De Filippis, Carlo; Kostakis, Chris; Howitt, Julia A

2018-06-01

Storage of drug-based evidence inside sealed safes may allow chemical vapors to accumulate, creating concerns of drug exposure by inhalation, or the possibility of cross-contamination of drug evidence. Air samples were taken from inside eight drug safes and one small storage room at nine city and country police stations, as well as a large centralized drug evidence storage vault, in New South Wales (NSW), Australia. Sorbent tubes containing charcoal were used to determine whether any drug residues could be detected in the air, and to identify the types of chemicals present. Carbon traps were extracted and analyzed by LC-MS-MS for a suite of 22 licit and illicit drug residues and 2 metabolites. Carbon traps and SPME fibers were also analyzed by GC-MS for general volatile organic compound (VOC) residues. No detectable drug residues, either as airborne dust or vapor, were found in the safes, the storage room or the large central repository vault. No drugs were detected in any of the 34 urine samples collected at 8 of the 10 sampling locations, while only one of the five hair samples was positive for cocaine (9 pg/mg) provided by police exhibit officers at 3 of the 10 sampling locations. VOC analysis identified a variety of solvents associated with drug manufacture, plasticisers, personal care products and volatiles associated with plants such as cannabis. The results indicate that strong chemical odours emanating from drug safes are unlikely to be drug residues due to low volatility of drugs, and are more likely VOCs associated with their manufacture or from plant growing operations. Consideration should be given to the quality of air flow in rooms in which safes are housed and the use of air filtering inside safes to reduce the likelihood of VOC accumulation, and therefore the risk of human exposure.

Modification of gold nanoparticle loaded on activated carbon with bis(4-methoxysalicylaldehyde)-1,2-phenylenediamine as new sorbent for enrichment of some metal ions.

PubMed

Karimipour, Gholamreza; Ghaedi, Mehrorang; Sahraei, Reza; Daneshfar, Ali; Biyareh, Mehdi Nejati

2012-01-01

In this study, a new sorbent based on the gold nanoparticle loaded in activated carbon (Au-NP-AC) was synthesized and modified by bis(4-methoxy salicylaldehyde)-1,2-phenylenediamine (BMSAPD). This sorbent, which is abbreviated as Au-NP-AC-BMSAPD, has been applied for the enrichment and preconcentration of trace amounts of Co(2+), Cu(2+), Ni(2+), Fe(2+), Pb(2+), and Zn(2+) ions in real samples. All metal ions under study were retained on the Au-NP-AC-BMSAPD sorbent by complexation of the ions with the BMSAPD ligand, providing an efficient preconcentration fashion. The retained metal ions were then eluted from the sorbent by HNO(3) and detected by flame atomic absorption spectrometry. The analytical parameters including pH, amount of ligand, and the nature of the eluent and solid phase were evaluated to obtain the optimum condition for the preconcentration factor. Following the optimum conditions, a preconcentration factor of 200 was obtained for all the metal ions under study with detection limits of 1.4-2.6 ng mL(-1). The method has been successfully applied for the extraction and determination of the ion content in the same real samples with recoveries in the range of 95-99.6% and a relative standard deviation lower than 4.0%.

Biocompatibility and Cytotoxic Evaluation of New Sorbent Cartridges for Blood Hemoperfusion.

PubMed

Pomarè Montin, Diego; Ankawi, Ghada; Lorenzin, Anna; Neri, Mauro; Caprara, Carlotta; Ronco, Claudio

2018-06-08

The use of adsorption cartridges for hemoperfusion (HP) is rapidly evolving. For these devices, the potential induced cytotoxicity is an important issue. The aim of this study was to investigate potential in vitro cytotoxic effects of different sorbent cartridges, HA130, HA230, HA330, HA380 (Jafron, China), on U937 monocytes. Monocytes were exposed to the sorbent material in static and dynamic manners. In static test, cell medium samples were collected after 24 h of incubation in the cartridges. In dynamic test, HP modality has been carried out and samples at 30, 60, 90, and 120 min were collected. Compared to control samples, there was no evidence of increased necrosis or apoptosis in monocytes exposed to the cartridges both in the static and dynamic tests. Our in vitro testing suggests that HA cartridges carry an optimal level of biocompatibility and their use in HP is not associated with adverse reactions or signs of cytotoxicity. © 2018 S. Karger AG, Basel.

Sorbents for High Temperature Removal of Arsenic from Coal-Derived Synthesis Gas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alptekin, G.O.; Copeland, R.; Dubovik, M.

2002-09-20

Gasification technologies convert coal and other heavy feedstocks into synthesis gas feed streams that can be used in the production of a wide variety of chemicals, ranging from hydrogen through methanol, ammonia, acetic anhydride, dimethyl ether (DME), methyl tertiary butyl ether (MTBE), high molecular weight liquid hydrocarbons and waxes. Syngas can also be burned directly as a fuel in advanced power cycles to generate electricity with very high efficiency. However, the coal-derived synthesis gas contains a myriad of trace contaminants that may poison the catalysts that are used in the downstream manufacturing processes and may also be regulated in powermore » plant emissions. Particularly, the catalysts used in the conversion of synthesis gas to methanol and other liquid fuels (Fischer-Tropsch liquids) have been found to be very sensitive to the low levels of poisons, especially arsenic, that are present in the synthesis gas from coal. TDA Research, Inc. (TDA) is developing an expendable high capacity, low-cost chemical absorbent to remove arsenic from coal-derived syngas. Unlike most of the commercially available sorbents that physically adsorb arsenic, TDA's sorbent operates at elevated temperatures and removes the arsenic through chemical reaction. The arsenic content in the coal gas stream is reduced to ppb levels with the sorbent by capturing and stabilizing the arsenic gas (As4) and arsenic hydrides (referred to as arsine, AsH3) in the solid state. To demonstrate the concept of high temperature arsenic removal from coal-derived syngas, we carried out bench-scale experiments to test the absorption capacity of a variety of sorbent formulations under representative conditions. Using on-line analysis techniques, we monitored the pre- and post-breakthrough arsine concentrations over different sorbent samples. Some of these samples exhibited pre-breakthrough arsine absorption capacity over 40% wt. (capacity is defined as lb of arsenic absorbed/lb of sorbent), while maintaining an arsine outlet concentration at less than 10 ppb.« less

Preparation of a reversed-phase/anion-exchange mixed-mode spherical sorbent by Pickering emulsion polymerization for highly selective solid-phase extraction of acidic pharmaceuticals from wastewater.

PubMed

Huang, Chaonan; Li, Yun; Yang, Jiajia; Peng, Junyu; Jin, Jing; Dhanjai; Wang, Jincheng; Chen, Jiping

2017-10-27

The present work represents a simple and effective preparation of a novel mixed-mode anion-exchange (MAX) sorbent based on porous poly[2-(diethylamino)ethyl methacrylate-divinylbenzene] (poly(DEAEMA-DVB)) spherical particles synthesized by one-step Pickering emulsion polymerization. The poly(DEAEMA-DVB) particles were quaternized with 1,4-butanediol diglycidyl ether (BDDE) followed by triethylamine (TEA) via epoxy-amine reaction to offer strong anion exchange properties. The synthesized MAX sorbent was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, nitrogen adsorption-desorption measurements and elemental analysis. The MAX sorbent possessed regular spherical shape and narrow diameter distribution (15-35μm), a high IEC of 0.54meq/g, with carbon and nitrogen contents of 80.3% and 1.62%, respectively. Compared to poly(DEAEMA-DVB), the MAX sorbent exhibited decreased S BET (390.5 vs. 515.3m 2 g -1 ), pore volume (0.74 vs. 0.85cm 3 g -1 ) and pore size (16.8 vs. 17.3nm). Moreover, changes of N content for producing the MAX sorbent reveal a successful two-step quaternization, which can be highly related to such a high IEC. Finally, the MAX sorbent was successfully evaluated for selective isolation and purification of some selected acidic pharmaceuticals (ketoprofen, KEP; naproxen, NAP; and ibuprofen, IBP) from neutral (hydrocortisone, HYC), basic (carbamazepine, CAZ; amitriptyline, AMT) pharmaceuticals and other interferences in water samples using solid phase extraction (SPE). An efficient analytical method based on the MAX-based mixed-mode SPE coupled with HPLC-UV was developed for highly selective extraction and cleanup of acidic KEP, NAP and IBP in spiked wastewater samples. The developed method exhibited good sensitivity (0.009-0.085μgL -1 limit of detection), satisfactory recoveries (82.1%-105.5%) and repeatabilities (relative standard deviation < 7.9%, n=3). Copyright © 2017 Elsevier B.V. All rights reserved.

Tantala-based sol-gel coating for capillary microextraction on-line coupled to high-performance liquid chromatography.

PubMed

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.

Effects of sorbent attrition on utilization. Final report, June 1, 1990--June 30, 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Keener, T.C.; Khang, Soon-Jai; Lee, S.K.

1992-03-01

Attrition of surface product levers of sulfite/sulfate may be the key to substantially increasing sorbent utilization in new dry scrubbing processes. This conclusion has been reached from research results obtained from new gas/solid contacting methods such as the Circulating Fluidized Bed Absorber and the Limestone Emission Control method. An additional savings may be reduced by the use of large initial sorbent, particle sizes which greatly reduces the cost of grinding and sorbent preparation. The objectives of project 1.7 were then to study attrition of sorbent particles in a systematic fashion in order to determine how to use attrition to increasemore » sorbent utilization. This was to be carried out by the construction of a bench scale fluidized bed where a series of experiments were to be conducted to measure attrition of lime and limestone samples. This has been accomplished and the project proceeded as anticipated. The results indicate that attrition differs for wet and dry conditions for certain sorbents and that these differences are substantial. Under dry conditions, the results of attrition tests on carefully characterized lime samples indicate that mechanical abrasion is the primary attrition mechanism. The rate of attrition is seen to be similar to a first order chemical reaction where the bed mass (or total surface area) is analagous to reactant concentration. A model for mechanical attrition is presented which expresses the rate constant in an Arrhenius type form proportional to a pseudo attrition activation energy and excess gas energy above a minimum level. The value of this pseudo attrition activation energy for lime has been found to be 106 KJ/KG. For the attrition of wetted lime particles in a fluidized bed. the attrition rate has been found to be directly related to the volumetric flow rate of injected water.« less

Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

PubMed

Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

2013-11-15

A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

2016-01-15

A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

A novel molybdenum disulfide nanosheet self-assembled flower-like monolithic sorbent for solid-phase extraction with high efficiency and long service life.

PubMed

Ran, Fanpeng; Liu, Hongmei; Wang, Xiaoqi; Guo, Yong

2017-07-21

A novel material consisting of molybdenum disulfide (MoS 2 ) nanosheet that self-assemble into flower-like microspheres which aggregate to form a monolithic matrix with a micro or nano-scaled mesopore structure was successfully synthesized and used as an efficient sorbent for solid-phase extraction (SPE) due to its large specific adsorption area and good stability. The extraction properties of the as-prepared sorbent were evaluated by high-performance liquid chromatography with variable wavelength detection (HPLC-VWD) by analyzing four flavonoids (apigenin, quercetin, luteolin, and kaempferol). Under optimal conditions, the LODs and LOQs were found to be in the ranges of 0.1-0.25 and 0.4-0.5μgL -1 , respectively, and wide linear ranges were obtained with correlation coefficients (R) ranging from 0.9991 to 0.9996. Compared with commercial C18 and Alumina-N sorbents, the as-prepared sorbent showed high extraction efficiency at different concentrations of flavonoids. After 100 uses, the extraction ability of the self-assembled MoS 2 nanosheet monolithic sorbent had no evident decline, denoting a long service life. Finally, the SPE-HPLC-VWD method using the as-prepared sorbent was applied to flavonoid analysis in beverage samples with satisfactory results. Copyright © 2017 Elsevier B.V. All rights reserved.

Sorbent amendment as a remediation strategy to reduce PFAS mobility and leaching in a contaminated sandy soil from a Norwegian firefighting training facility.

PubMed

Hale, Sarah E; Arp, Hans Peter H; Slinde, Gøril Aasen; Wade, Emma Jane; Bjørseth, Kamilla; Breedveld, Gijs D; Straith, Bengt Fredrik; Moe, Kamilla Grotthing; Jartun, Morten; Høisæter, Åse

2017-03-01

Aqueous film-forming foams (AFFF) containing poly- and perfluoroalkyl substances (PFAS) used for firefighting have led to the contamination of soil and water at training sites. The unique physicochemical properties of PFAS results in environmental persistency, threatening water quality and making remediation of such sites a necessity. This work investigated the role of sorbent amendment to PFAS contaminated soils in order to immobilise PFAS and reduce mobility and leaching to groundwater. Soil was sampled from a firefighting training facility at a Norwegian airport and total and leachable PFAS concentrations were quantified. Perfluorooctanesulfonic acid (PFOS) was the most dominant PFAS present in all soil samples (between 9 and 2600 μg/kg). Leaching was quantified using a one-step batch test with water (L/S 10). PFOS concentrations measured in leachate water ranged between 1.2 μg/L and 212 μg/L. Sorbent amendment (3%) was tested by adding activated carbon (AC), compost soil and montmorillonite to selected soils. The extent of immobilisation was quantified by measuring PFAS concentrations in leachate before and after amendment. Leaching was reduced between 94 and 99.9% for AC, between 29 and 34% for compost soil and between 28 and 40% for the montmorillonite amended samples. Sorbent + soil/water partitioning coefficients (K D ) were estimated following amendment and were around 8 L/kg for compost soil and montmorillonite amended soil and ranged from 1960 to 16,940 L/kg for AC amended soil. The remediation of AFFF impacted soil via immobilisation of PFAS following sorbent amendment with AC is promising as part of an overall remediation strategy. Copyright © 2016 Elsevier Ltd. All rights reserved.

Attrition of limestone by impact loading in fluidized beds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fabrizio Scala; Fabio Montagnaro; Piero Salatino

2007-09-15

The present study addresses limestone attrition and fragmentation associated with impact loading, a process which may occur extensively in various regions of fluidized bed (FB) combustors/gasifiers, primarily the jetting region of the bottom bed, the exit region of the riser, and the cyclone. An experimental protocol for the characterization of the propensity of limestone to undergo attrition/fragmentation by impact loading is reported. The application of the protocol is demonstrated with reference to an Italian limestone whose primary fragmentation and attrition by surface wear have already been characterized in previous studies. The experimental procedure is based on the characterization of themore » amount and particle size distribution of the debris generated upon the impact of samples of sorbent particles against a target. Experiments were carried out at a range of particle impact velocities between 10 and 45 m/s, consistent with jet velocities corresponding to typical pressure drops across FB gas distributors. The protocol has been applied to either raw or preprocessed limestone samples. In particular, the effect of calcination, sulfation, and calcination/recarbonation cycles on the impact damage suffered by sorbent particles has been assessed. The measurement of particle voidage and pore size distribution by mercury intrusion was also accomplished to correlate fragmentation with the structural properties of the sorbent samples. Fragmentation by impact loading of the limestone is significant. Lime displays the largest propensity to undergo impact damage, followed by the sorbent sulfated to exhaustion, the recarbonated sorbent, and the raw limestone. Fragmentation of the raw limestone and of the sulfated lime follows a pattern typical of the failure of brittle materials. The fragmentation behavior of lime and recarbonated lime better conforms to a disintegration failure mode, with an extensive generation of very fine fragments. 27 refs., 9 figs. 1 tab.« less

Magnetic solid-phase extraction using carbon nanotubes as sorbents: a review.

PubMed

Herrero-Latorre, C; Barciela-García, J; García-Martín, S; Peña-Crecente, R M; Otárola-Jiménez, J

2015-09-10

Magnetic solid-phase extraction (M-SPE) is a procedure based on the use of magnetic sorbents for the separation and preconcentration of different organic and inorganic analytes from large sample volumes. The magnetic sorbent is added to the sample solution and the target analyte is adsorbed onto the surface of the magnetic sorbent particles (M-SPs). Analyte-M-SPs are separated from the sample solution by applying an external magnetic field and, after elution with the appropriate solvent, the recovered analyte is analyzed. This approach has several advantages over traditional solid phase extraction as it avoids time-consuming and tedious on-column SPE procedures and it provides a rapid and simple analyte separation that avoids the need for centrifugation or filtration steps. As a consequence, in the past few years a great deal of research has been focused on M-SPE, including the development of new sorbents and novel automation strategies. In recent years, the use of magnetic carbon nanotubes (M-CNTs) as a sorption substrate in M-SPE has become an active area of research. These materials have exceptional mechanical, electrical, optical and magnetic properties and they also have an extremely large surface area and varied possibilities for functionalization. This review covers the synthesis of M-CNTs and the different approaches for the use of these compounds in M-SPE. The performance, general characteristics and applications of M-SPE based on magnetic carbon nanotubes for organic and inorganic analysis have been evaluated on the basis of more than 110 references. Finally, some important challenges with respect the use of magnetic carbon nanotubes in M-SPE are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of drugs of abuse in human plasma using microextraction by packed sorbents and ultra-high-performance liquid chromatography.

PubMed

Fernández, P; González, M; Regenjo, M; Ares, A M; Fernández, A M; Lorenzo, R A; Carro, A M

2017-02-17

A miniaturized and simple method based on digitally programmed microextraction by packed sorbent (eVol ® -MEPS) coupled to ultra-performance liquid chromatography (UPLC) has been developed for quantitative determination of three synthetic cathinones and seven conventional drugs of abuse and metabolites. The influence of several extraction parameters, such as washing and elution solvents were tested. In addition important variables affecting MEPS performance, namely sample volume, sorbent drying time, washing solvent volume, elution volume, number of extraction cycles, sorbent phase and pH, were evaluated using an asymmetrical screening design. The optimal experimental conditions involved 300μL of plasma, loading 10×100μL of sample through a C8/SCX sorbent in a MEPS syringe placed in the semi-automatic eVol ® system, washing using 150μL H 2 O:MeOH (90:10, v/v), drying for 0.5min and elution using 200μL dichloromethane:2-propanol:ammonium hydroxide (78:20:2, v/v/v). The drugs separation was achieved using an ACQUITY BEH Shield RP18 column (2.1mm×100mm×1.7μm) in 3min. Under optimized conditions the proposed method was validated in terms of selectivity, linearity, limits of detection (LOD) and quantitation (LOQ), precision and matrix effect, using standard addition calibration. The combination of MEPS and UPLC provides a method for the primary screening of the analytes in 18min with excellent recoveries at three concentration levels, ranging between 80 and 104% (relative standard deviation <11%). The developed methodology has been successfully applied to plasma samples from polydrug abusers. Copyright © 2017 Elsevier B.V. All rights reserved.

The evaluation of different sorbents for the preconcentration of phenoxyacetic acid herbicides and their metabolites from soils.

PubMed

Moret, Sònia; Sánchez, Juan M; Salvadó, Victòria; Hidalgo, Manuela

2005-12-16

A procedure using alkaline extraction, solid-phase extraction (SPE) and HPLC is developed to analyze the polar herbicides 2,4-dichlorophenoxyacetic acid (2,4-D) and 4-chloro-2-methylphenoxyacetic acid (MCPA) together with their main metabolites in soils. An ion-pairing HPLC method is used for the determination as it permits the baseline separation of these highly polar herbicides and their main metabolites. The use of a highly cross-linked polystyrene-divinylbenzene sorbent (PS-DVB) gives the best results for the analysis of these compounds. This sorbent allows the direct preconcentration of the analytes at the high pH values obtained after quantitative alkaline extraction of the herbicides from soil samples. Different parameters are evaluated for the SPE preconcentration step. The high polarity of the main analytes of interest (2,4-D and MCPA) makes it necessary to work at low flow rates (< or =0.5 mL min(-1)) in order for these compounds to be retained by the PS-DVB sorbent. A two stage desorption from the SPE sorbent is required to obtain the analytes in solvents that are appropriate for HPLC determination. A first desorption with a 50:50 methanol:water mixture elutes the most polar analytes (2,4-D, MCPA and 2CP). The second elution step with methanol permits the analysis of the other phenol derivatives. The humic and fulvic substances present in the soil are not efficiently retained by PS-DVB sorbents at alkaline pH's and so do not interfere in the analysis. This method has been successfully applied in the analysis of soil samples from a golf course treated with a commercial product containing esters of 2,4-D and MCPA as the active components.

Development and evaluation of needle trap device geometry and packing methods for automated and manual analysis.

PubMed

Warren, Jamie M; Pawliszyn, Janusz

2011-12-16

For air/headspace analysis, needle trap devices (NTDs) are applicable for sampling a wide range of volatiles such as benzene, alkanes, and semi-volatile particulate bound compounds such as pyrene. This paper describes a new NTD that is simpler to produce and improves performance relative to previous NTD designs. A NTD utilizing a side-hole needle used a modified tip, which removed the need to use epoxy glue to hold sorbent particles inside the NTD. This design also improved the seal between the NTD and narrow neck liner of the GC injector; therefore, improving the desorption efficiency. A new packing method has been developed and evaluated using solvent to pack the device, and is compared to NTDs prepared using the previous vacuum aspiration method. The slurry packing method reduced preparation time and improved reproducibility between NTDs. To evaluate the NTDs, automated headspace extraction was completed using benzene, toluene, ethylbenzene, p-xylene (BTEX), anthracene, and pyrene (PAH). NTD geometries evaluated include: blunt tip with side-hole needle, tapered tip with side-hole needle, slider tip with side-hole, dome tapered tip with side-hole and blunt with no side-hole needle (expanded desorptive flow). Results demonstrate that the tapered and slider tip NTDs performed with improved desorption efficiency. Copyright © 2011 Elsevier B.V. All rights reserved.

Evaluation of carbon aerogel-based solid-phase extraction sorbent for the analysis of sulfur mustard degradation products in environmental water samples.

PubMed

Jõul, Piia; Vaher, Merike; Kuhtinskaja, Maria

2018-05-01

In this study, SPE method using a carbon aerogel(CA)-based sorbent was developed and evaluated for the simultaneous extraction of sulfur mustard (HD) degradation products from environmental water samples. Applied CAs proved to be very promising materials for use as SPE sorbents, due to their high porosity, very low density and a large specific surface area. 10 degradation products of HD, both aliphatic and cyclic (thiodiglycol (TDG), TDG sulfoxide, TDG sulfone, 3,5-dithia-1,7-heptanediol, 3,6-dithia-1,8-octanediol, 1,4-thioxane, 1,3-dithiolane, 1,4-dithiane, 1,2,5-trithiepane, and 1,4,5-oxadithiepane) were extracted on a CA-based SPE cartridge. The concentrations of target analytes in the eluate were determined by HPLC-DAD and CE-DAD. Several parameters affecting the extraction efficiency, including the kind and volume of the eluting solvent, sample loading flow rate, volume and ionic strength as well as the reusability of the cartridge, were investigated and optimized to achieve the best performance for the analytes. A series of quantitative parameters such as linear range, coefficient of determination, LOD, LOQ and precision were examined under the optimized conditions. High sensitivity (LODs 0.17-0.50 μM) and high precision (intraday RSD = 2.0-7.7% and interday RSD = 2.7-9.9%) for all the analytes were achieved. The performance of the CA-based sorbent was compared with that of commonly used SPE sorbents. Applied for the analysis of spiked pore water samples collected from the Bornholm Basin, one of the largest chemical warfare dumping sites in the Baltic Sea, the proposed method allowed high SPE recoveries of all the analytes ranging from 83.5 to 99.7% to be obtained. Copyright © 2018 Elsevier Ltd. All rights reserved.

Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

PubMed

Sheikhian, Leila; Bina, Sedigheh

2016-01-15

In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Vortex-Assisted Dispersive Micro-Solid Phase Extraction Using CTAB-Modified Zeolite NaY Sorbent Coupled with HPLC for the Determination of Carbamate Insecticides.

PubMed

Salisaeng, Pawina; Arnnok, Prapha; Patdhanagul, Nopbhasinthu; Burakham, Rodjana

2016-03-16

A vortex-assisted dispersive micro-solid phase extraction (VA-D-μ-SPE) based on cetyltrimethylammonium bromide (CTAB)-modified zeolite NaY was developed for preconcentration of carbamate pesticides in fruits, vegetables, and natural surface water prior to analysis by high performance liquid chromatography with photodiode array detection. The small amounts of solid sorbent were dispersed in a sample solution, and extraction occurred by adsorption in a short time, which was accelerated by vortex agitation. Finally, the sorbents were filtered from the solution, and the analytes were subsequently desorbed using an appropriate solvent. Parameters affecting the VA-D-μ-SPE performance including sorbent amount, sample volume, desorption solvent ,and vortex time were optimized. Under the optimum condition, linear dynamic ranges were achieved between 0.004-24.000 mg kg(-1) (R(2) > 0.9946). The limits of detection (LODs) ranged from 0.004-4.000 mg kg(-1). The applicability of the developed procedure was successfully evaluated by the determination of the carbamate residues in fruits (dragon fruit, rambutan, and watermelon), vegetables (cabbage, cauliflower, and cucumber), and natural surface water.

Synthesis and application of nano-, meso- and macroporous sorbents based on lignin for detoxication of biological fluids

NASA Astrophysics Data System (ADS)

Chopabayeva, Nazira N.; Mukanov, Kanatbek N.; Tasmagambet, Amandyk T.

2014-05-01

Novel nano-, meso- and macroporous sorbents based on hydrolysis lignin have been synthesized by catalytic o-alkylation of biolpolymer with epoxy resin ED-20 and subsequent amination of formed α-oxyde derivative. Composition, structure, morphology and physical, chemical properties of ion-exchangers were investigated by FTIR, SEM, TEM, porosimetry and potentiometric titration method. It has been established that alkaline activated lignin shows an increase of SBET to 20.9 m2/g while modification leads to decrease of SBET more than double (from 9.2 to 5.2 m2/g) that of an untreared sample (14.5 m2/g). Synthesized sorbents are characterized by approximately identical mesoporous structure and mainly contained a pore size of 10-14 nm. The results clearly demonstrate the efficiency of lignin based sorbents for the removal of water and lipid soluble toxic metabolites from blood serum of diabetic retinopathy patients. Samples reduced the high level of total cholesterol, including its most atherogenic fractions (LDL-C, VLDL-C), triglyceride to the level of optimum compensated diabetes without significant removal of HDL-C. Concentration of glucose was decreased to physiological norms.

Removal of copper(II) from some environmental samples by sorptive-flotation using powdered marble wastes as sorbents and oleic acid as surfactant.

PubMed

Ghazy, S E; Samra, S E; Mahdy, A F M; El-Morsy, S M

2004-11-01

A simple and economic experimental sorptive -flotation procedure is presented for the removal of copper(II) species from aqueous solutions. It is based on using powdered marble wastes (PMW), which are widespread and inexpensive and may represent an environmental problem, as the effective inorganic sorbent and oleic (HOL) as the surfactant. The main parameters (i.e. initial solution pH, sorbent, surfactant and copper concentrations, stirring times, ionic strength, temperature and the presence of foreign ions) influencing the flotation of PMW and /or Cu(II) were examined. Nearly, 100% of PMW and Cu(II) were removed from aqueous solutions at pH7 after stirring for 10 min and at room temperature, (approximately 25 degrees C). The procedure was successfully applied to recover Cu(II) spiked to some natural water samples. A mechanism for sorption and flotation is suggested.

Determination of acrylamide in brewed coffee and coffee powder using polymeric ionic liquid-based sorbent coatings in solid-phase microextraction coupled to gas chromatography-mass spectrometry.

PubMed

Cagliero, Cecilia; Ho, Tien D; Zhang, Cheng; Bicchi, Carlo; Anderson, Jared L

2016-06-03

This study describes a simple and rapid sampling method employing a polymeric ionic liquid (PIL) sorbent coating in direct immersion solid-phase microextraction (SPME) for the trace-level analysis of acrylamide in brewed coffee and coffee powder. The crosslinked PIL sorbent coating demonstrated superior sensitivity in the extraction of acrylamide compared to all commercially available SPME coatings. A spin coating method was developed to evenly distribute the PIL coating on the SPME support and reproducibly produce fibers with a large film thickness. Ninhydrin was employed as a quenching reagent during extraction to inhibit the production of interfering acrylamide. The PIL fiber produced a limit of quantitation for acrylamide of 10μgL(-1) and achieved comparable results to the ISO method in the analysis of six coffee powder samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of azoxystrobin and chlorothalonil using a methacrylate-based polymer modified with gold nanoparticles as solid-phase extraction sorbent.

PubMed

Catalá-Icardo, Mónica; Gómez-Benito, Carmen; Simó-Alfonso, Ernesto Francisco; Herrero-Martínez, José Manuel

2017-01-01

This paper describes a novel and sensitive method for extraction, preconcentration, and determination of two important widely used fungicides, azoxystrobin, and chlorothalonil. The developed methodology is based on solid-phase extraction (SPE) using a polymeric material functionalized with gold nanoparticles (AuNPs) as sorbent followed by high-performance liquid chromatography (HPLC) with diode array detector (DAD). Several experimental variables that affect the extraction efficiency such as the eluent volume, sample flow rate, and salt addition were optimized. Under the optimal conditions, the sorbent provided satisfactory enrichment efficiency for both fungicides, high selectivity and excellent reusability (>120 re-uses). The proposed method allowed the detection of 0.05 μg L -1 of the fungicides and gave satisfactory recoveries (75-95 %) when it was applied to drinking and environmental water samples (river, well, tap, irrigation, spring, and sea waters).

Selective extraction of clonazepam from human plasma and urine samples by molecularly imprinted polymeric beads.

PubMed

Panahi, Homayon Ahmad; Mehramizi, Ali; Ghassemi, Somayeh; Moniri, Elham

2014-03-01

A molecularly imprinted polymer (MIP) based on free-radical polymerization was prepared with 1-(N,N-biscarboxymethyl)amino-3-allylglycerol and N,N-dimethylacrylamide as functional monomers, N,N-methylene diacrylamide as the cross-linker, copper ion-clonazepam as the template and 2,2-azobis(2-methylbutyronitrile) as the initiator. The imprinted polymer was characterized by Fourier transform infrared spectroscopy, elemental analysis, thermo-gravimetric analysis, and SEM. The MIP of agglomerated microparticles with multipores was used for SPE. The imprinted polymer sorbent was selective for clonazepam. The optimum pH and sorption capacity were 5 and 0.18 mg/g at 20C, respectively. The profile of the drug uptake by the sorbent reflects good accessibility of the active sites in the imprinted polymer sorbent. The MIP-SPE was the most feasible technique for the extraction of clonazepam with a high recovery from human plasma and urine samples.

Evaluation of sample recovery of malodorous livestock gases from air sampling bags, solid-phase microextraction fibers, Tenax TA sorbent tubes, and sampling canisters.

PubMed

Koziel, Jacek A; Spinhirne, Jarett P; Lloyd, Jenny D; Parker, David B; Wright, Donald W; Kuhrt, Fred W

2005-08-01

Odorous gases associated with livestock operations are complex mixtures of hundreds if not thousands of compounds. Research is needed to know how best to sample and analyze these compounds. The main objective of this research was to compare recoveries of a standard gas mixture of 11 odorous compounds from the Carboxen/PDMS 75-microm solid-phase microextraction fibers, polyvinyl fluoride (PVF; Tedlar), fluorinated ethylene propylene copolymer (FEP; Teflon), foil, and polyethylene terephthalate (PET; Melinex) air sampling bags, sorbent 2,b-diphenylene-oxide polymer resin (Tenax TA) tubes, and standard 6-L Stabilizer sampling canisters after sample storage for 0.5, 24, and 120 (for sorbent tubes only) hrs at room temperature. The standard gas mixture consisted of 7 volatile fatty acids (VFAs) from acetic to hexanoic, and 4 semivolatile organic compounds including p-cresol, indole, 4-ethylphenol, and 2'-aminoacetophenone with concentrations ranging from 5.1 ppb for indole to 1270 ppb for acetic acid. On average, SPME had the highest mean recovery for all 11 gases of 106.2%, and 98.3% for 0.5- and 24-hr sample storage time, respectively. This was followed by the Tenax TA sorbent tubes (94.8% and 88.3%) for 24 and 120 hr, respectively; PET bags (71.7% and 47.2%), FEP bags (75.4% and 39.4%), commercial Tedlar bags (67.6% and 22.7%), in-house-made Tedlar bags (47.3% and 37.4%), foil bags (16.4% and 4.3%), and canisters (4.2% and 0.5%), for 0.5 and 24 hr, respectively. VFAs had higher recoveries than semivolatile organic compounds for all of the bags and canisters. New FEP bags and new foil bags had the lowest and the highest amounts of chemical impurities, respectively. New commercial Tedlar bags had measurable concentrations of N,N-dimethyl acetamide and phenol. Foil bags had measurable concentrations of acetic, propionic, butyric, valeric, and hexanoic acids.

Selectivity and limitations of carbon sorption tubes for capturing siloxanes in biogas during field sampling.

PubMed

Tansel, Berrin; Surita, Sharon C

2016-06-01

Siloxane levels in biogas can jeopardize the warranties of the engines used at the biogas to energy facilities. The chemical structure of siloxanes consists of silicon and oxygen atoms, alternating in position, with hydrocarbon groups attached to the silicon side chain. Siloxanes can be either in cyclic (D) or linear (L) configuration and referred with a letter corresponding to their structure followed by a number corresponding to the number of silicon atoms present. When siloxanes are burned, the hydrocarbon fraction is lost and silicon is converted to silicates. The purpose of this study was to evaluate the adequacy of activated carbon gas samplers for quantitative analysis of siloxanes in biogas samples. Biogas samples were collected from a landfill and an anaerobic digester using multiple carbon sorbent tubes assembled in series. One set of samples was collected for 30min (sampling 6-L gas), and the second set was collected for 60min (sampling 12-L gas). Carbon particles were thermally desorbed and analyzed by Gas Chromatography Mass Spectrometry (GC/MS). The results showed that biogas sampling using a single tube would not adequately capture octamethyltrisiloxane (L3), hexamethylcyclotrisiloxane (D3), octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6). Even with 4 tubes were used in series, D5 was not captured effectively. The single sorbent tube sampling method was adequate only for capturing trimethylsilanol (TMS) and hexamethyldisiloxane (L2). Affinity of siloxanes for activated carbon decreased with increasing molecular weight. Using multiple carbon sorbent tubes in series can be an appropriate method for developing a standard procedure for determining siloxane levels for low molecular weight siloxanes (up to D3). Appropriate quality assurance and quality control procedures should be developed for adequately quantifying the levels of the higher molecular weight siloxanes in biogas with sorbent tubes. Copyright © 2016 Elsevier Ltd. All rights reserved.

Immobilized humic substances and immobilized aggregates of humic substances as sorbent for solid phase extraction.

PubMed

Erny, Guillaume L; Gonçalves, Bruna M; Esteves, Valdemar I

2013-09-06

In this work, humic substances (HS) immobilized, as a thin layer or as aggregates, on silica gel were tested as material for solid phase extraction. Some triazines (simazine, atrazine, therbutylazine, atrazine-desethyl-desisopropyl-2-hydroxy, ametryn and terbutryn), have been selected as test analytes due to their environmental importance and to span a large range of solubility and octanol/water partition coefficient (logP). The sorbent was obtained immobilizing a thin layer of HS via physisorption on a pre-coated silica gel with a cationic polymer (polybrene). While the sorbent could be used as it is, it was demonstrated that additional HS could be immobilized, via weak interactions, to form stable humic aggregates. However, while a higher quantity of HS could be immobilized, no significant differences were observed in the sorption parameters. This sorbent have been tested for solid phase extraction to concentrate triazines from aqueous matrixes. The sorbent demonstrated performances equivalent to commercial alternatives as a concentration factor between 50 and 200, depending on the type of triazines, was obtained. Moreover the low cost and the high flow rate of sample through the column allowed using high quantity of sorbent. The analytical procedure was tested with different matrixes including tap water, river water and estuarine water. Copyright © 2013 Elsevier B.V. All rights reserved.

Long-Term Uptake of Phenol-Water Vapor Follows Similar Sigmoid Kinetics on Prehydrated Organic Matter- and Clay-Rich Soil Sorbents.

PubMed

Borisover, Mikhail; Bukhanovsky, Nadezhda; Lado, Marcos

2017-09-19

Typical experimental time frames allowed for equilibrating water-organic vapors with soil sorbents might lead to overlooking slow chemical reactions finally controlling a thermodynamically stable state. In this work, long-term gravimetric examination of kinetics covering about 4000 h was performed for phenol-water vapor interacting with four materials pre-equilibrated at three levels of air relative humidity (RHs 52, 73, and 92%). The four contrasting sorbents included an organic matter (OM)-rich peat soil, an OM-poor clay soil, a hydrophilic Aldrich humic acid salt, and water-insoluble leonardite. Monitoring phenol-water vapor interactions with the prehydrated sorbents, as compared with the sorbent samples in phenol-free atmosphere at the same RH, showed, for the first time, a sigmoid kinetics of phenol-induced mass uptake typical for second-order autocatalytic reactions. The apparent rate constants were similar for all the sorbents, RHs and phenol activities studied. A significant part of sorbed phenol resisted extraction, which was attributed to its abiotic oxidative coupling. Phenol uptake by peat and clay soils was also associated with a significant enhancement of water retention. The delayed development of the sigmoidal kinetics in phenol-water uptake demonstrates that long-run abiotic interactions of water-organic vapor with soil may be overlooked, based on short-term examination.

Determination of airborne carbonyls: comparison of a thermal desorption/GC method with the standard DNPH/HPLC method.

PubMed

Ho, Steven Sai Hang; Yu, Jian Zhen

2004-02-01

The standard method for the determination of gaseous carbonyls is to collect carbonyls onto 2,4-dinitrophenyl hydrazine (DNPH) coated solid sorbent followed by solvent extraction of the solid sorbent and analysis of the derivatives using high-pressure liquid chromatography (HPLC). This paper describes a newly developed approach that involves collection of the carbonyls onto pentafluorophenyl hydrazine (PFPH) coated solid sorbents followed by thermal desorption and gas chromatographic (GC) analysis of the PFPH derivatives with mass spectrometric (MS) detection. Sampling tubes loaded with 510 nmol of PFPH on Tenax sorbent effectively collect gaseous carbonyls, including formaldehyde, acetaldehyde, propanal, butanal, heptanal, octanal, acrolein, 2-furfural, benzaldehyde, p-tolualdehyde, glyoxal, and methylglyoxal, at a flow rate of at least up to 100 mL/min. All of the tested carbonyls are shown to have method detection limits (MDLs) of subnanomoles per sampling tube, corresponding to air concentrations of <0.3 ppbv for a sampled volume of 24 L. These limits are 2-12 times lower than those that can be obtained using the DNPH/HPLC method. The improvement of MDLs is especially pronounced for carbonyls larger than formaldehyde and acetaldehyde. The PFPH/GC method also offers better peak separation and more sensitive and specific detection through the use of MS detection. Comparison studies on ambient samples and kitchen exhaust samples have demonstrated that the two methods do not yield systematic differences in concentrations of the carbonyls that are above their respective MDLs in both methods, including formaldehyde, acetaldehyde, acrolein, and butanal. The lower MDLs afforded by the PFPH/ GC method also enable the determination of a few more carbonyls in both applications.

Removal of dissolved textile dyes from wastewater by a compost sorbent

USGS Publications Warehouse

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.

Dithizone-modified graphene oxide nano-sheet as a sorbent for pre-concentration and determination of cadmium and lead ions in food.

PubMed

Moghadam Zadeh, Hamid Reza; Ahmadvand, Parvaneh; Behbahani, Ali; Amini, Mostafa M; Sayar, Omid

2015-01-01

Graphene oxide nano-sheet was modified with dithizone as a novel sorbent for selective pre-concentration and determination of Cd(II) and Pb(II) in food. The sorbent was characterised by various analytical methods and the effective parameters for Cd(II) and Pb(II) adsorption were optimised during this work. The high adsorption capacity and selectivity of this sorbent makes the method capable of fast determinations of the Cd(II) and Pb(II) content in complicated matrices even at μg l(-1) levels using commonly available instrumentation. The precision of this method was < 1.9% from 10 duplicate determinations and its accuracy verified using standard reference materials. Finally, this method was applied to the determination of Cd(II) and Pb(II) ions in common food samples and satisfactory results were obtained.

Effect of sorbent attrition on utilization

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

1992-10-01

During this period, the project has focused on two aspects of attrition; (1) mechanical attrition which is responsible for particle fracture whenever particles are moving with respect to a fixed reference frame, and (2) chemical attrition which can be responsible for particle fracture whenever particles undergo reactions. The experiments were conducted with calcium based sorbent materials. Two specific project objectives were identified and studied. The first of these was to determine the effect of temperature, particle velocity, and particle surface area on the extent of attrition in a circulating fluidized reactor. The second was to investigate if attrition could improvemore » sorbent utilization of typical calcium based sorbents of small size (<20 [mu]m). A sample of sulfated calcium hydroxide sorbent was obtained for attrition tests in a circulating fluidized bed reactor. Attempts at attriting this material in the fluidized bed were not successful, and no improvements in sorbent utilization were measured in subsequent TGA tests with the solids. However, an analysis of the other constituents in the particles revealed that a major portion of the hydroxide had been converted to calcium carbonate. This gave rise to the possibility that dolomitic hydroxide may have characteristics which may be beneficial and that improvements in utilization could be realized by means of chemical attrition. This is due to the thermal instability of magnesium carbonate at temperatures above 650[degree]F which means that magnesium oxide will be the major unreacted magnesium species in spent sorbent.« less

Effect of sorbent attrition on utilization. Final report, August 1, 1991--August 31, 1992

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

1992-10-01

During this period, the project has focused on two aspects of attrition; (1) mechanical attrition which is responsible for particle fracture whenever particles are moving with respect to a fixed reference frame, and (2) chemical attrition which can be responsible for particle fracture whenever particles undergo reactions. The experiments were conducted with calcium based sorbent materials. Two specific project objectives were identified and studied. The first of these was to determine the effect of temperature, particle velocity, and particle surface area on the extent of attrition in a circulating fluidized reactor. The second was to investigate if attrition could improvemore » sorbent utilization of typical calcium based sorbents of small size (<20 {mu}m). A sample of sulfated calcium hydroxide sorbent was obtained for attrition tests in a circulating fluidized bed reactor. Attempts at attriting this material in the fluidized bed were not successful, and no improvements in sorbent utilization were measured in subsequent TGA tests with the solids. However, an analysis of the other constituents in the particles revealed that a major portion of the hydroxide had been converted to calcium carbonate. This gave rise to the possibility that dolomitic hydroxide may have characteristics which may be beneficial and that improvements in utilization could be realized by means of chemical attrition. This is due to the thermal instability of magnesium carbonate at temperatures above 650{degree}F which means that magnesium oxide will be the major unreacted magnesium species in spent sorbent.« less

Trapping guests within a nanoporous metal-organic framework through pressure-induced amorphization.

PubMed

Chapman, Karena W; Sava, Dorina F; Halder, Gregory J; Chupas, Peter J; Nenoff, Tina M

2011-11-23

The release of guest species from within a nanoporous metal-organic framework (MOF) has been inhibited by amorphization of the guest-loaded framework structure under applied pressure. Thermogravimetric analyses have shown that by amorphizing ZIF-8 following sorption of molecular I(2), a hazardous radiological byproduct of nuclear energy production, the pore apertures in the framework are sufficiently distorted to kinetically trap I(2) and improve I(2) retention. Pair distribution function (PDF) analysis indicates that the local structure of the captive I(2) remains essentially unchanged upon amorphization of the framework, with the amorphization occurring under the same conditions for the vacant and guest-loaded framework. The low, accessible pressure range needed to effect this change in desorption is much lower than in tradition sorbents such as zeolites, opening the possibility for new molecular capture, interim storage, or controlled release applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harper, M.

A sorbent to be used for air sampling must meet certain performance criteria including sample background, capacity, stability, and recovery. Anasorb{sup R} 747 is a proprietary 20/40 mesh beaded active carbon prepared from raw materials with a very low ash content in a process which creates a regular pore structure. The background is very low for both inorganic and organic species, and the surface is more inert and less hydrophilic than coconut charcoal, while capacity is similar. The low catalytic activity of the surface means samples of many reactive compounds remain stable for longer periods. The sorbent is compatible withmore » most solvent systems in use (e.g. carbon disulfide, methylene chloride, methanol, dimethyformamide). Anasorb 747 can be coated with chemicals for efficient adsorption of inorganic gases, which can be analyzed at very low levels because of low background interference. A large number of validated sampling methods use Anasorb 747, including methods from OSHA and NIOSH, corporate industrial hygiene laboratories, various branches of the EPA, and international agencies. These methods refer to around fifty different gases and vapors. Although this sorbent is not compatible with some compounds (e.g. low molecular weight aldehydes) it is quite close to being of universal application.« less

Development of a flow system for the determination of cadmium in fuel alcohol using vermicompost as biosorbent and flame atomic absorption spectrometry.

PubMed

Bianchin, Joyce Nunes; Martendal, Edmar; Mior, Renata; Alves, Vanessa Nunes; Araújo, Cleide Sandra Tavares; Coelho, Nívia Maria Melo; Carasek, Eduardo

2009-04-30

In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L(-1), a sample flow rate of 4.5 mL min(-1) and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 microg L(-1) and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 microg L(-1), with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 microg L(-1), n=7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%.

In situ studies of materials for high temperature CO2 capture and storage.

PubMed

Dunstan, Matthew T; Maugeri, Serena A; Liu, Wen; Tucker, Matthew G; Taiwo, Oluwadamilola O; Gonzalez, Belen; Allan, Phoebe K; Gaultois, Michael W; Shearing, Paul R; Keen, David A; Phillips, Anthony E; Dove, Martin T; Scott, Stuart A; Dennis, John S; Grey, Clare P

2016-10-20

Carbon capture and storage (CCS) offers a possible solution to curb the CO 2 emissions from stationary sources in the coming decades, considering the delays in shifting energy generation to carbon neutral sources such as wind, solar and biomass. The most mature technology for post-combustion capture uses a liquid sorbent, amine scrubbing. However, with the existing technology, a large amount of heat is required for the regeneration of the liquid sorbent, which introduces a substantial energy penalty. The use of alternative sorbents for CO 2 capture, such as the CaO-CaCO 3 system, has been investigated extensively in recent years. However there are significant problems associated with the use of CaO based sorbents, the most challenging one being the deactivation of the sorbent material. When sorbents such as natural limestone are used, the capture capacity of the solid sorbent can fall by as much as 90 mol% after the first 20 carbonation-regeneration cycles. In this study a variety of techniques were employed to understand better the cause of this deterioration from both a structural and morphological standpoint. X-ray and neutron PDF studies were employed to understand better the local surface and interfacial structures formed upon reaction, finding that after carbonation the surface roughness is decreased for CaO. In situ synchrotron X-ray diffraction studies showed that carbonation with added steam leads to a faster and more complete conversion of CaO than under conditions without steam, as evidenced by the phases seen at different depths within the sample. Finally, in situ X-ray tomography experiments were employed to track the morphological changes in the sorbents during carbonation, observing directly the reduction in porosity and increase in tortuosity of the pore network over multiple calcination reactions.

Solid-phase extraction of galloyl- and caffeoylquinic acids from natural sources (Galphimia glauca and Arnicae flos) using pure zirconium silicate and bismuth citrate powders as sorbents inside micro spin columns.

PubMed

Hussain, Shah; Schönbichler, Stefan A; Güzel, Yüksel; Sonderegger, Harald; Abel, Gudrun; Rainer, Matthias; Huck, Christian W; Bonn, Günther K

2013-10-01

Galloyl- and caffeoylquinic acids are among the most important pharmacological active groups of natural compounds. This study describes a pre-step in isolation of some selected representatives of these groups from biological samples. A selective solid-phase extraction (SPE) method for these compounds may help assign classes and isomer designations within complex mixtures. Pure zirconium silicate and bismuth citrate powders (325 mesh) were employed as two new sorbents for optimized SPE of phenolic acids. These sorbents possess electrostatic interaction sites which accounts for additional interactions for carbon acid moieties as compared to hydrophilic and hydrophobic sorbents alone. Based on this principle, a selective SPE method for 1,3,4,5-tetragalloylquinic acid (an anti-HIV and anti-asthamatic agent) as a starting compound was developed and then deployed upon other phenolic acids with success. The recoveries and selectivities of both sorbents were compared to most commonly applied and commercially available sorbents by using high performance liquid chromatography. The nature of interaction between the carrier sorbent and the acidic target molecules was investigated by studying hydrophilic (silica), hydrophobic (C18), mixed-mode (ionic and hydrophobic: Oasis(®) MAX) and predominantly electrostatic (zirconium silicate) materials. The newly developed zirconium silicate and bismuth citrate stationary phases revealed promising results for the selective extraction of galloyl- and caffeoylquinic acids from natural sources. It was observed that zirconium silicate exhibited maximum recovery and selectivity for tetragalloylquinic acid (84%), chlorogenic acid (82%) and dicaffeoylquinic acid (94%) among all the tested sorbents. Copyright © 2013 Elsevier B.V. All rights reserved.

Final Project Report for DOE/EERE High-Capacity and Low-Cost Hydrogen-Storage Sorbents for Automotive Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Hong-Cai; Liu, Di-Jia

This report provides a review of the objectives, progress, and milestones of the research conducted during this project on the topic of developing innovative metal-organic frameworks (MOFs) and porous organic polymers (POPs) for high-capacity and low-cost hydrogen-storage sorbents in automotive applications.1 The objectives of the proposed research were to develop new materials as next-generation hydrogen storage sorbents that meet or exceed DOE’s 2017 performance targets of gravimetric capacity of 0.055 kg H 2/kg system and volumetric capacity of 0.040 kg H 2/L system at a cost of $400/kg H 2 stored. Texas A&M University (TAMU) and Argonne National Laboratory (ANL)more » collaborated in developing low-cost and high-capacity hydrogen-storage sorbents with appropriate stability, sorption kinetics, and thermal conductivity. The research scope and methods developed to achieve the project’s goals include the following: Advanced ligand design and synthesis to construct MOF sorbents with optimal hydrogen storage capacities, low cost and high stability; Substantially improve the hydrogen uptake capacity and chemical stability of MOF-based sorbents by incorporating high valent metal ions during synthesis or through the post-synthetic metal metathesis oxidation approach; Enhance sorbent storage capacity through material engineering and characterization; Generate a better understanding of the H 2-sorbent interaction through advanced characterization and simulation. Over the course of the project 5 different MOFs were developed and studied: PCN-250, PCN-12, PCN-12’, PCN-608 and PCN-609.2-3 Two different samples were submitted to the National Renewable Energy Laboratory (NREL) in order to validate their hydrogen adsorption capacity, PCN-250 and PCN-12. Neither of these samples reached the project’s Go/No-Go requirements but the data obtained did further prove the hypothesis that the presence of open metal sites oriented towards MOF pores help to surpass the predicted hydrogen uptakes described by Chahine’s rule.4 These observations are believed to have a major impact on the hydrogen storage community, and may potentially lead to the development of a material that could meet the DOE goals for hydrogen storage systems for automotive applications.« less

Molecularly imprinted polymer/cryogel composites for solid-phase extraction of bisphenol A from river water and wine.

PubMed

Baggiani, Claudio; Baravalle, Patrizia; Giovannoli, Cristina; Anfossi, Laura; Giraudi, Gianfranco

2010-05-01

Superporous monolithic hydrogels (cryogel monoliths) are elastic, sponge-like materials that can be prepared in an aqueous medium through a cryotropic gelation technique. These monoliths show interesting properties for the development of high-throughput solid-phase extraction supports to treat large volumes of aqueous samples. In this work, a cryogel-supported molecularly imprinted solid-phase extraction approach for the endocrine disruptor bisphenol A (BPA) from river water and wine samples is presented. An imprinted polymer with molecular recognition properties for BPA was prepared in acetonitrile by thermal polymerization of a mixture of 4,4'-dihydroxy-2,2-diphenyl-1,1,1,3,3,3-trifluoropropane as a mimic template of BPA, 4-vinylpyridine and trimethylolpropane trimethacrylate in a molar ratio of 1 + 6 + 6. Fine imprinted particles (<10 microm) were embedded in a poly-acrylamide-co-N,N'-methylenbisacrylamide cryogel obtained by ammonium persulfate-induced cryopolymerization at -18 degrees C. The resulting monolithic gel was evaluated for its use as a sorbent support in an off-line solid-phase extraction approach to recover BPA from dilute aqueous samples with minimum pre-loading work-up. The optimized extraction protocol resulted in a reliable MISPE method suitable to selectively extract and preconcentrate BPA from river water and red wine samples, demonstrating the practical feasibility of cryogel-trapped imprinted polymers as solid-phase extraction materials.

Magnetic dispersive solid-phase extraction based on graphene oxide/Fe3 O4 @polythionine nanocomposite followed by atomic absorption spectrometry for zinc monitoring in water, flour, celery and egg.

PubMed

Babaei, Azar; Zeeb, Mohsen; Es-Haghi, Ali

2018-07-01

Magnetic graphene oxide nanocomposite has been proposed as a promising and sustainable sorbent for the extraction and separation of target analytes from food matrices. Sample preparation based on nanocomposite presents several advantages, such as desired efficiency, reasonable selectivity and high surface-area-to-volume ratio. A new graphene oxide/Fe 3 O 4 @polythionine (GO/Fe 3 O 4 @PTh) nanocomposite sorbent was introduced for magnetic dispersive solid-phase extraction and flame atomic absorption spectrometric detection of zinc(II) in water, flour, celery and egg. To fabricate the sorbent, an oxidative polymerization of thionine on the surface of magnetic GO was applied, while polythionine was simply employed as a surface modifier to improve extraction yield. The properties of the sorbent were characterized by transmission electron microscopy, scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray analysis, vibrating sample magnetometry and Fourier transform-infrared spectroscopy. The calibration curve showed linearity in the range of 0.5-30 ng mL -1 . Limits of detection (S/N = 3) and quantification (S/N = 10) were 0.08 and 0.5 ng mL -1 , respectively. The method was applied for trace-level determination of Zn(II) in water and food samples, and its validation was investigated by recovery experiments and analyzing certified reference material. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A sensitive microextraction by packed sorbent-based methodology combined with ultra-high pressure liquid chromatography as a powerful technique for analysis of biologically active flavonols in wines.

PubMed

Silva, Catarina L; Gonçalves, João L; Câmara, José S

2012-08-20

A new approach based on microextraction by packed sorbent (MEPS) and reversed-phase high-throughput ultra high pressure liquid chromatography (UHPLC) method that uses a gradient elution and diode array detection to quantitate three biologically active flavonols in wines, myricetin, quercetin, and kaempferol, is described. In addition to performing routine experiments to establish the validity of the assay to internationally accepted criteria (selectivity, linearity, sensitivity, precision, accuracy), experiments are included to assess the effect of the important experimental parameters such as the type of sorbent material (C2, C8, C18, SIL, and C8/SCX), number of extraction cycles (extract-discard), elution volume, sample volume, and ethanol content, on the MEPS performance. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (250μL) in five extraction cycle and in a short time period (about 5min for the entire sample preparation step). Under optimized conditions, excellent linearity (R(values)(2)>0.9963), limits of detection of 0.006μgmL(-1) (quercetin) to 0.013μgmL(-1) (myricetin) and precision within 0.5-3.1% were observed for the target flavonols. The average recoveries of myricetin, quercetin and kaempferol for real samples were 83.0-97.7% with relative standard deviation (RSD, %) lower than 1.6%. The results obtained showed that the most abundant flavonol in the analyzed samples was myricetin (5.8±3.7μgmL(-1)). Quercetin (0.97±0.41μgmL(-1)) and kaempferol (0.66±0.24μgmL(-1)) were found in a lower concentration. The optimized MEPS(C8) method was compared with a reverse-phase solid-phase extraction (SPE) procedure using as sorbent a macroporous copolymer made from a balanced ratio of two monomers, the lipophilic divinylbenzene and the hydrophilic N-vinylpyrrolidone (Oasis HLB) were used as reference. MEPS(C8) approach offers an attractive alternative for analysis of flavonols in wines, providing a number of advantages including highest extraction efficiency (from 85.9±0.9% to 92.1±0.5%) in the shortest extraction time with low solvent consumption, fast sample throughput, more environmentally friendly and easy to perform. Copyright © 2012 Elsevier B.V. All rights reserved.

Subtask 4.24 - Field Evaluation of Novel Approach for Obtaining Metal Emission Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pavlish, John; Laudal, Dennis; Thompson, Jeffrey

2013-12-31

Over the past two decades, emissions of mercury, nonmercury metals, and acid gases from energy generation and chemical production have increasingly become an environmental concern. On February 16, 2012, the U.S. Environmental Protection Agency (EPA) promulgated the Mercury and Air Toxics Standards (MATS) to reduce mercury, nonmercury metals, and HCl emissions from coal-fired power plants. The current reference methods for trace metals and halogens are wet-chemistry methods, EPA Method (M) 29 and M26A, respectively. As a possible alternative to EPA M29 and M26A, the Energy & Environmental Research Center (EERC) has developed a novel multielement sorbent trap (ME-ST) method tomore » be used to sample for trace elements and/or halogens. Testing was conducted at three different power plants, and the results show that for halogens, the ME-ST halogen (ME-ST-H) method did not show any significant bias compared to EPA M26A and appears to be a potential candidate to serve as an alternative to the reference method. For metals, the ME-ST metals (ME-ST-M) method offers a lower detection limit compared to EPA M29 and generally produced comparable data for Sb, As, Be, Cd, Co, Hg, and Se. Both the ME-ST-M and M29 had problems associated with high blanks for Ni, Pb, Cr, and Mn. Although this problem has been greatly reduced through improved trap design and material selection, additional research is still needed to explore possible longer sampling durations and/or selection of lower background materials before the ME-ST-M can be considered as a potential alternative method for all the trace metals listed in MATS.« less

Multiresidue analysis of synthetic pyrethroid pesticides in grapes by gas chromatography with programmed temperature vaporizing-large volume injection coupled with ion trap mass spectrometry.

PubMed

Banerjee, Kaushik; Savant, Rahul H; Dasgupta, Soma; Patil, Sangram H; Oulkar, Dasharath P; Adsule, Pandurang G

2010-01-01

A multiresidue analysis method was optimized and validated for simultaneous estimation of 21 synthetic pyrethroid pesticides and their isomers in grape matrix at 10 ng/g and higher levels. The method involves extraction of a 10 g sample with 10 mL ethyl acetate, cleanup by dispersive SPE with primary-secondary amine (25 mg) sorbent, and estimation by GC/MS/MS large volume injection (LVI) through a programmed temperature vaporizer (PTV) injector. The PTV-LVI parameters of the gas chromatograph and the multiple reaction monitoring (MRM) parameters of the ion trap mass spectrometer were optimized for each compound to achieve the highest SIN. For each analyte, the unique and most abundant MRM transition was used for quantification, along with the next most abundant MRM transition for confirmatory identification. The abundance ratio of the confirmatory to quantifier MRMs was used to ensure unambiguous residue monitoring in unknown samples within a 20% tolerance range at the 10 ng/g level. The analytes were separated on a TR-5MS capillary column within a 22 min run time. The method was selective and sensitive and ensured separation of the synthetic pyrethroids from high-boiling matrix components. The LOD and LOQ of the analytes ranged between 0.5 to 3.1 and 2.5 to 10 ng/g, respectively. Linearity of solvent and matrix-matched calibrations between 2.0 and 250 ng/g was established for each compound with r2 > 0.99. Recovery at 10, 25, and 50 ng/g levels of fortification in grapes ranged within 77-115% with associated RSD values (n = 8) up to 20%.

Trace quantification of selected sulfonamides in aqueous media by implementation of a new dispersive solid-phase extraction method using a nanomagnetic titanium dioxide graphene-based sorbent and HPLC-UV.

PubMed

Izanloo, Maryam; Esrafili, Ali; Behbahani, Mohammad; Ghambarian, Mahnaz; Reza Sobhi, Hamid

2018-02-01

Herein, a new dispersive solid-phase extraction method using a nano magnetic titanium dioxide graphene-based sorbent in conjunction with high-performance liquid chromatography and ultraviolet detection was successfully developed. The method was proved to be simple, sensitive, and highly efficient for the trace quantification of sulfacetamide, sulfathiazole, sulfamethoxazole, and sulfadiazine in relatively large volume of aqueous media. Initially, the nano magnetic titanium dioxide graphene-based sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy and X-ray diffraction. Then, the sorbent was used for the sorption and extraction of the selected sulfonamides mainly through π-π stacking hydrophobic interactions. Under the established conditions, the calibration curves were linear over the concentration range of 1-200 μg/L. The limit of quantification (precision of 20%, and accuracy of 80-120%) for the detection of each sulfonamide by the proposed method was 1.0 μg/L. To test the extraction efficiency, the method was applied to various fortified real water samples. The average relative recoveries obtained from the fortified samples varied between 90 and 108% with the relative standard deviations of 5.3-10.7%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of several solid-phase extraction sorbents for continuous determination of amines in water by gas chromatography-mass spectrometry.

PubMed

Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

2009-08-15

A semiautomatic method has been proposed for the determination of different types of amines in water samples including anilines, chloroanilines, N-nitrosamines and aliphatic amines. The analytes were retained on a solid-phase extraction sorbent column and after elution, 1 microL of the extract was analysed by gas chromatography coupled with electron impact ionization mass spectrometry. A systematic overview is given of the advantages and disadvantages of several sorbents (LiChrolut EN, Oasis HLB, RP-C(18), graphitized carbon black, fullerenes and nanotubes) in the retention of amine compounds and based on sensitivity, selectivity and reliability. The retention efficiency for the studied amines was higher (ca. 100%) with LiChrolut EN and Oasis HLB than it was with RP-C(18) and fullerenes (53 and 62%, respectively, on average). Detection limits of 0.5-16 ng L(-1) for the 27 amines studied were obtained when using a sorbent column containing 75 mg of LiChrolut EN for 100mL of sample, the RSD being lower than 6.5%. The method was applied with good accuracy and precision in the determination of amines in various types of water including river, pond, tap, well, drinking, swimming pool and waste.

Selective trace enrichment of chlorotriazine pesticides from natural waters and sediment samples using terbuthylazine molecularly imprinted polymers

USGS Publications Warehouse

Ferrer, I.; Lanza, F.; Tolokan, A.; Horvath, V.; Sellergren, B.; Horvai, G.; Barcelo, D.

2000-01-01

Two molecularly imprinted polymers were synthesized using either dichloromethane or toluene as the porogen and terbuthylazine as the template and were used as solid-phase extraction cartridges for the enrichment of six chlorotriazines (deisopropylatrazine, deethylatrazine, simazine, atrazine, propazine, and terbuthylazine) in natural water and sediment samples. The extracted samples were analyzed by liquid chromatography/diode array detection (LC/DAD). Several washing solvents, as well as different volumes, were tested for their ability to remove the matrix components nonspecifically adsorbed on the sorbents. This cleanup step was shown to be of prime importance to the successful extraction of the pesticides from the aqueous samples. The optimal analytical conditions were obtained when the MIP imprinted using dichloromethane was the sorbent, 2 mL of dichloromethane was used in the washing step, and the preconcentrated analytes were eluted with 8 mL of methanol. The recoveries were higher than 80% for all the chlorotriazines except for propazine (53%) when 50- or 100-mL groundwater samples, spiked at 1 ??g/L level, were analyzed. The limits of detection varied from 0.05 to 0.2 ??g/L when preconcentrating a 100-mL groundwater sample. Natural sediment samples from the Ebre Delta area (Tarragona, Spain) containing atrazine and deethylatrazine were Soxhlet extracted and analyzed by the methodology developed in this work. No significant interferences from the sample matrix were noticed, thus indicating good selectivity of the MIP sorbents used.

Sample integrity evaluation and EPA method 325B interlaboratory comparison for select volatile organic compounds collected diffusively on Carbopack X sorbent tubes

NASA Astrophysics Data System (ADS)

Oliver, Karen D.; Cousett, Tamira A.; Whitaker, Donald A.; Smith, Luther A.; Mukerjee, Shaibal; Stallings, Casson; Thoma, Eben D.; Alston, Lillian; Colon, Maribel; Wu, Tai; Henkle, Stacy

2017-08-01

A sample integrity evaluation and an interlaboratory comparison were conducted in application of U.S. Environmental Protection Agency (EPA) Methods 325A and 325B for diffusively monitoring benzene and other selected volatile organic compounds (VOCs) using Carbopack X sorbent tubes. To evaluate sample integrity, VOC samples were refrigerated for up to 240 days and analyzed using thermal desorption/gas chromatography-mass spectrometry at the EPA Office of Research and Development laboratory in Research Triangle Park, NC, USA. For the interlaboratory comparison, three commercial analytical laboratories were asked to follow Method 325B when analyzing samples of VOCs that were collected in field and laboratory settings for EPA studies. Overall results indicate that the selected VOCs collected diffusively on sorbent tubes generally were stable for 6 months or longer when samples were refrigerated. This suggests the specified maximum 30-day storage time of VOCs collected diffusively on Carbopack X passive samplers and analyzed using Method 325B might be able to be relaxed. Interlaboratory comparison results were in agreement for the challenge samples collected diffusively in an exposure chamber in the laboratory, with most measurements within ±25% of the theoretical concentration. Statistically significant differences among laboratories for ambient challenge samples were small, less than 1 part per billion by volume (ppbv). Results from all laboratories exhibited good precision and generally agreed well with each other.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lu, D.Y.; Hughes, R.W.; Anthony, E.J.

Sintering during calcination/carbonation may introduce substantial economic penalties for a CO{sub 2} looping cycle using limestone/dolomite-derived sorbents. Cyclic carbonation and calcination reactions were investigated for CO{sub 2} capture under fluidized bed combustion (FBC) conditions. The cyclic carbonation characteristics of CaCO{sub 3}-derived sorbents were compared at various calcination temperatures (700-925{sup o} C) and different gas stream compositions: pure -2 and a realistic calciner environment where high concentrations of CO{sub 2}>80-90% are expected. The conditions during carbonation were 700 {sup o}C and 15% CO{sub 2} in N{sub 2} and 0.18% or 0.50% SO{sub 2} in selected tests. Up to 20 calcination/carbonation cyclesmore » were conducted using a thermogravimetric analyzer (TGA) apparatus. Three Canadian limestones were tested: Kelly Rock, Havelock, and Cadomin, using a prescreened particle size range of 400-650 {mu} m. Calcined Kelly Rock and Cadomin samples were hydrated by steam and examined. Sorbent reactivity was reduced whenever SO{sub 2} was introduced to either the calcining or carbonation streams. The multicyclic capture capacity of CaO for CO{sub 2} was substantially reduced at high concentrations of CO{sub 2} during the sorbent regeneration process and carbonation conversion of the Kelly Rock sample obtained after 20 cycles was only 10.5%. Hydrated sorbents performed better for CO{sub 2} capture but showed deterioration following calcination in high CO{sub 2} gas streams indicating that high CO{sub 2} and SO{sub 2} levels in the gas stream lead to lower CaO conversion because of enhanced sintering and irreversible formation of CaSO{sub 4}.« less

Preparation of dye waste-barium sulfate hybrid adsorbent and application in organic wastewater treatment.

PubMed

Hu, Zhang-Jun; Xiao, Yan; Zhao, Dan-Hua; Shen, Yu-Lin; Gao, Hong-Wen

2010-03-15

A new hybrid material was developed by the template-free hybridization of weak acidic pink red B (APRB, C.I. 18073) with BaSO(4). The composition and structure of the material were determined and characterized. In contrast to conventional sorbents, the hybrid material has a specific surface area of 0.89 m(2)/g, but it contains lots of negative charges and lipophilic groups as the basis of specific adsorption. The efficient removal of cationic dyes and persistent organic pollutants (POPs) indicates that it has an improved adsorption capacity and selectivity with a short removal time less than 2 min; while the hybrid sorbents fit the Langmuir isotherm model, and follow the octanol-water partition law. Instead of using APRB reagent, an APRB-producing wastewater was reused to prepare the cost-effective sorbent, and the equilibrium adsorption capacities of which reached 222 and 160 mg/g for EV and BPR, respectively. The sorbents was then used to treat three wastewater samples with satisfactory results of over 97% decolonization and 88% COD-decreasing. In addition, the hybrid sorbent was regenerated from sludge over five cycles, and its adsorption capacity was not appreciably changed. This work has developed a simple and eco-friendly method for synthesizing a practical and efficient sorbent. (c) 2009 Elsevier B.V. All rights reserved.

Quaternary ammonium-functionalized silica sorbents for the solid-phase extraction of aromatic amines under normal phase conditions.

PubMed

Vidal, Lorena; Robin, Orlane; Parshintsev, Jevgeni; Mikkola, Jyri-Pekka; Riekkola, Marja-Liisa

2013-04-12

Quaternary ammonium-functionalized silica materials were synthesized and applied for solid-phase extraction (SPE) of aromatic amines, which are classified as priority pollutants by US Environmental Protection Agency. Hexamethylenetetramine used for silica surface modification for the first time was employed as SPE sorbent under normal phase conditions. Hexaminium-functionalized silica demonstrated excellent extraction efficiencies for o-toluidine, 4-ethylaniline and quinoline (recoveries 101-107%), while for N,N-dimethylaniline and N-isopropylaniline recoveries were from low to moderate (14-46%). In addition, the suitability of 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica as SPE sorbent was tested under normal phase conditions. The recoveries achieved for the five aromatic amines ranged from 89 to 99%. The stability of the sorbent was evaluated during and after 150 extractions. Coefficients of variation between 4.5 and 10.2% proved a high stability of the synthesized sorbent. Elution was carried out using acetonitrile in the case of hexaminium-functionalized silica and water for 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent. After the extraction the analytes were separated and detected by liquid chromatography ultraviolet detection (LC-UV). The retention mechanism of the materials was primarily based on polar hydrogen bonding and π-π interactions. Comparison made with activated silica proved the quaternary ammonium-functionalized materials to offer different selectivity and better extraction efficiencies for aromatic amines. Finally, 1-alkyl-3-(propyl-3-sulfonate) imidazolium-functionalized silica sorbent was successfully tested for the extraction of wastewater and soil samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Potential Use of Passive Sampling for Environmental Monitoring of Petroleum E&P Operations

EPA Pesticide Factsheets

Traditional environmental monitoring relies on water or soil samples being taken at various time increments and sent to offsite laboratories for analysis. Reliance on grab samples generally captures limited “snapshots” of environmental contaminant concentrations, is time intensive, costly, and generates residual waste from excess sample and/or reagents used in the analysis procedures. As an alternative, we are evaluating swellable organosilica sorbents to create passive sampling systems for monitoring applications. Previous work has focused on absorption and detection of fuels, chlorinated solvents, endocrine disruptors, explosives, pesticides, fluorinated chemicals, and metals including Ba, Sr, Hg, Pb, Fe, Cu, and Zn. The advantages of swellable organosilica are that the material cancapture target compounds for an extended periods of time, does not absorb natural organic matter, and resists biofilm formation since the sorbent possesses an animated surface morphology.

Alternative Methods for Assessing Contaminant Transport from the Vadose Zone to Indoor Air

NASA Astrophysics Data System (ADS)

Baylor, K. J.; Lee, A.; Reddy, P.; Plate, M.

2010-12-01

Vapor intrusion, which is the transport of contaminant vapors from groundwater and the vadose zone to indoor air, has emerged as a significant human health risk near hazardous waste sites. Volatile organic compounds (VOCs) such as trichloroethylene (TCE) and tetrachloroethylene (PCE) can volatilize from groundwater and from residual sources in the vadose zone and enter homes and commercial buildings through cracks in the slab, plumbing conduits, or other preferential pathways. Assessment of the vapor intrusion pathway typically requires collection of groundwater, soil gas, and indoor air samples, a process which can be expensive and time-consuming. We evaluated three alternative vapor intrusion assessment methods, including 1) use of radon as a surrogate for vapor intrusion, 2) use of pressure differential measurements between indoor/outdoor and indoor/subslab to assess the potential for vapor intrusion, and 3) use of passive, longer-duration sorbent methods to measure indoor air VOC concentrations. The primary test site, located approximately 30 miles south of San Francisco, was selected due to the presence of TCE (10 - 300 ug/L) in shallow groundwater (5 to 10 feet bgs). At this test site, we found that radon was not a suitable surrogate to asses vapor intrusion and that pressure differential measurements are challenging to implement and equipment-intensive. More significantly, we found that the passive, longer-duration sorbent methods are easy to deploy and compared well quantitatively with standard indoor air sampling methods. The sorbent technique is less than half the cost of typical indoor air methods, and also provides a longer duration sample, typically 3 to 14 days rather than 8 to 24 hours for standard methods. The passive sorbent methods can be a reliable, cost-effective, and easy way to sample for TCE, PCE and other VOCs as part of a vapor intrusion investigation.

Use of graphene supported on aminopropyl silica for microextraction of parabens from water samples.

PubMed

Fumes, Bruno Henrique; Lanças, Fernando Mauro

2017-03-03

This paper describes the synthesis, characterization and use of graphene supported on aminopropyl silica through covalent bonds (Si-G) as a sorbent for microextraction by packed sorbent (MEPS). Five parabens (methyl, ethyl, propyl, butyl and benzyl) present in water matrices were used as model compounds for this evaluation. The Si-G phase was compared to other sorbents used in MEPS (C18 and Strata™-X) and also with graphene supported on primary-secondary amine (PSA) silica, where Si-G showed better results. After this, the MEPS experimental parameters were optimized using the Si-G sorbent. The following variables were optimized through univariate experiments: pH (4,7 and 10), desorption solvent (ACN:MeOH (50:50), ACN:H 2 O (40:60), MeOH and ACN) and ionic strength (0, 10 and 20% of NaCl). A factorial design 2 6-2 was then employed to evaluate other variables, such as the sample volume, desorption volume, sampling cycles, wash cycles and desorption cycles, as well as the influence of NaCl% on the extraction performance. The optimized method achieved a linear range of 0.2-20μg/L for most parabens; weighted calibration models were employed during the linearity evaluation to reduce the absolute sum of the residue values and improve R 2 , which ranged from 0.9753 to 0.9849. The method's accuracy was 82.3-119.2%; precision, evaluated as the coefficient of variance for intraday and interday analysis, ranged from 1.5 to 19.2%. After evaluation of the figures of merit, the method was applied to the determination of parabens in water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

High-efficiency headspace sampling of volatile organic compounds in explosives using capillary microextraction of volatiles (CMV) coupled to gas chromatography-mass spectrometry (GC-MS).

PubMed

Fan, Wen; Almirall, José

2014-03-01

A novel geometry configuration based on sorbent-coated glass microfibers packed within a glass capillary is used to sample volatile organic compounds, dynamically, in the headspace of an open system or in a partially open system to achieve quantitative extraction of the available volatiles of explosives with negligible breakthrough. Air is sampled through the newly developed sorbent-packed 2 cm long, 2 mm diameter capillary microextraction of volatiles (CMV) and subsequently introduced into a commercially available thermal desorption probe fitted directly into a GC injection port. A sorbent coating surface area of ∼5 × 10(-2) m(2) or 5,000 times greater than that of a single solid-phase microextraction (SPME) fiber allows for fast (30 s), flow-through sampling of relatively large volumes using sampling flow rates of ∼1.5 L/min. A direct comparison of the new CMV extraction to a static (equilibrium) SPME extraction of the same headspace sample yields a 30 times improvement in sensitivity for the CMV when sampling nitroglycerine (NG), 2,4-dinitrotoluene (2,4-DNT), and diphenylamine (DPA) in a mixture containing a total mass of 500 ng of each analyte, when spiked into a liter-volume container. Calibration curves were established for all compounds studied, and the recovery was determined to be ∼1 % or better after only 1 min of sampling time. Quantitative analysis is also possible using this extraction technique when the sampling temperature, flow rate, and time are kept constant between calibration curves and the sample.

Balsam-Pear-Skin-Like Porous Polyacrylonitrile Nanofibrous Membranes Grafted with Polyethyleneimine for Postcombustion CO2 Capture.

PubMed

Zhang, Yufei; Guan, Jiming; Wang, Xianfeng; Yu, Jianyong; Ding, Bin

2017-11-22

Amine-containing sorbents have been extensively studied for postcombustion carbon dioxide (CO 2 ) capture because of their ability to chemisorb CO 2 from the flue gas. However, most sorbents are in the form of powders currently, which is not the ideal configuration for the flue gas separation because of the fragile nature and poor mechanical properties, resulting in blocking of the flow pipes and difficult recycling. Herein, we present a novel approach for the facile fabrication of flexible, robust, and polyethyleneimine-grafted (PEI-grafted) hydrolyzed porous PAN nanofibrous membranes (HPPAN-PEI NFMs) through the combination of electrospinning, pore-forming process, hydrolysis reaction, and the subsequent grafting technique. Excitingly, we find that all the resultant porous PAN (PPAN) fibers exhibit a balsam-pear-skin-like porous structure due to the selective removal of poly(vinylpyrrolidone) (PVP) from PAN/PVP fibers by water extraction. Significantly, the HPPAN-PEI NFMs retain their mesoporosity, as well as exhibit good thermal stability and prominent tensile strength (11.1 MPa) after grafting, guaranteeing their application in CO 2 trapping from the flue gas. When exposed to CO 2 at 40 °C, the HPPAN-PEI NFMs show an enhanced CO 2 adsorption capacity of 1.23 mmol g -1 (based on the overall quantity of the sample) or 6.15 mmol g -1 (based on the quantity of grafted PEI). Moreover, the developed HPPAN-PEI NFMs display significantly selective capture for CO 2 over N 2 and excellent recyclability. The CO 2 capacity retains 92% of the initial value after 20 adsorption-desorption cycle tests, indicating that the resultant HPPAN-PEI NFMs have good long-term stability. This work paves the way for fabricating NFM-based solid adsorption materials endowed with a porous structure applied to efficient postcombustion CO 2 capture.

Green Preconcentration of Trace Amounts of Copper from Water and Food Samples onto Novel Organo-Nanoclay Prior to Flame Atomic Absorption Spectrometry.

PubMed

Beyki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

2014-01-01

In this work, the nanoclay was intercalated with acyclovir (9-[(2-hydroxyethoxy) methyl] guanine), the toxicity of which to mammalian cells is very low. We used no organic solvents for preparation of modified clay and desorption of Cu ions from the sorbent. Batch and column methods were used, and sorption of Cu was quantitative (>98%) in the pH range of 7.5 to 10.0. Quantitative desorption occurred with 5.0 mL of 3.0 M HCl, and the amount of Cu(II) was measured by using flame atomic absorption spectrometry. In the initial solution the linear dynamic range and the LOD were 3.0-1000.0 and 0.58 μg/L, respectively. With 500.0 mL of sample, an enrichment factor of 100 was obtained. The RSD was 2.0% (n = 8, concentration = 0.5 mg/L), and the maximum capacity of the sorbent was 45.0 mg/g. The influence of experimental parameters including sample pH, ionic strength, type and volume of the eluent, and interference of some ions on the recoveries of Cu was investigated. The proposed method using a new and easier prepared solid sorbent was applied to the determination of Cu in different real samples with satisfactory results.

Sol-gel/nanoclay composite as a sorbent for microextraction in packed syringe combined with corona discharge ionization ion mobility spectrometry for the determination of diazinon in water samples.

PubMed

Saraji, Mohammad; Jafari, Mohammad Taghi; Amooshahi, Mohammad Mehdi

2018-01-01

In this work, the microextraction in packed syringe technique combined with corona discharge ion mobility spectrometry was used for determining diazinon in water samples. A new porous composite of nanoclay and polysiloxane was prepared using a sol-gel process. An amount of 2.0 mg of the sorbent was packed in a 250 μL syringe and used for extraction. A volume of 2 mL of the sample was passed through the sorbent bed, and the entrapped analyte was eluted by 25 μL of methanol. Important parameters influencing the extraction performance were investigated. Under optimum experimental conditions, the detection limit for diazinon was 0.07 ng/mL. The intra- and inter-day relative standard deviations were 5.0 and 12.3%, respectively. The calibration curve was linear in the concentration range from 0.2 to 20.0 ng/mL (r 2  = 0.999). The applicability of the method was demonstrated by analyzing spiked real water samples and the spiking recoveries were in the range of 95 to 106%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

PubMed

Ebrahimi, Bahram

2017-03-01

A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

Device for collecting chemical compounds and related methods

DOEpatents

Scott, Jill R.; Groenewold, Gary S.; Rae, Catherine

2013-01-01

A device for sampling chemical compounds from fixed surfaces and related methods are disclosed. The device may include a vacuum source, a chamber and a sorbent material. The device may utilize vacuum extraction to volatilize the chemical compounds from the fixed surfaces so that they may be sorbed by the sorbent material. The sorbent material may then be analyzed using conventional thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) instrumentation to determine presence of the chemical compounds. The methods may include detecting release and presence of one or more chemical compounds and determining the efficacy of decontamination. The device may be useful in collection and analysis of a variety of chemical compounds, such as residual chemical warfare agents, chemical attribution signatures and toxic industrial chemicals.

Devices for collecting chemical compounds

DOEpatents

Scott, Jill R; Groenewold, Gary S

2013-12-24

A device for sampling chemical compounds from fixed surfaces and related methods are disclosed. The device may include a vacuum source, a chamber and a sorbent material. The device may utilize vacuum extraction to volatilize the chemical compounds from a fixed surface so that they may be sorbed by the sorbent material. The sorbent material may then be analyzed using conventional thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) instrumentation to determine presence of the chemical compounds. The methods may include detecting release and presence of one or more chemical compounds and determining the efficacy of decontamination. The device may be useful in collection and analysis of a variety of chemical compounds, such as residual chemical warfare agents, chemical attribution signatures and toxic industrial chemicals.

EVALUATION OF SOLID SORBENTS FOR WATER SAMPLING

EPA Science Inventory

The report describes a systematic evaluation of the applicability of macroreticular resins for general and compound-specific sampling of organics. The first portion is an extensive review of current pertinent literature concerned with the use of macroreticular resins for sampling...

Magnetic solid phase extraction and gas chromatography-mass spectrometrical analysis of sixteen polycyclic aromatic hydrocarbons.

PubMed

Cai, Ying; Yan, Zhihong; NguyenVan, Manh; Wang, Lijia; Cai, Qingyun

2015-08-07

Fluorenyl functionalized superparamagnetic core/shell magnetic nanoparticles (MNPs, Fe3O4@SiO2@Flu) were prepared and characterized by transmission electron microscope, X-ray diffraction and infrared spectroscopy. The MNPs having an average diameter of 200nm were then used as solid-phase extraction sorbent for the determination of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in water samples designated by United States Environmental Protection Agency (U.S. EPA). The main influencing parameters, including sorbent amount, desorption solvent, sample volume and extraction time were optimized. Analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels. Limit of detection ranging from 0.5 to 4.0ng/L were obtained. The repeatability was investigated by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) lower than 13.1%. Finally, the proposed method was successfully applied for the determination of PAHs in water samples with the recoveries in the range of 96.0-106.7%. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of Bark Beetle Infestation on Secondary Organic Aerosol Precursors in the Western United States

NASA Astrophysics Data System (ADS)

Huff Hartz, K. E.; Amin, H.; Dodson, C.; Atkins, P. T.; Hallar, G.

2009-12-01

Bark beetles are a potentially destructive force in forest ecosytems; however, it is not known how insect attacks affect the atmosphere. Other insects, such as the weevil (Strophosoma melanogrammum) attacks on spruce trees in Denmark, have a significant local effect on monoterpene emissions. In fact, a single weevil induced a three-fold increase in monoterpene emission, and the response lasted for several weeks. Mountain pine bark beetles (Dendroctonus ponderosae) have infested the forests in the vicinity of Storm Peak Laboratory near Steamboat Springs, Colorado. Emissions were sampled from the headspace of bark at the trunk and from the tree branches in the canopy from bark beetle infested and healthy lodgepole pine (Pinus contorta var. latifolia) and Engelmann spruce (Picea engelmannii) trees. The emissions were collected onto scent traps, containing 110 mg of Porapak Q sorbent, using PAS-500 micro air samplers set to a 0.4 mL/min flow rate for two hours. After collection, the scent traps were spiked with a recovery standard, perdeutrated decane, and extracted with 1.5 mL hexanes (in three portions). The analytes in the extracts were separated and detected using gas chromatography/mass spectroscopy. The analytes were identified and quantified using calibration curves from authentic standards, and when authentic standards were not available, the NIST mass spectra library and Adams retention time indices were used. The samples from lodgepole pine trees suggest an enhancement in the 3-carene, beta-phellandrene, and estragole (methyl chavicol) emissions upon bark beetle infestation. The samples from the Engelmann spruce trees suggest an enhancement in the 1,4-cineole, p-cymene, and beta-phellandrene emissions upon bark beetle infestation. A shift in the type and the quantity of VOC emissions due to bark beetle infestation may lead increases in SOA from these forests, since potent SOA precursors are produced.

A novel metal-organic framework composite MIL-101(Cr)@GO as an efficient sorbent in dispersive micro-solid phase extraction coupling with UHPLC-MS/MS for the determination of sulfonamides in milk samples.

PubMed

Jia, Xiuna; Zhao, Pan; Ye, Xiu; Zhang, Lianjun; Wang, Ting; Chen, Qinyu; Hou, Xiaohong

2017-07-01

As a novel material, metal-organic framework/graphite oxide (MIL-101(Cr)@GO) has great potential for the pretreatment of trace analytes. In the present study, MIL-101(Cr)@GO was synthesized using a solvothermal synthesis method at the nanoscale and was applied as sorbent in the dispersive micro-solid phase extraction (DMSPE) for the enrichment of the trace sulfonamides (SAs) from milk samples for the first time. Several experimental parameters including kinds of sorbents, the effect of pH, the amount of MIL-101(Cr)@GO, ionic strength, adsorption time, desorption solvent and desorption time were investigated. Under the optimal conditions, the linear ranges were from 0.1 to 10μg/L, 0.2-20μg/L or 0.5-50μg/L for the analytes with regression coefficients (r) from 0.9942 to 0.9999. The limits of detection were between 0.012 and 0.145μg/L. The recoveries ranged from 79.83% to 103.8% with relative standard deviations (RSDs)<10% (n=3). MIL-101(Cr)@GO exhibited remarkable advantages compared to MIL-101(Cr), MIL-100(Fe), activated carbon and other sorbent materials used in pretreatment methods. A simple, rapid, sensitive, inexpensive and less solvent consuming method of DMSPE-ultra-high performance liquid chromatography-tandem mass spectrometry (DMSPE-UHPLC-MS/MS) was successfully applied to the pre-concentration and determination of twelve SAs in milk samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Preconcentration of Trace Neonicotinoid Insecticide Residues Using Vortex-Assisted Dispersive Micro Solid-Phase Extraction with Montmorillonite as an Efficient Sorbent.

PubMed

Moyakao, Khwankaew; Santaladchaiyakit, Yanawath; Srijaranai, Supalax; Vichapong, Jitlada

2018-04-11

In this work, we investigated montmorillonite for adsorption of neonicotinoid insecticides in vortex-assisted dispersive micro-solid phase extraction (VA-d-μ-SPE). High-performance liquid chromatography with photodiode array detection was used for quantification and determination of neonicotinoid insecticide residues, including thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid. In this method, the solid sorbent was dispersed into the aqueous sample solution and vortex agitation was performed to accelerate the extraction process. Finally, the solution was filtered from the solid sorbent with a membrane filter. The parameters affecting the extraction efficiency of the proposed method were optimized, such as amount of sorbent, sample volume, salt addition, type and volume of extraction solvent, and vortex time. The adsorbing results show that montmorillonite could be reused at least 4 times and be used as an effective adsorbent for rapid extraction/preconcentration of neonicotinoid insecticide residues. Under optimum conditions, linear dynamic ranges were achieved between 0.5 and 1000 ng mL -1 with a correlation of determination ( R² ) greater than 0.99. Limit of detection (LOD) ranged from 0.005 to 0.065 ng mL -1 , while limit of quantification (LOQ) ranged from 0.008 to 0.263 ng mL -1 . The enrichment factor (EF) ranged from 8 to 176-fold. The results demonstrated that the proposed method not only provided a more simple and sensitive method, but also can be used as a powerful alternative method for the simultaneous determination of insecticide residues in natural surface water and fruit juice samples.

Multi-Column Xe/Kr Separation with AgZ-PAN and HZ-PAN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Greenhalgh, Mitchell Randy; Garn, Troy Gerry; Welty, Amy Keil

Previous multi-column xenon/krypton separation tests have demonstrated the capability of separating xenon from krypton in a mixed gas feed stream. The results of this initial testing with AgZ-PAN and HZ-PAN indicated that an excellent separation of xenon from krypton could be achieved. Building upon these initial results, a series of additional multi-column testing were performed in FY-16. The purpose of this testing was to scale up the sorbent beds, test a different composition of feed gas and attempt to improve the accuracy of the analysis of the individual capture columns’ compositions. Two Stirling coolers were installed in series to performmore » this testing. The use of the coolers instead of the cryostat provided two desired improvements, 1) removal of the large dilution due to the internal volume of the cryostat adsorption chamber, and 2) ability to increase the sorbent bed size for scale-up. The AgZ-PAN sorbent, due to its xenon selectivity, was loaded in the first column to capture the xenon while allowing the krypton to flow through and be routed to a second column containing the HZ-PAN for capture and analysis. The gases captured on both columns were sampled with evacuated sample bombs and subsequently analyzed via GC-MS for both krypton and xenon. The results of these tests can be used to develop the scope of future testing and analysis using this test bed for demonstrating the capture and separation of xenon and krypton using sorbents, for demonstrating desorption and regeneration of the sorbents, and for determining compositions of the desorbed gases. They indicate a need for future desorption studies in order to better quantify co-adsorbed species and final krypton purity.« less

Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

PubMed Central

Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

2014-01-01

In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

Evaluation of the stability of a mixture of volatile organic compounds on sorbents for the determination of emissions from indoor materials and products using thermal desorption/gas chromatography/mass spectrometry.

PubMed

Brown, Veronica M; Crump, Derrick R; Plant, Neil T; Pengelly, Ian

2014-07-11

The standard method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air (ISO 16000-6:2011) specifies sampling onto the sorbent Tenax TA followed by analysis using thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS). The informative Annex D to the standard suggests the use of multi-sorbent samplers to extend the volatility range of compounds which can be determined. The aim of this study was to investigate the storage performance of Tenax TA and two multi-sorbent tubes loaded with a mixture of nine VOCs of relevance for material emissions testing. The sorbent combinations tested were quartz wool/Tenax TA/Carbograph™ 5TD and quartz wool/Tenax TA/Carbopack™ X. A range of loading levels, loading conditions (humidities and air volume), storage times (1-4 weeks) and storage conditions (refrigerated and ambient) were investigated. Longer term storage trials (up to 1 year) were conducted with Tenax TA tubes to evaluate the stability of tubes used for proficiency testing (PT) of material emissions analyses. The storage performance of the multi-sorbent tubes tested was found to be equal to that for Tenax TA, with recoveries after 4 weeks storage of within about 10% of the amounts loaded. No consistent differences in recoveries were found for the different loading or storage conditions. The longer term storage trials also showed good recovery for these compounds, although two other compounds, hexanal and BHT, were found to be unstable when stored on Tenax TA. The results of this study provide confidence in the stability of nine analytes for up to 4 weeks on two multi-sorbent tubes for material emissions testing and the same compounds loaded on Tenax TA sorbent for a recently introduced PT scheme for material emissions testing. Copyright © 2014 Elsevier B.V. All rights reserved.

Process for the enhanced capture of heavy metal emissions

DOEpatents

Biswas, Pratim; Wu, Chang-Yu

2001-01-01

This invention is directed to a process for forming a sorbent-metal complex. The process includes oxidizing a sorbent precursor and contacting the sorbent precursor with a metallic species. The process further includes chemically reacting the sorbent precursor and the metallic species, thereby forming a sorbent-metal complex. In one particular aspect of the invention, at least a portion of the sorbent precursor is transformed into sorbent particles during the oxidation step. These sorbent particles then are contacted with the metallic species and chemically reacted with the metallic species, thereby forming a sorbent-metal complex. Another aspect of the invention is directed to a process for forming a sorbent metal complex in a combustion system. The process includes introducing a sorbent precursor into a combustion system and subjecting the sorbent precursor to an elevated temperature sufficient to oxidize the sorbent precursor and transform the sorbent precursor into sorbent particles. The process further includes contacting the sorbent particles with a metallic species and exposing the sorbent particles and the metallic species to a complex-forming temperature whereby the metallic species reacts with the sorbent particles thereby forming a sorbent-metal complex under UV irradiation.

Synthesis and application of surface-imprinted activated carbon sorbent for solid-phase extraction and determination of copper (II)

NASA Astrophysics Data System (ADS)

Li, Zhenhua; Li, Jingwen; Wang, Yanbin; Wei, Yajun

2014-01-01

A new Cu(II)-imprinted amino-functionalized activated carbon sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Cu(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of Cu(II) were optimized with respect to different experimental parameters using static and dynamic procedures in detail. Compared with non-imprinted sorbent, the ion-imprinted sorbent had higher selectivity and adsorption capacity for Cu(II). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cu(II) was 26.71 and 6.86 mg g-1, respectively. The relatively selectivity factor values (αr) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 166.16, 50.77, 72.26 and 175.77, respectively, which were greater than 1. Complete elution of the adsorbed Cu(II) from Cu(II)-imprinted sorbent was carried out using 2 mL of 0.1 mol L-1 EDTA solution. The relative standard deviation of the method was 2.4% for eleven replicate determinations. The method was validated for the analysis by two certified reference materials (GBW 08301, GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace copper in natural water samples with satisfactory results.

Synthesis and application of surface-imprinted activated carbon sorbent for solid-phase extraction and determination of copper (II).

PubMed

Li, Zhenhua; Li, Jingwen; Wang, Yanbin; Wei, Yajun

2014-01-03

A new Cu(II)-imprinted amino-functionalized activated carbon sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Cu(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of Cu(II) were optimized with respect to different experimental parameters using static and dynamic procedures in detail. Compared with non-imprinted sorbent, the ion-imprinted sorbent had higher selectivity and adsorption capacity for Cu(II). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cu(II) was 26.71 and 6.86 mg g(-1), respectively. The relatively selectivity factor values (αr) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 166.16, 50.77, 72.26 and 175.77, respectively, which were greater than 1. Complete elution of the adsorbed Cu(II) from Cu(II)-imprinted sorbent was carried out using 2 mL of 0.1 mol L(-1) EDTA solution. The relative standard deviation of the method was 2.4% for eleven replicate determinations. The method was validated for the analysis by two certified reference materials (GBW 08301, GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace copper in natural water samples with satisfactory results. Copyright © 2013 Elsevier B.V. All rights reserved.

Integrated microwave processing system for the extraction of organophosphorus pesticides in fresh vegetables.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-03-01

A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of Magnetic Sorbent with Surface Modified by C18for Removal of Selected Organic Pollutants from Aqueous Samples

NASA Astrophysics Data System (ADS)

Kuráň, Pavel; Pilnaj, Dominik; Ciencialová, Lucie; Pšenička, Martin

2017-12-01

Magnetic sorbents have great potential in environmental applications due to their simple synthesis and separation in magnetic field, usability in heterogeneous systems and low toxicity. Possible syntheses, surface modifications and characteristics were described by Li et al 2013. This type of solid-phase extraction is being successfully used in various fields as health care, microbiology, biotechnologies or sample preconcentration in analytical chemistry. In this preliminary study we report on the preparation and application of magnetically separable sorbent with surface modified by C18 alkyl chain for purification of water contaminated by environmentally hazardous organic compounds. Magnetic cores were co-precipitated from Fe2+ and Fe3+ chlorides in alkalic aqueous solution. Surface of synthetized Fe3O4 was modified with SiO2 by tetraethylorthosilicate to assure physico-chemical stability. Furthermore, Fe3O4/SiO2 complex has been treated by C18 functional group, which provides good affinity towards hydrophobic substances in water. Efficiency of sorption under various conditions has been examined on benzene, toluene, ethylbenzene and xylenes (BTEX), compounds found in petroleum products which contaminate air, soil and groundwater near of store tanks. Sorption kinetics was followed by gas chromatography with mass spectrometry. The preliminary sorption kinetics data and efficiency of BTEX removal point at the possible application of prepared magnetic sorbent for BTEX removal, especially for ethylbenzene and xylenes.

A sublimate sorbent for stir-bar sorptive extraction of aqueous endocrine disruptor pesticides for gas chromatography-electron capture detection.

PubMed

Huang, Yu-Wen; Lee, Hua Kwang; Shih, Hou-Kuang; Jen, Jen-Fon

2018-06-06

A dumbbell-shaped magnetic stir-bar with sublimate sorbent was prepared for the stir bar sorptive extraction (SBSE) of pesticides in an aqueous sample prior to gas chromatography-micro-electron capture detection (GC-μECD). Cyclododecane (CDD) was coated onto a magnetic stir-bar surface as a sublimate sorbent, and steel balls were placed on both ends to form a dumbbell-shaped magnetic stir-bar for SBSE. Four EDC pesticides including chlorpyrifos, ethion, bromopropylate, and λ-cyhalothrin in aqueous samples were selected as model species to examine the proposed SBSE and the following desorption. The parameters studied were those affecting the extraction efficiencies including the coating (solvent for CDD and thickness), extraction (sample pH, stirring rate, time, and salting out effect), dissolution solvent volume, and the loss of CDD sublimated in air. The maximum extraction efficiency was obtained under the following conditions. The stir bar (with CDD thickness of 5.2 μm) was added into a 10 mL sample solution (at pH 7) for a 20-min extraction at 600 rpm. Then, the stir bar was gently removed from the sample solution, disassembled, and immersed into a 0.2 mL insert tube consisting of 3 μL hexane to dissolve; 1 μL was used for GC-ECD analysis. The linear ranges were 0.005-5 μg L -1 with coefficients of determination ranging from 0.9950 - 0.9994. Detection limits (based on S/N = 3) of the four EDCs were 0.4-4.5 ngL -1 with a relative standard deviation (RSD) of 2.4-6.3%, and quantitation limits (based on S/N = 5) were 1-15 ngL -1 . The relative recoveries of the spiked samples were in the range of 83.2-98.7% with RSDs of 2.1-8.4% in farm field waters. The proposed sublimation sorbent obtained excellent enrichment factors (101-834) and provided a simple, rapid, sensitive, and eco-friendly sample preparation method. Copyright © 2018 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

M. Mercedes Maroto-Valer; John M. Andresen; Yinzhi Zhang

This research program focused on the development of fly ash derived sorbents to capture CO{sub 2} from power plant flue gas emissions. The fly ash derived sorbents developed represent an affordable alternative to existing methods using specialized activated carbons and molecular sieves, that tend to be very expensive and hinder the viability of the CO{sub 2} sorption process due to economic constraints. Under Task 1 'Procurement and characterization of a suite of fly ashes', 10 fly ash samples, named FAS-1 to -10, were collected from different combustors with different feedstocks, including bituminous coal, PRB coal and biomass. These samples presentedmore » a wide range of LOI value from 0.66-84.0%, and different burn-off profiles. The samples also spanned a wide range of total specific surface area and pore volume. These variations reflect the difference in the feedstock, types of combustors, collection hopper, and the beneficiation technologies the different fly ashes underwent. Under Task 2 'Preparation of fly ash derived sorbents', the fly ash samples were activated by steam. Nitrogen adsorption isotherms were used to characterize the resultant activated samples. The cost-saving one-step activation process applied was successfully used to increase the surface area and pore volume of all the fly ash samples. The activated samples present very different surface areas and pore volumes due to the range in physical and chemical properties of their precursors. Furthermore, one activated fly ash sample, FAS-4, was loaded with amine-containing chemicals (MEA, DEA, AMP, and MDEA). The impregnation significantly decreased the surface area and pore volume of the parent activated fly ash sample. Under Task 3 'Capture of CO{sub 2} by fly ash derived sorbents', sample FAS-10 and its deashed counterpart before and after impregnation of chemical PEI were used for the CO{sub 2} adsorption at different temperatures. The sample FAS-10 exhibited a CO{sub 2} adsorption capacity of 17.5mg/g at 30 C, and decreases to 10.25mg/g at 75 C, while those for de-ashed counterpart are 43.5mg/g and 22.0 mg/g at 30 C and 75 C, respectively. After loading PEI, the CO{sub 2} adsorption capacity increased to 93.6 mg/g at 75 C for de-ashed sample and 62.1 mg/g at 75 C for raw fly ash sample. The activated fly ash, FAS-4, and its chemical loaded counterparts were tested for CO{sub 2} capture capacity. The activated carbon exhibited a CO{sub 2} adsorption capacity of 40.3mg/g at 30 C that decreased to 18.5mg/g at 70 C and 7.7mg/g at 120 C. The CO{sub 2} adsorption capacity profiles changed significantly after impregnation. For the MEA loaded sample the capacity increased to 68.6mg/g at 30 C. The loading of MDEA and DEA initially decreased the CO{sub 2} adsorption capacity at 30 C compared to the parent sample but increased to 40.6 and 37.1mg/g, respectively, when the temperature increased to 70 C. The loading of AMP decrease the CO{sub 2} adsorption capacity compared to the parent sample under all the studied temperatures. Under Task 4 'Comparison of the CO{sub 2} capture by fly ash derived sorbents with commercial sorbents', the CO{sub 2} adsorption capacities of selected activated fly ash carbons were compared to commercial activated carbons. The CO{sub 2} adsorption capacity of fly ash derived activated carbon, FAS-4, and its chemical loaded counterpart presented CO{sub 2} capture capacities close to 7 wt%, which are comparable to, and even better than, the published values of 3-4%.« less

Stable carbon isotope ratio in atmospheric CO2 collected by new diffusive devices.

PubMed

Proto, Antonio; Cucciniello, Raffaele; Rossi, Federico; Motta, Oriana

2014-02-01

In this paper, stable carbon isotope ratios (δ (13)C) were determined in the atmosphere by using a Ca-based sorbent, CaO/Ca12Al14O33 75:25 w/w, for passively collecting atmospheric CO2, in both field and laboratory experiments. Field measurements were conducted in three environments characterized by different carbon dioxide sources. In particular, the environments under consideration were a rather heavily trafficked road, where the source of CO2 is mostly vehicle exhaust, a rural unpolluted area, and a private kitchen where the major source of CO2 was gas combustion. Samplers were exposed to the free atmosphere for 3 days in order to allow collection of sufficient CO2 for δ(13)C analysis, then the collected CO2 was desorbed from the adsorbent with acid treatment, and directly analyzed by nondispersive infrared (NDIR) instrument. δ (13)C results confirmed that the samplers collected representative CO2 samples and no fractionation occurred during passive trapping, as also confirmed by an appositely designed experiment conducted in the laboratory. Passive sampling using CaO/Ca12Al14O33 75:25 w/w proved to be an easy and reliable method to collect atmospheric carbon dioxide for δ (13)C analysis in both indoor and outdoor places.

Detecting low levels of radionuclides in fluids

DOEpatents

Patch, Keith D.; Morgan, Dean T.

2000-01-01

An apparatus and method for detecting low levels of one or more radionuclides in a fluid sample uses a substrate that includes an ion exchange resin or other sorbent material to collect the radionuclides. A collecting apparatus includes a collecting chamber that exposes the substrate to a measured amount of the fluid sample such that radionuclides in the fluid sample are collected by the ion exchange resin. A drying apparatus, which can include a drying chamber, then dries the substrate. A measuring apparatus measures emissions from radionuclides collected on the substrate. The substrate is positioned in a measuring chamber proximate to a detector, which provides a signal in response to emissions from the radionuclides. Other analysis methods can be used to detect non-radioactive analytes, which can be collected with other types of sorbent materials.

Characterization and measurement of natural gas trace constituents. Volume 1. Arsenic. Final report, June 1989-October 1993

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chao, S.S.; Attari, A.

1995-01-01

The discovery of arsenic compounds, as alkylarsines, in natural gas prompted this research program to develop reliable measurement techniques needed to assess the efficiency of removal processes for these environmentally sensitive substances. These techniques include sampling, speciation, quantitation and on-line instrumental methods for monitoring the total arsenic concentration. The current program has yielded many products, including calibration standards, arsenic-specific sorbents, sensitive analytical methods and instrumentation. Four laboratory analytical methods have been developed and successfully employed for arsenic determination in natural gas. These methods use GC-AED and GC-MS instruments to speciate alkylarsines, and peroxydisulfate extraction with FIAS, special carbon sorbent withmore » XRF and an IGT developed sorbent with GFAA for total arsenic measurement.« less

Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

PubMed

Sajid, Muhammad; Basheer, Chanbasha

2016-07-15

In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Quantitative determination of n-propane, iso-butane, and n-butane by headspace GC-MS in intoxications by inhalation of lighter fluid.

PubMed

Bouche, Marie-Paule L A; Lambert, Willy E; Van Bocxlaer, Jan F P; Piette, Michel H; De Leenheer, André P

2002-01-01

This report describes a fully elaborated and validated method for quantitation of the hydrocarbons n-propane, iso-butane, and n-butane in blood samples. The newly developed analytical procedure is suitable for both emergency cases and forensic medicine investigations. Its practical applicability is illustrated with a forensic blood sample after acute inhalative intoxication with lighter fluid; case history and toxicological findings are included. Identification and quantitation of the analytes were performed using static headspace extraction combined with gas chromatography-mass spectrometry. In order to reconcile the large gas volumes injected (0.5 mL) with the narrowbore capillary column and thus achieve preconcentration, cold trapping on a Tenax sorbent followed by flash desorption was applied. Adequate retention and separation were achieved isothermally at 35 degrees C on a thick-film capillary column. Sample preparation was kept to a strict minimum and involved simply adding 2.5 microL of a liquid solution of 1,1,2-trichlorotrifluoroethane in t-butyl-methylether as an internal standard to aliquots of blood in a capped vial. Standards were created by volumetric dilution departing from a gravimetrically prepared calibration gas mixture composed of 0.3% of n-propane, 0.7% of iso-butane, and 0.8% of n-butane in nitrogen. In the forensic blood sample, the following concentrations were measured: 90.0 microg/L for n-propane, 246 microg/L for iso-butane, and 846 microg/L for n-butane.

40 CFR 1065.1107 - Sample media and sample system preparation; sample system assembly.

Code of Federal Regulations, 2014 CFR

2014-07-01

...) For capturing PM, we recommend using pure quartz filters with no binder. Select the filter diameter to minimize filter change intervals, accounting for the expected PM emission rate, sample flow rate, and... filter without replacing the sorbent or otherwise disassembling the batch sampler. In those cases...

A STRINGENT COMPARISON OF SAMPLING AND ANALYSIS METHODS FOR VOCS IN AMBIENT AIR

EPA Science Inventory

A carefully designed study was conducted during the summer of 1998 to simultaneously collect samples of ambient air by canisters and compare the analysis results to direct sorbent preconcentration results taken at the time of sample collection. A total of 32 1-h sample sets we...

Modified surface based on magnetic nanocomposite of dithiooxamide/Fe3O4 as a sorbent for preconcentration and determination of trace amounts of copper

NASA Astrophysics Data System (ADS)

Mirabi, Ali; Shokuhi Rad, Ali; Khodadad, Hadiseh

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-1 with detection limit of 0.2 ng ml-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.

Boron nitride nanotubes as novel sorbent for solid-phase microextraction of polycyclic aromatic hydrocarbons in environmental water samples.

PubMed

Fu, Meizhen; Xing, Hanzhu; Chen, Xiangfeng; Zhao, Rusong; Zhi, Chunyi; Wu, Chiman Lawrence

2014-09-01

Boron nitride nanotube (BNNT) is a novel material that shows potential ability in capturing organic pollutants. In this study, BNNTs fixed on a stainless steel fiber by a sol-gel technique were used as sorbent for solid-phase microextraction. Five polycyclic aromatic hydrocarbons with different numbers of aromatic rings were selected as target analysts. Gas chromatography coupled with tandem mass spectrometry was used for detection and quantitative determination. Under optimized conditions, the experimental results show a wide range of linearity (1 to 1,000 ng L(-1)), less than 10.1 % repeatability of relative standard deviation, and low detection limits (0.08 to 0.39 ng L(-1)). In addition, the fabricated fiber offered good thermal and chemical stability. The proposed method was successfully applied for the analysis of real water samples, and satisfactory results were obtained with relative recoveries ranging from 80.2 to 116.8 %. The results demonstrated that BNNTs could be used as sorbent for the analysis of environmental pollutants at trace levels.

Synthesis of a novel molecularly imprinted organic-inorganic hybrid polymer for the selective isolation and determination of fluoroquinolones in tilapia.

PubMed

Yang, Xun; Wang, Ruiling; Wang, Weihua; Yan, Hongyuan; Qiu, Mande; Song, Yanxue

2014-01-15

A novel molecularly imprinted organic-inorganic hybrid polymer (MI-MAA/APTS) based on a dummy molecular imprinting technique and an organic-inorganic hybrid material technique was synthesised and used as a sorbent in solid-phase extraction for the selective isolation and determination of ofloxacin (OFL), lomefloxacin (LOM), and ciprofloxacin (CIP) in tilapia samples. The MI-MAA/APTS sorbent was prepared from 3-aminopropyltriethoxysilanes (APTS) as an inorganic source and methacrylic acid (MAA) as an organic source and exhibited high mechanical strength and special affinities to the analytes. A comparison of MI-MAA/APTS with other conventional sorbents (C18 and HLB) showed that MI-MAA/APTS displayed good selectivity and affinity for OFL, LOM, and CIP, and the recoveries of the analytes at three spiked levels were in the range of 85.1-101.0%, with the relative standard deviations ≤5.1%. The presented MI-MAA/APTS-SPE-HPLC method could be potentially applied to the determination of fluoroquinolones (FQs) in complex fish samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Ionic liquids in solid-phase microextraction: a review.

PubMed

Ho, Tien D; Canestraro, Anthony J; Anderson, Jared L

2011-06-10

Solid-phase microextraction (SPME) has undergone a surge in popularity within the field of analytical chemistry in the past two decades since its introduction. Owing to its nature of extraction, SPME has become widely known as a quick and cost-effective sample preparation technique. Although SPME has demonstrated extraordinary versatility in sampling capabilities, the technique continues to experience a tremendous growth in innovation. Presently, increasing efforts have been directed towards the engineering of novel sorbent material in order to expand the applicability of SPME for a wider range of analytes and matrices. This review highlights the application of ionic liquids (ILs) and polymeric ionic liquids (PILs) as innovative sorbent materials for SPME. Characterized by their unique physico-chemical properties, these compounds can be structurally-designed to selectively extract target analytes based on unique molecular interactions. To examine the advantages of IL and PIL-based sorbent coatings in SPME, the field is reviewed by gathering available experimental data and exploring the sensitivity, linear calibration range, as well as detection limits for a variety of target analytes in the methods that have been developed. Copyright © 2011 Elsevier B.V. All rights reserved.

Development of magnetic graphene @hydrophilic polydopamine for the enrichment and analysis of phthalates in environmental water samples.

PubMed

Wang, Xianying; Song, Guoxin; Deng, Chunhui

2015-01-01

Magnetic graphene @hydrophilic polydopamine composites were successfully fabricated via a simple solvothermal reaction and self-polymerization of dopamine. Benefit from the excellent characteristics of strong magnetic responsivity, super-hydrophilicity and abundant π-electron system, the prepared material showed great potential as a magnetic solid phase extraction (MSPE) sorbent. In this work, six kinds of phthalates (PAEs) were selected as the target analytes to evaluate the extraction ability of the adsorbents combined with MSPE-GC-MS. And various extraction parameters were optimized by selecting the pH value of samples, the amount of sorbents, adsorption and desorption time, the type and volume of eluting solution. Meanwhile, the whole extraction process could be finished in 30 min. Under the optimized conditions, validations of the method were evaluated as well. And the results presented excellent linearity with a wide range of 50-20,000 μg/L (R(2)>0.9991). The detection of limits were in the range from 0.05-5 μg/L (S/N=3). Therefore, the novel magnetic graphene@polydopamine composites were successfully used as the sorbents for the enrichment and analysis of PAEs in real water samples. This proposed method provided a simple, efficient and sensitive approach for the determination of aromatic compounds in real environmental samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Combination of sorption properties of polydimethylsiloxane and solid-phase extraction sorbents in a single composite material for the passive sampling of polar and apolar pesticides in water.

PubMed

Martin, Alexis; Margoum, Christelle; Coquery, Marina; Randon, Jérôme

2016-10-01

Passive sampling techniques have been developed as an alternative method for in situ integrative monitoring of trace levels of neutral pesticides in environmental waters. The objective of this work was to develop a new receiving phase for pesticides with a wide range of polarities in a single step. We describe the development of three new composite silicone rubbers, combining polydimethylsiloxane mechanical and sorption properties with solid-phase extraction sorbents, prepared as a receiving phase for passive sampling. A composite silicone rubber composed of polydimethylsiloxane/poly(divinylbenzene-co-N-vinylpyrrolidone) was selected by batch experiments for its high sorption properties for pesticides with octanol-water partition coefficients ranging from 2.3 to 5.5. We named this composite material "Polar/Apolar Composite Silicone Rubber". A structural study by scanning electron microscopy confirmed the homogeneous dispersion of the sorbent particles and the encapsulation of particles within the polydimethylsiloxane matrix. We also demonstrate that this composite material is resistant to common solvents used for the back-extraction of analytes and has a maximal resistance temperature of 350°C. Therefore, the characteristics of the "Polar/Apolar Composite Silicone Rubber" meet most of the criteria for use as a receiving phase for the passive sampling of pesticides. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of toxic compounds from saliva by magnetic-stirring-assisted micro-solid-phase extraction step followed by headspace-gas chromatography-ion mobility spectrometry.

PubMed

Criado-García, Laura; Arce, Lourdes

2016-09-01

A new sample extraction procedure based on micro-solid-phase extraction (μSPE) using a mixture of sorbents of different polarities (polymeric reversed-phase sorbent HLB, silica-based sorbent C18, and multiwalled carbon nanotubes) was applied to extract benzene, toluene, butyraldehyde, benzaldehyde, and tolualdehyde present in saliva to avoid interference from moisture and matrix components and enhance sensitivity and selectivity of the ion mobility spectrometry (IMS) methodology proposed. The extraction of target analytes from saliva samples by using μSPE were followed by the desorption step carried out in the headspace vials placed in the autosampler of the IMS device. Then, 200 μL of headspace was injected into the GC column coupled to the IMS for its analysis. The method was fully validated in terms of sensitivity, precision, and recovery. The LODs and LOQs obtained, when analytes were dissolved in saliva samples to consider the matrix effect, were within the range of 0.38-0.49 and 1.26-1.66 μg mL(-1), respectively. The relative standard deviations were <3.5 % for retention time and drift time values, which indicate that the method proposed can be applied to determine toxic compounds in saliva samples. Graphical abstract Summary of steps followed in the experimental set up of this work.

Direct Zinc Determination in Brazilian Sugar Cane Spirit by Solid-Phase Extraction Using Moringa oleifera Husks in a Flow System with Detection by FAAS.

PubMed

Alves, Vanessa N; Borges, Simone S O; Coelho, Nivia M M

2011-01-01

This paper reports a method for the determination of zinc in Brazilian sugar cane spirit, (cachaça in Portuguese), using solid-phase extraction with a flow injection analysis system and detection by FAAS. The sorbent material used was activated carbon obtained from Moringa oleifera husks. Flow and chemical variables of the proposed system were optimized through multivariate designs. The factors selected were sorbent mass, sample pH, sample flow rate, and eluent concentration. The optimum extraction conditions were obtained using a sample pH of 4.0, a sample flow rate of 6.0 mL min(-1), 30.0 mg of sorbent mass, and 1.0 mol L(-1) HNO(3) as the eluent at a flow rate of 4.0 mL min(-1). The limit of detection for zinc was 1.9 μg L(-1), and the precision was below 0.82% (20.0 μg L(-1), n = 7). The analytical curve was linear from 2 to 50 μg L(-1), with a correlation coefficient of 0.9996. The method developed was successfully applied to spiked Brazilian sugar cane spirit, and accuracy was assessed through recovery tests, with results ranging from 83% to 100%.

Direct Zinc Determination in Brazilian Sugar Cane Spirit by Solid-Phase Extraction Using Moringa oleifera Husks in a Flow System with Detection by FAAS

PubMed Central

Alves, Vanessa N.; Borges, Simone S. O.; Coelho, Nivia M. M.

2011-01-01

This paper reports a method for the determination of zinc in Brazilian sugar cane spirit, (cachaça in Portuguese), using solid-phase extraction with a flow injection analysis system and detection by FAAS. The sorbent material used was activated carbon obtained from Moringa oleifera husks. Flow and chemical variables of the proposed system were optimized through multivariate designs. The factors selected were sorbent mass, sample pH, sample flow rate, and eluent concentration. The optimum extraction conditions were obtained using a sample pH of 4.0, a sample flow rate of 6.0 mL min−1, 30.0 mg of sorbent mass, and 1.0 mol L−1 HNO3 as the eluent at a flow rate of 4.0 mL min−1. The limit of detection for zinc was 1.9 μg L−1, and the precision was below 0.82% (20.0 μg L−1, n = 7). The analytical curve was linear from 2 to 50 μg L−1, with a correlation coefficient of 0.9996. The method developed was successfully applied to spiked Brazilian sugar cane spirit, and accuracy was assessed through recovery tests, with results ranging from 83% to 100%. PMID:21785595

Evaluation of polyethersulfone performance for the microextraction of polar chlorinated herbicides from environmental water samples.

PubMed

Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Cela, Rafael; Möder, Monika; Rodríguez, Isaac

2014-05-01

In this work, the suitability of bulk polyethersulfone (PES) for sorptive microextraction of eight polar, chlorinated phenoxy acids and dicamba from environmental water samples is assessed and the analytical features of the optimized method are compared to those reported for other microextraction techniques. Under optimized conditions, extractions were performed with samples (18 mL) adjusted at pH 2 and containing a 30% (w/v) of sodium chloride, using a tubular PES sorbent (1 cm length × 0.7 mm o.d., sorbent volume 8 µL). Equilibrium conditions were achieved after 3h of direct sampling, with absolute extraction efficiencies ranging from 39 to 66%, depending on the compound. Analytes were recovered soaking the polymer with 0.1 mL of ethyl acetate, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). Achieved quantification limits (LOQs) varied between 0.005 and 0.073 ng mL(-1). After normalization with the internal surrogate (IS), the efficiency of the extraction was only moderately affected by the particular characteristics of different water samples (surface and sewage water); thus, pseudo-external calibration, using spiked ultrapure water solutions, can be used as quantification technique. The reduced cost of the PES polymer allowed considering it as a disposable sorbent, avoiding variations in the performance of the extraction due to cross-contamination problems and/or surface modification with usage. Copyright © 2014 Elsevier B.V. All rights reserved.

Matrix-compatible sorbent coatings based on structurally-tuned polymeric ionic liquids for the determination of acrylamide in brewed coffee and coffee powder using solid-phase microextraction.

PubMed

Cagliero, Cecilia; Nan, He; Bicchi, Carlo; Anderson, Jared L

2016-08-12

Nine crosslinked polymeric ionic liquid (PIL)-based SPME sorbent coatings were designed and screened in this study for the trace level determination of acrylamide in brewed coffee and coffee powder using gas chromatography-mass spectrometry (GC-MS). The structure of the ionic liquid (IL) monomer was tailored by introducing different functional groups to the cation and the nature of the IL crosslinker was designed by altering both the structure of the cation as well as counteranions. The extraction efficiency of the new PIL coatings towards acrylamide was investigated and compared to a previously reported PIL sorbent coating. All PIL fibers exhibited excellent analytical precision and linearity. The PIL fiber coating consisting of 50% 1,12-di(3-vinylbenzylbenzimidazolium)dodecane dibis[(trifluoromethyl)sulfonyl]imide as IL crosslinker in 1-vinyl-3-(10-hydroxydecyl)imidazolium bis[(trifluoromethyl)sulfonyl]imide IL monomer resulted in a limit of quantitation of 0.5μgL(-1) with in-solution SPME sampling. The hydroxyl moiety appended to the IL cation was observed to significantly increase the sensitivity of the PIL coating toward acrylamide. The quantitation of acrylamide in brewed coffee and coffee powder was performed using the different PIL-based fibers by the method of standard addition after a quenching reaction using ninhydrin to inhibit the formation of interfering acrylamide in the GC inlet, mainly by asparagine thermal degradation. Excellent repeatability with relative standard deviations below 10% were obtained on the real coffee samples and the structure of the coatings appeared intact by scanning electron microscopy after coffee sampling proving the matrix-compatibility of the PIL sorbent coatings. Copyright © 2016 Elsevier B.V. All rights reserved.

Ultrasound assisted extraction of Maxilon Red GRL dye from water samples using cobalt ferrite nanoparticles loaded on activated carbon as sorbent: Optimization and modeling.

PubMed

Mehrabi, Fatemeh; Vafaei, Azam; Ghaedi, Mehrorang; Ghaedi, Abdol Mohammad; Alipanahpour Dil, Ebrahim; Asfaram, Arash

2017-09-01

In this research, a selective, simple and rapid ultrasound assisted dispersive solid-phase micro-microextraction (UA-DSPME) was developed using cobalt ferrite nanoparticles loaded on activated carbon (CoFe 2 O 4 -NPs-AC) as an efficient sorbent for the preconcentration and determination of Maxilon Red GRL (MR-GRL) dye. The properties of sorbent are characterized by X-ray diffraction (XRD), Transmission Electron Microscopy (TEM), Vibrating sample magnetometers (VSM), Fourier transform infrared spectroscopy (FTIR), Particle size distribution (PSD) and Scanning Electron Microscope (SEM) techniques. The factors affecting on the determination of MR-GRL dye were investigated and optimized by central composite design (CCD) and artificial neural networks based on genetic algorithm (ANN-GA). CCD and ANN-GA were used for optimization. Using ANN-GA, optimum conditions were set at 6.70, 1.2mg, 5.5min and 174μL for pH, sorbent amount, sonication time and volume of eluent, respectively. Under the optimized conditions obtained from ANN-GA, the method exhibited a linear dynamic range of 30-3000ngmL -1 with a detection limit of 5.70ngmL -1 . The preconcentration factor and enrichment factor were 57.47 and 93.54, respectively with relative standard deviations (RSDs) less than 4.0% (N=6). The interference effect of some ions and dyes was also investigated and the results show a good selectivity for this method. Finally, the method was successfully applied to the preconcentration and determination of Maxilon Red GRL in water and wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Miniaturized solid-phase extraction of macrolide antibiotics in honey and bovine milk using mesoporous MCM-41 silica as sorbent.

PubMed

Du, Li-Jing; Yi, Ling; Ye, Li-Hong; Chen, Yu-Bo; Cao, Jun; Peng, Li-Qing; Shi, Yu-Ting; Wang, Qiu-Yan; Hu, Yu-Han

2018-02-16

A simple and effective method of miniaturized solid-phase extraction (mini-SPE) was developed for the simultaneous purification and enrichment of macrolide antibiotics (MACs) (i.e. azithromycin, clarithromycin, erythromycin, lincomycin and roxithromycin) from honey and skim milk. Mesoporous MCM-41 silica was synthesized and used as sorbent in mini-SPE. Several key parameters affecting the performance of mini-SPE procedure were thoroughly investigated, including sorbent materials, amount of sorbent and elution solvents. Under the optimized condition, satisfactory linearity (r 2  > 0.99), acceptable precision (RSDs, 0.3-7.1%), high sensitivity (limit of detection in the range of 0.01-0.76 μg/kg), and good recoveries (83.21-105.34%) were obtained. With distinct advantages of simplicity, reliability and minimal sample requirement, the proposed mini-SPE procedure coupled with ultrahigh performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry could become an alternative tool to analyze the residues of MACs in complex food matrixes. Copyright © 2018 Elsevier B.V. All rights reserved.

Barium alginate caged Fe3O4@C18 magnetic nanoparticles for the pre-concentration of polycyclic aromatic hydrocarbons and phthalate esters from environmental water samples.

PubMed

Zhang, Shengxiao; Niu, Hongyun; Cai, Yaqi; Shi, Yali

2010-04-30

The hydrophobic octadecyl (C(18)) functionalized Fe(3)O(4) magnetic nanoparticles (Fe(3)O(4)@C(18)) were caged into hydrophilic barium alginate (Ba(2+)-ALG) polymers to obtain a novel type of solid-phase extraction (SPE) sorbents, and the sorbents were applied to the pre-concentration of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs) pollutants from environmental water samples. The hydrophilicity of the Ba(2+)-ALG cage enhances the dispersibility of sorbents in water samples, and the superparamagnetism of the Fe(3)O(4) core facilitates magnetic separation. With the magnetic SPE technique based on the Fe(3)O(4)@C(18)@Ba(2+)-ALG sorbents, it requires only 30 min to extract trace levels of analytes from 500 mL water samples. After the eluate is condensed to 0.5 mL, concentration factors for both phenanthrene and di-n-propyl-phthalate are over 500, while for other analytes are about 1000. The recoveries of target compounds are independent of salinity and solution pH under testing conditions. Under optimized conditions, the detection limits for phenanthrene, pyrene, benzo[a]anthracene, and benzo[a]pyrene are 5, 5, 3, and 2 ng L(-1), and for di-n-propyl-phthalate, di-n-butyl-phthalate, di-cyclohexyl-phthalate, and di-n-octyl-phthalate are 36, 59, 19, and 36 ng L(-1), respectively. The spiked recoveries of several real water samples for PAHs and PAEs are in the range of 72-108% with relative standard deviations varying from 1% to 9%, showing good accuracy of the method. The advantages of the new SPE method include high extraction efficiency, short analysis time and convenient extraction procedure. To the best of our knowledge, it is unprecedented that hydrophilic Ba(2+)-ALG polymer caged Fe(3)O(4)@C(18) magnetic nanomaterial is used to extract organic pollutants from large volumes of water samples. Copyright 2010 Elsevier B.V. All rights reserved.

Cyclodextrin based polymer sorbents for micro-solid phase extraction followed by liquid chromatography tandem mass spectrometry in determination of endogenous steroids.

PubMed

Manaf, Normaliza Abdul; Saad, Bahruddin; Mohamed, Mohamed H; Wilson, Lee D; Latiff, Aishah A

2018-03-30

Sorbents were prepared by cross-linking β-cyclodextrin (β-CD) using two different types of cross-linker units at variable reactant mole ratios. The resulting polymers containing β-CD were evaluated as sorbents in micro-solid phase extraction (μ-SPE) format for the extraction of the endogenous steroids testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5α-androstane-3α,17β-diol (5αAdiol) and 5β-androstane-3α,17β-diol (5βAdiol). The best sorbent (C1; cyclodextrin polymer) showed superior extraction characteristics compared with commercial sorbents (C18 and Bond Elut Plexa). Parameters influencing the extraction efficiency of the C1 sorbent such as extraction and desorption times, desorption solvent and volume of sample were investigated. The extracts were separated using a Hypersil Gold column (50 × 2.1 mm, 1.9 μm) under gradient elution coupled to a LC-MS/MS. The compounds were successfully separated within 8 min. The method offers good repeatability (RSD < 10%) and linearity (r 2  > 0.995) were within the range of 1-200 ng mL -1 for T and E, 250-4000 ng mL -1 for A and Etio and 25-500 ng mL -1 for 5αAdiol and 5βAdiol, respectively. The method was applied for the determination of steroid profile of urine from volunteers. Copyright © 2018 Elsevier B.V. All rights reserved.

Kinetic and thermodynamic studies of the Co(II) and Ni(II) ions removal from aqueous solutions by Ca-Mg phosphates.

PubMed

Ivanets, A I; Srivastava, V; Kitikova, N V; Shashkova, I L; Sillanpää, M

2017-03-01

The aim of this work was to study the sorption kinetics and thermodynamics of Co(II) and Ni(II) from aqueous solutions by sorbents on the basis of hydrogen (PD-1) and tertiary (PD-2) Ca-Mg phosphates depending on the solution temperature and sorbents chemical composition. Kinetic studies of adsorption of Co(II) and Ni(II) ions onto samples of phosphate sorbents were performed in batch experiment at the temperatures 288, 303, 318 and 333 K. The sorbent dose was fixed at 10 g L -1 , initial pH value 2.6, and contact time varied from 5 to 600 min. The kinetics of Co(II) and Ni(II) adsorption were analyzed by using pseudo-first order, pseudo-second order and intraparticle diffusion models. Thermodynamic parameters (ΔG°, ΔH° and ΔS°) for the sorption of Co(II) and Ni(II) were determined using the Gibbs-Helmholtz equation. The calculated kinetic parameters and corresponding correlation coefficients revealed that Co(II) and Ni(II) uptake process followed the pseudo-second order rate expression. Thermodynamic studies confirmed the spontaneous and endothermic nature of removal process which indicate that sorption of Co(II) and Ni(II) ions onto both phosphate sorbents is favoured at higher temperatures and has the chemisorptive mechanism. The data thus obtained would be useful for practical application of the low cost and highly effective Ca-Mg phosphate sorbents. Copyright © 2016 Elsevier Ltd. All rights reserved.

Gas chromatographic detection of some nitro explosive compounds in soil samples after solid-phase microextraction with carbon ceramic copper nanoparticle fibers.

PubMed

Farhadi, Khalil; Bochani, Shayesteh; Hatami, Mehdi; Molaei, Rahim; Pirkharrati, Hossein

2014-07-01

In this research, a new solid-phase microextraction fiber based on carbon ceramic composites with copper nanoparticles followed by gas chromatography with flame ionization detection was applied for the extraction and determination of some nitro explosive compounds in soil samples. The proposed method provides an overview of trends related to synthesis of solid-phase microextraction sorbents and their applications in preconcentration and determination of nitro explosives. The sorbents were prepared by mixing of copper nanoparticles with a ceramic composite produced by mixture of methyltrimethoxysilane, graphite, methanol, and hydrochloric acid. The prepared sorbents were coated on copper wires by dip-coating method. The prepared nanocomposites were evaluated statistically and provided better limits of detection than the pure carbon ceramic. The limit of detection of the proposed method was 0.6 μg/g with a linear response over the concentration range of 2-160 μg/g and square of correlation coefficient >0.992. The new proposed fiber has been demonstrated to be a suitable, inexpensive, and sensitive candidate for extraction of nitro explosive compounds in contaminated soil samples. The constructed fiber can be used more than 100 times without the need for surface generation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A robust, simple, high-throughput technique for time-resolved plant volatile analysis in field experiments

PubMed Central

Kallenbach, Mario; Oh, Youngjoo; Eilers, Elisabeth J.; Veit, Daniel; Baldwin, Ian T.; Schuman, Meredith C.

2014-01-01

Summary Plant volatiles (PVs) mediate interactions between plants and arthropods, microbes, and other plants, and are involved in responses to abiotic stress. PV emissions are therefore influenced by many environmental factors, including herbivore damage, microbial invasion, and cues from neighboring plants, but also light regime, temperature, humidity, and nutrient availability. Thus an understanding of the physiological and ecological functions of PVs must be grounded in measurements reflecting PV emissions under natural conditions. However, PVs are usually sampled in the artificial environments of laboratories or climate chambers. Sampling of PVs in natural environments is difficult, limited by the need to transport, maintain, and power instruments, or use expensive sorbent devices in replicate. Ideally, PVs should be measured in natural settings with high replication, spatiotemporal resolution, and sensitivity, and at modest costs. Polydimethysiloxane (PDMS), a sorbent commonly used for PV sampling, is available as silicone tubing (ST) for as little as 0.60 €/m (versus 100-550 € apiece for standard PDMS sorbent devices). Small (mm-cm) ST pieces (STs) can be placed in any environment and used for headspace sampling with little manipulation of the organism or headspace. STs have sufficiently fast absorption kinetics and large capacity to sample plant headspaces on a timescale of minutes to hours, and thus can produce biologically meaningful “snapshots” of PV blends. When combined with thermal desorption (TD)-GC-MS analysis – a 40-year-old and widely available technology – STs yield reproducible, sensitive, spatiotemporally resolved, quantitative data from headspace samples taken in natural environments. PMID:24684685

Application of NaClO-treated multiwalled carbon nanotubes as solid phase extraction sorbents for preconcentration of trace 2,4-dichlorophenoxyacetic acid in aqueous samples.

PubMed

Lu, Ping; Deng, Dayi; Ni, Xiaodan

2012-09-01

Multiwalled carbon nanotubes functionalized by oxidation of original multiwalled carbon nanotubes with NaClO were prepared and their application as solid phase extraction sorbent for 2,4-dichlorophenoxyacetic acid (2,4-D) was investigated systemically, and a new method was developed for the determination of trace 2,4-D in water samples based on extraction and preconcentration of 2,4-D with solid phase extraction columns packed with NaClO-treated multiwalled carbon nanotubes prior to its determination by HPLC. The optimum experimental parameters for preconcentration of 2,4-D, including the column activating conditions, the amount of the sorbent, pH of the sample, elution composition, and elution volume, were investigated. The results indicated 2,4-D could be quantitatively retained by 100 mg NaClO-treated multiwalled carbon nanotubes at pH 5, and then eluted completely with 10 mL 3:1 (v/v) methanol-ammonium acetate solution (0.3 mol/L). The detection limit of this method for 2,4-D was 0.15 μg/L, and the relative standard deviation was 2.3% for fortified tap water samples and 2.5% for fortified riverine water sample at the 10 μg/L level. The method was validated using fortified tap water and riverine water samples with known amount of 2,4-D at the 0.4, 10, and 30 μg/L levels, respectively. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Potential of sawdust as a green and economical sorbent for simultaneous preconcentration of trace amounts of cadmium, cobalt, and lead from water, biological, food, and herbal samples.

PubMed

Baki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

2013-05-01

Application of treated sawdust with NaOH as a green and economical sorbent for simultaneous preconcentration of trace amounts of Cd(II), Co(II), and Pb(II) ions from liver, lettuce, fish, and water as test samples with complicated matrices was investigated. Various parameters, such as effect of pH and contact time, breakthrough volume, type, and concentration of eluent and interference of ions were studied. The sorption was quantitative in the pH of 5.0 to 7.0 and desorption occurred instantaneously with 5.0 mL of mixed solutions of ethanol and 2.0 mol/L HNO3 -HCl and the amount of ions was measured by using flame atomic absorption spectrometry. Linearity was maintained at 3 to 500 μg/L for cobalt, 5.0 to 800 μg/L for lead, and 2.0 to 300 μg/L for cadmium in the original solution. The relative standard deviation was less than 1.80% (n = 6, with concentration of 0.3 mg/L for cadmium and 0.5 mg/L for lead and cobalt). Detection limits and maximum capacity of the sorbent for Co (II), Cd (II), and Pb (II) in the original solution were 0.86, 0.50, and 1.7 μg/L and 28.5, 30.6, and 47.3 mg/g, respectively. The results for spiked real samples, effect of interfering ions, and adsorption capacity indicated that the applicability of this method for lead preconcentration is better than cadmium and cobalt preconcentration from complicated matrices. Practical Application: Sawdust can be applied as a green and economical sorbent for simultaneous preconcentration and solid-phase extraction of metal ions from food and environmental samples with complicated matrices. © 2013 Institute of Food Technologists®

A comparison of three macroinvertebrate sampling devices for use in conducting rapid-assessment procedures of Delmarva Peninsula wetlands

USGS Publications Warehouse

Lowe, Terrence (Peter); Tebbs, Kerry; Sparling, Donald W.

2016-01-01

Three types of macroinvertebrate collecting devices, Gerking box traps, D-shaped sweep nets, and activity traps, have commonly been used to sample macroinvertebrates when conducting rapid biological assessments of North American wetlands. We compared collections of macroinvertebrates identified to the family level made with these devices in 6 constructed and 2 natural wetlands on the Delmarva Peninsula of Maryland. We also assessed their potential efficacy in comparisons among wetlands using several proportional and richness attributes. Differences in median diversity among samples from the 3 devices were significant; the sweep-net samples had the greatest diversity and the activity-trap samples had the least diversity. Differences in median abundance were not significant between the Gerking box-trap samples and sweep-net samples, but median abundance among activity-trap samples was significantly lower than among samples of the other 2 devices. Within samples, the proportions of median diversity composed of major class and order groupings were similar among the 3 devices. However the proportions of median abundance composed of the major class and order groupings within activity-trap samples were not similar to those of the other 2 devices. There was a slight but significant increase in the total number of families captured when we combined activity-trap samples with Gerking box-trap samples or with sweep-net samples, and the per-sample median numbers of families of the combined activity-trap and sweep-net samples was significantly higher than that of the combined activity-trap and Gerking box-trap samples. We detected significant differences among wetlands for 4 macroinvertebrate attributes with the Gerking box-trap data, 6 attributes with sweep-net data, and 5 attributes with the activity-trap data. A small, but significant increase in the number of attributes showing differences among wetlands occurred when we combined activity-trap samples with those of the Gerking boxtrap or sweep net.

Inexpensive, effective novel activated carbon fibers for sample cleanup: application to multipesticide residue analysis in food commodities using a QuEChERS method.

PubMed

Singh, Shiv; Srivastava, Anshuman; Singh, Sheelendra Pratap

2018-03-01

Phenolic resin based activated carbon fibers (ACFs) were applied for the first time as a reversed-dispersive solid-phase extraction (r-DSPE) sorbent. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was applied to determine 26 pesticides (organophosphates, organochlorines, synthetic pyrethroids, and herbicides) in different complex matrices, including cauliflower, cucumber, banana, apple, wheat, and black gram. Different physicochemical characterization techniques were used to investigate the engineering and structural properties of the r-DSPE sorbent. All the chromatographic analyses were performed with a gas chromatograph equipped with an electron capture detector. The recoveries of all 26 pesticides were acceptable (70-120%), with relative standard deviations of less than 15%. The limit of detection and the limit of quantification were 1.13-5.48 ng/g and 3.42-16.60 ng/g, respectively. In the original QuEChERS method, primary secondary amine is extensively used as the r-DSPE sorbent in the cleanup process, but it is eightfold more expensive than the ACFs used in this study. Therefore, the modified QuEChERS method using ACFs during the cleanup process is more efficient, cheaper, and more robust to determine pesticides from different types of matrices, including vegetables, grains, and fruits, and ACFs could be used as a cost-effective alternative to primary secondary amine. Graphical Abstract Sample clean-up using PSA and ACF as r-DSPE sorbent in QuEChERS method.

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.

PubMed

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) (4.2-26.3 ng L -1 ) for environmentally important analytes including polycyclic aromatic hydrocarbons, ketones and aliphatic hydrocarbons. In CME-GC experiments (n = 5), the capillary-to-capillary RSD value was ∼2.1%; such a low RSD value is indicative of excellent reproducibility of the sol-gel method used for the preparation of these CME coatings. The dual-ligand sol-gel coating provided stable performance in capillary microextraction of analytes from saline samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Magnetic sorbents added to soil slurries lower Cr aqueous concentration

NASA Astrophysics Data System (ADS)

Aravantinos, Konstantinos; Isari, Ekavi; Karapanagioti, Hrissi K.; Manariotis, Ioannis D.; Werner, David

2016-04-01

Activated carbon (AC) acts as a strong binding agent that lowers the pollutant concentration and, thus its toxicity. Another promising sorbent material in environmental applications is biochar (BC) which is obtained from the incomplete combustion of carbon-rich biomass under oxygen-limited conditions. Both of these materials could be used as soil or sediment amendments that would lower the toxicity in the aqueous phase. A draw back of this technique is that although the pollutant will remain non- bioavailable for many years being sorbed into these sorbents, it actually stays into the system. The objective of this study was (a) to synthesize a magnetic powdered activated carbon (AC/Fe) and magnetic powdered biochar (BC/Fe) produced from a commercial AC sample and BC, respectively and (b) to evaluate the potential use of AC/Fe and BC/Fe to lower Cr concentration that desorb from two soils in their soil slurries. The two soil samples originate from the vicinity of a local metal shop. The BC was produced from olive pomace. The surface area, the pore volume, and the average pore size of each sorbent were determined using gas (N2) adsorption-desorption cycles and the Brunauer, Emmett, and Teller (BET) equation. Isotherms with 30 adsorption and 20 desorption points were conducted at liquid nitrogen temperature (77K). Open surface area and micropore volume were determined using t-plot method and Harkins & Jura equation. For both AC/Fe, surface area measurements resulted in 66% those of corresponding AC. For BC/Fe, the surface area was 82% that of BC. Our previous studies have shown that both AC/Fe and BC/Fe are effective sorbents for mercury in aqueous solutions but with lower sorption capacity compared to the initial materials (50-75% lower). Batch experiments with all sorbent samples and each soil were conducted at room temperature (25oC) in order to compare the sorption properties of the materials. The soil slurries demonstrated low Cr concentrations (10.9 and 14.6 μg/L, respectively). One month after the addition of amendments AC, AC/Fe, and BC/Fe, Cr concentration in the slurry was lower than the detection limit which was 0.5 μg/L (except of one of the soils with the AC that was 2.1 μg/L). The slurries with BC demonstrated Cr concentrations equal to 4.2 and 7.1 μg/L, respectively. All these properties point to promising materials that can effectively be used for in-situ environmental remediation and also be recovered.

Fixing atmospheric CO2 by environment adaptive sorbent and renewable energy

NASA Astrophysics Data System (ADS)

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 optimization. Chemical reaction kinetics could be enhanced by stronger binding energy or higher temperature. However, the total kinetics can only be significantly improved by chemical reaction enhancement if the physical diffusion is fast enough.

Irreversible sorption of trace concentrations of perfluorocarboxylic acids to fiber filters used for air sampling

NASA Astrophysics Data System (ADS)

Arp, Hans Peter H.; Goss, Kai-Uwe

Due to the apparent environmental omnipresence of perfluorocarboxylic acids (PFAs), an increasing number of researchers are investigating their ambient particle- and gas-phase concentrations. Typically this is done using a high-volume air sampler equipped with Quartz Fiber Filters (QFFs) or Glass Fiber Filters (GFFs) to sample the particle-bound PFAs and downstream sorbents to sample the gas-phase PFAs. This study reports that at trace, ambient concentrations gas-phase PFAs sorb to QFFs and GFFs irreversibly and hardly pass through these filters to the downstream sorbents. As a consequence, it is not possible to distinguish between particle- and gas-phase concentrations, or to distinguish concentrations on different particle size fractions, unless precautions are taken. Failure to take such precautions could have already caused reported data to be misinterpreted. Here it is also reported that deactivating QFFs and GFFs with a silylating agent renders them suitable for sampling PFAs. Based on the presented study, a series of recommendations for air-sampling PFAs are provided.

Sorbents for mercury removal from flue gas

DOE Office of Scientific and Technical Information (OSTI.GOV)

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.

Semiautomated solid-phase extraction followed by derivatisation and gas chromatography–mass spectrometry for determination of perfluoroalkyl acids in water.

PubMed

Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

2013-11-29

This paper describes a sensitive approach for the determination of 6 perfluoroalkyl carboxylic acids and perfluorooctane sulfonic acid in water. Samples were preconcentrated using an automatic solid-phase extraction module and then manually derivatised and determined by gas chromatography–mass spectrometry. The analytes were derivatised with a isobutyl chloroformate/isobutanol mixture, using 3% N,N-dicyclohexylcarbodiimide in pyridine as the catalyst. From a systematic comparison of several reversed-phase and anion-exchange sorbent materials for the retention of perfluoroalkyl acids, the high-est retention efficiencies (∼100%) were achieved with LiChrolut EN and Discovery DSC-SAX columns.LiChrolut EN was the sorbent selected due to several advantages (sample pH ∼1; sample flow rate,5.5 mL/min; breakthrough volume, 300 mL) over Discovery DSC-SAX (sample pH ∼6; sample flow rate,3.0 mL/min; breakthrough volume, 45 mL), for the retention of the studied compounds. Detection and quantification limits within the range of 0.1–0.5 ng/L and 0.4–1.7 ng/L, respectively, were obtained for a sorbent column of 70 mg of LiChrolut EN and 250 mL of sample, the relative standard deviation being lower than 7%. The method was applied both to the analysis of water collected at the intake (raw) and atthe exit (treated) of two drinking water treatment plants, as well as to various types of water. Few samples were positive for perfluoroalkyl acids and only one acid (perfluoroheptanoic or perfluorooctanoic) was found in each treatment plant. The highest number and concentration of analytes (perfluoroheptanoic,perfluorooctanoic and perfluorodecanoic acid) were found in one wastewater.

Testing of nylon 6 nanofibers with different surface densities as sorbents for solid phase extraction and their selectivity comparison with commercial sorbent.

PubMed

Háková, Martina; Raabová, Hedvika; Havlíková, Lucie Chocholoušová; Chocholouš, Petr; Chvojka, Jiří; Šatínský, Dalibor

2018-05-01

Nylon 6 nanofibers were tested for their ability to serve as a sorbent for solid phase extraction (SPE). The regular nanostructure providing a great sorption area and amidic functionality should lead to the assumption that nylon 6 nanofibers could be used as a novel sorbent with great potential for sample pre-treatment. However, due to the substantial differences between classical particle sorbents used for solid phase extraction and nanofibers, it is necessary to evaluate this novel approach. This article describes three types of laboratory fabricated nylon 6 nanofibers with different surface density (5.04gm -2 , 3.90gm -2 and 0.75gm -2 ) and corresponding surface areas for solid phase extraction of several groups of compounds with different structural and physicochemical properties (parabens, steroids, flavonoids and pesticides). The nanofibers were created by needleless electrospinning. Extraction columns were manually packed in classic 1- or 3-mL plastic syringe cartridges with 26-30mg of nanofibers and the column bed was sealed with polypropylene frits. The SPE procedure followed a typical five-step protocol and the collected eluates were analyzed by HPLC with UV detection. Extraction recovery was used as a parameter to evaluate the behavior of the analytes within the SPE process. Under this set condition, the recovery of the SPE process ranged from 23.1% to 125.8%. SPE showed good repeatability (0.58-11.87% RSD) and inter-day reproducibility (3.86-9.79% RSD). The achieved results were compared with SPE using a classic particle sorbent column. Good mechanical and chemical stability of nanofibers was proved. Scanning electron microscope was used for the evaluation of morphological changes in nanostructure. Nylon 6 nanofibers proved being a cost-effective sorbent for repeated use in SPE. Nylon 6 nanofibers have great potential in miniaturized SPE enabling users to overcome troubles with high back-pressure. Copyright © 2018 Elsevier B.V. All rights reserved.

Thermal desorption comprehensive two-dimensional gas chromatography coupled to time of flight mass spectrometry for vapour phase mainstream tobacco smoke analysis.

PubMed

Savareear, Benjamin; Brokl, Michał; Wright, Chris; Focant, Jean-Francois

2017-11-24

A thermal desorption comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (TD-GC×GC-TOFMS) method has been developed for the analysis of mainstream tobacco smoke (MTS) vapour phase (VP). The selection process of the sample introduction approach involved comparing the results obtained from three different approaches: a) use of gas sampling bag followed by SPME (Tedlar ® -SPME), b) gas sampling bag followed by TD (Tedlar ® -TD), and c) sampling directly on TD sorbents (Direct-TD). Six different SPME fibers and six different TD sorbent beds were evaluated for the extraction capacities in terms of total number of peaks and related intensities or peak areas. The best results were obtained for the Direct-TD approach using Tenax TA/Carbograph1TD/Carboxen1003 sorbent tubes. The optimisation of TD tube desorption parameters was carried out using a face-centered central composite experimental design and resulted in the use of the Tenax TA/Carbograph 1TD/Carboxen 1003 sorbent with a 7.5min desorption time, a 60mL/min tube desorption flow, and a 250°C tube desorption temperature. The optimised method was applied to the separation of MTS-VP constituents, with 665 analytes detected. The method precision ranged from 1% to 15% for over 99% of identified peak areas and from 0% to 3% and 0% to 1% for both first ( 1 t R ) and second ( 2 t R ) dimension retention times, respectively. The method was applied to the analyses of two cigarette types differing in their filter construction. Principal component analysis (PCA) allowed a clear differentiation of the studied cigarette types (PC1 describing 94% of the explained variance). Supervised Fisher ratio analysis permitted the identification of compounds responsible for the chemical differences between the two sample types. A set of 91 most relevant compounds was selected by applying a Fisher ratio cut-off approach and most of them were selectively removed by one of the cigarette filter types. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of magnetic dispersive solid phase extraction using toner powder as an efficient and economic sorbent in combination with dispersive liquid-liquid microextraction for extraction of some widely used pesticides in fruit juices.

PubMed

Farajzadeh, Mir Ali; Mohebbi, Ali

2018-01-12

In this study, for the first time, a magnetic dispersive solid phase extraction method using an easy-accessible, cheap, and efficient magnetic sorbent (toner powder) combined with dispersive liquid-liquid microextraction has been developed for the extraction and preconcentration of some widely used pesticides (diazinon, ametryn, chlorpyrifos, penconazole, oxadiazon, diniconazole, and fenazaquin) from fruit juices prior to their determination by gas chromatography-flame ionization detection. In this method, the magnetic sorbent is mixed with an appropriate dispersive solvent (methanol-water, 80:20, v/v) and then injected into an aqueous sample containing the analytes. By this action the analytes are rapidly adsorbed on the sorbent by binding to its carbon. The sorbent particles are isolated from the aqueous solution in the presence of an external magnetic field. Then an appropriate organic solvent (acetone) is used to desorb the analytes from the sorbent. Finally, the obtained supernatant is mixed with an extraction solvent and injected into deionized water in order to achieve high enrichment factors and sensitivity. Several significant factors affecting the performance of the introduced method were investigated and optimized. Under the optimum experimental conditions, the extraction recoveries of the proposed method for the selected analytes ranged from 49-75%. The relative standard deviations were ≤7% for intra- (n = 6) and inter-day (n = 4) precisions at a concentration of 10 μg L -1 of each analyte. The limits of detection were in the range of 0.15-0.36 μg L -1 . Finally, the applicability of the proposed method was evaluated by analysis of the selected analytes in some fruit juices. Copyright © 2017 Elsevier B.V. All rights reserved.

Towards the determination of sulfonamides in meat samples: A magnetic and mesoporous metal-organic framework as an efficient sorbent for magnetic solid phase extraction combined with high-performance liquid chromatography.

PubMed

Xia, Lian; Liu, Lijie; Lv, Xiaoxia; Qu, Fei; Li, Guoliang; You, Jinmao

2017-06-02

A magnetic, mesoporous core/shell structured Fe 3 O 4 @JUC-48 nanocomposite was synthesized and employed as a magnetic solid phase extraction (MSPE) sorbent for the determination of trace sulfonamides (SAs) in meat samples. The synthesized nanocomposite was characterized by X-ray diffraction, Fourier transform infrared spectra, transmission electron microscopy, scanning electron microscopy, Brunner-Emmet-Teller, and vibrating sample magnetometry; the Fe 3 O 4 @JUC-48 nanocomposite exhibited a distinctive morphology, large surface area, high magnetism, open adsorption sites, and high chemical stability. By combining the optimized MSPE conditions with high performance liquid chromatography diode array detection, an accurate and sensitive method for the determination of 5 SAs, including sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMR), sulfamethazine (SMZ), and sulfamethoxypyridazine (SMP), was developed. The method exhibited good linearity in the range of 3.97-1000ng/g with R ranging from 0.9991 to 0.9994, high sensitivity with LODs ranging from 1.73 to 5.23ng/g, adequate recoveries between 76.1 and 102.6% with low relative standard deviations ranging from 2.1 to 6.4%, and high precision with RSD<4.5%. The Fe 3 O 4 @JUC-48 magnetic nanocomposite is a promising sorbent for the rapid and efficient extraction of SAs from complex biological samples such as chicken, pork, and shrimp. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis and application of mesoporous molecular sieve for miniaturized matrix solid-phase dispersion extraction of bioactive flavonoids from toothpaste, plant, and saliva.

PubMed

Cao, Wan; Cao, Jun; Ye, Li-Hong; Xu, Jing-Jing; Hu, Shuai-Shuai; Peng, Li-Qing

2015-12-01

This article describes the use of the mesoporous molecular sieve KIT-6 as a sorbent in miniaturized matrix solid-phase dispersion (MSPD) in combination with ultra-performance LC for the determination of bioactive flavonoids in toothpaste, Scutellariae Radix, and saliva. In this study, for the first time, KIT-6 was used as a sorbent material for this mode of extraction. Compared with common silica-based sorbents (C18 and activated silica gel), the proposed KIT-6 dispersant with a three-dimensional cubic Ia3d structure and highly ordered arrays of mesoporous channels exhibits excellent adsorption capability of the tested compounds. In addition, several experimental variables, such as the mass ratio of sample to dispersant, grinding time, and elution solvent, were optimized to maximize the extraction efficiency. The proposed analytical method is simple, fast, and entails low consumption of samples, dispersants and elution solvents, thereby meeting "green chemistry" requirements. Under the optimized conditions, the recoveries of three bioactive flavonoids obtained by analyzing the spiked samples were from 89.22 to 101.17%. Also, the LODs and LOQs for determining the analytes were in the range of 0.02-0.04 μg/mL and 0.07-0.13 μg/mL, respectively. Finally, the miniaturized matrix solid-phase dispersion method was successfully applied to the analysis of target solutes in real samples, and satisfactory results were obtained. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effectiveness of different types of hair traps for brown bear research and monitoring

PubMed Central

Okarma, Henryk; Selva, Nuria

2017-01-01

Non-invasive sampling by hair-trapping is increasingly used worldwide in wildlife research. Despite this rise and the potential of hair samples for ecology and conservation studies, the relative performance of hair collection devices has been rarely tested. Here, we compare the effectiveness of five types of hair traps for brown bears Ursus arctos in the Carpathian Mountains (SE Poland) and test the effects of trap type, season, number of days elapsed since trap installation and trap features on the trapping success in order to provide recommendations for optimal sampling in future studies. The trap types were corral, path-trap, “smola”(beechwood tar) tree-trap, turpentine tree-trap and natural rub. In 2010, we collected 858 hair samples during 2330 inspections of 175 hair traps and found that the most effective traps were smola tree-traps (mean percentage of successful inspections ± SD: 30.2% ± 26.0) and natural rubs (50.8% ± 16.7). Based on this finding, over the following 2 years we focused on 24 smola tree-traps and eight natural rubs. During this long-term survey (2010–2012, 969 inspections, 1322 samples collected) the trapping success increased with time and smola tree-traps achieved similar effectiveness to natural rubs (45.5% ± 29.7 and 45.9 ± 23.4, respectively). We show that when baiting smola tree-traps ten weeks prior to research or monitoring, sampling effectiveness can reach up to 30%. Taking into account the logistical and methodological constraints associated with detecting and using natural rubs for a proper survey design, we recommend using smola tree-traps baited in advance for hair sampling in wildlife studies. PMID:29073161

Effectiveness of different types of hair traps for brown bear research and monitoring.

PubMed

Berezowska-Cnota, Teresa; Luque-Márquez, Ignacio; Elguero-Claramunt, Isabel; Bojarska, Katarzyna; Okarma, Henryk; Selva, Nuria

2017-01-01

Non-invasive sampling by hair-trapping is increasingly used worldwide in wildlife research. Despite this rise and the potential of hair samples for ecology and conservation studies, the relative performance of hair collection devices has been rarely tested. Here, we compare the effectiveness of five types of hair traps for brown bears Ursus arctos in the Carpathian Mountains (SE Poland) and test the effects of trap type, season, number of days elapsed since trap installation and trap features on the trapping success in order to provide recommendations for optimal sampling in future studies. The trap types were corral, path-trap, "smola"(beechwood tar) tree-trap, turpentine tree-trap and natural rub. In 2010, we collected 858 hair samples during 2330 inspections of 175 hair traps and found that the most effective traps were smola tree-traps (mean percentage of successful inspections ± SD: 30.2% ± 26.0) and natural rubs (50.8% ± 16.7). Based on this finding, over the following 2 years we focused on 24 smola tree-traps and eight natural rubs. During this long-term survey (2010-2012, 969 inspections, 1322 samples collected) the trapping success increased with time and smola tree-traps achieved similar effectiveness to natural rubs (45.5% ± 29.7 and 45.9 ± 23.4, respectively). We show that when baiting smola tree-traps ten weeks prior to research or monitoring, sampling effectiveness can reach up to 30%. Taking into account the logistical and methodological constraints associated with detecting and using natural rubs for a proper survey design, we recommend using smola tree-traps baited in advance for hair sampling in wildlife studies.

Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.

PubMed

Akbarzade, Samaneh; Chamsaz, Mahmoud; Rounaghi, Gholam Hossein; Ghorbani, Mahdi

2018-01-01

A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL -1 , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.

OPTIMIZING THE PAKS METHOD FOR MEASURING AIRBORNE ACROLEIN

EPA Science Inventory

Airborne acrolein is produced from the combustion of fuel and tobacco and is of concern due to its potential for respiratory tract irritation and other adverse health effects. Active sampling with DNPH-coated solid sorbents has been widely used for sampling airborne carbonyls; ...

Carboxylated graphene oxide/polyvinyl chloride as solid-phase extraction sorbent combined with ion chromatography for the determination of sulfonamides in cosmetics.

PubMed

Zhong, Zhixiong; Li, Gongke; Luo, Zhibin; Liu, Zhe; Shao, Yijuan; He, Wanwen; Deng, Jianchao; Luo, Xingling

2015-08-12

A carboxylated graphene oxide/polyvinyl chloride (CGO/PVC) material was prepared as a sorbent for the selective extraction of sulphonamides from complex sample. After being dispersed in buffer solution, sample was transferred into the prefabricated solid-phase extraction (SPE) column, which integrated extraction and cleanup into one single-step. A multi-response optimization based on the Box-Behnken design was used to optimize factors affecting extraction efficiency. Compared with the commonly commercial sorbents including MCX, WCX and C18, CGO/PVC hybrid material had higher extraction selectivity and capacity to sulphonamides. The limits of detection and quantification for seven target compounds were in the range of 3.4-7.1 μg/L and 11.4-23.7 μg/L, respectively. The self-assembly SPE cartridge was successfully used to enrich seven analytes in anti-acne cosmetics prior to ion chromatography detection with good recoveries of 87.8-102.0% and relative standard deviations of 1.2-6.4%, implying that this method was suitable for routine analysis of cosmetics. Copyright © 2015 Elsevier B.V. All rights reserved.

Efficient MgO-based mesoporous CO2 trapper and its performance at high temperature.

PubMed

Han, Kun Kun; Zhou, Yu; Chun, Yuan; Zhu, Jian Hua

2012-02-15

A novel MgO-based porous adsorbent has been synthesized in a facile co-precipitation method for the first time, in order to provide a candidate for trapping CO(2) in flue gas at high temperature. The resulting composite exhibits a mesoporous structure with a wide pore size distribution, due to the even dispersion and distribution of microcrystalline MgO in the framework of alumina to form a concrete-like structure. These sorbents can capture CO(2) at high temperature (150-400°C), possessing high reactivity and stability in cyclic adsorption-desorption processes, providing competitive candidates to control CO(2) emission. Copyright © 2011 Elsevier B.V. All rights reserved.

Application of flotation for the separation of metal-loaded zeolites.

PubMed

Matis, Kostas A; Zouboulis, Anastasios I; Gallios, George P; Erwe, Torsten; Blöcher, Christoph

2004-04-01

Several industrial wastewater streams may contain heavy metal ions, which must be effectively removed, before the discharge or reuse of treated waters could take place. Different bonding materials, presenting selectivity and fast reaction kinetics for the removal of metals, have been examined for this purpose. The objective of the present paper was to investigate the application of dispersed-air flotation for the separation of metal-loaded sorbents. Two similar zeolite samples were applied as effective bonding agents for the removal of zinc, a toxic metal commonly found in many industrial wastewaters. This combined process, termed sorptive flotation, involves the preliminary scavenging of metal ions, by using the appropriate sorbent particles (usually present as ultrafine particulates), followed by flotation for the effective separation of them. The obtained results were very promising, as both metal and sorbent were effectively removed/separated from the dispersion.

Development of cost-effective noncarbon sorbents for Hg(0) removal from coal-fired power plants.

PubMed

Lee, Joo-Youp; Ju, Yuhong; Keener, Tim C; Varma, Rajender S

2006-04-15

Noncarbonaceous materials or mineral oxides (silica gel, alumina, molecular sieves, zeolites, and montmorillonite) were modified with various functional groups such as amine, amide, thiol, urea, and active additives such as elemental sulfur, sodium sulfide, and sodium polysulfide to examine their potential as sorbents for the removal of elemental mercury (Hg(0)) vapor at coal-fired utility power plants. A number of sorbent candidates such as amine- silica gel, urea- silica gel, thiol- silica gel, amide-silica gel, sulfur-alumina, sulfur-molecular sieve, sulfur-montmorillonite, sodium sulfide-montmorillonite, and sodium polysulfide-montmorillonite, were synthesized and tested in a lab-scale fixed-bed system under an argon flow for screening purposes at 70 degrees C and/or 140 degrees C. Several functionalized silica materials reported in previous studies to effectively control heavy metals in the aqueous phase showed insignificant adsorption capacities for Hg(0) control in the gas phase, suggesting that mercury removal mechanisms in both phases are different. Among elemental sulfur-, sodium sulfide-, and sodium polysulfide-impregnated inorganic samples, sodium polysulfide-impregnated montmorillonite K 10 showed a moderate adsorption capacity at 70 degrees C, which can be used for sorbent injection prior to the wet FGD system.

Sampling bee communities using pan traps: alternative methods increase sample size

USDA-ARS?s Scientific Manuscript database

Monitoring of the status of bee populations and inventories of bee faunas require systematic sampling. Efficiency and ease of implementation has encouraged the use of pan traps to sample bees. Efforts to find an optimal standardized sampling method for pan traps have focused on pan trap color. Th...

Fused Deposition Modeling Enables the Low-Cost Fabrication of Porous, Customized-Shape Sorbents for Small-Molecule Extraction.

PubMed

Belka, Mariusz; Ulenberg, Szymon; Bączek, Tomasz

2017-04-18

Fused deposition modeling, one of the most common techniques in three-dimensional printing and additive manufacturing, has many practical applications in the fields of chemistry and pharmacy. We demonstrate that a thermoplastic elastomer-poly(vinyl alcohol) (PVA) composite material (LAY-FOMM 60), which presents porous properties after PVA removal, is useful for the extraction of small-molecule drug-like compounds from water samples. The usefulness of the proposed approach is demonstrated by the extraction of glimepiride from a water sample, followed by LC-MS analysis. The recovery was 82.24%, with a relative standard deviation of less than 5%. The proposed approach can change the way of thinking about extraction and sample preparation due to a shift to the use of sorbents with customizable size, shape, and chemical properties that do not rely on commercial suppliers.

Small Column Testing of Superlig 639 for Removal of 99Tc from Hanford Tank Waste Envelope C (Tank 241-AN-107)

DOE Office of Scientific and Technical Information (OSTI.GOV)

DL Blanchard; DE Kurath; BM Rapko

The current BNFL Inc. flow sheet for pretreating Hanford High-Level tank wastes includes the use of Superlig(reg.sign)639 (SL-639) in a dual column system for removing technetium-99 ({sup 99}Tc) from the aqueous fraction of the waste. This sorbent material has been developed and supplied by IBC Advanced Technologies, Inc., American Fork, UT. This report documents the results of testing the SL-639 sorbent with diluted waste [Na{sup +}] {approx} 5 M from Tank 241-AN-107 (an Envelope C waste, abbreviated AN-107) at Battelle Northwest Laboratories (BNW). The equilibrium behavior was assessed with batch contacts between the sorbent and the waste. Two AN-107 samplesmore » were used: (1) an archived sample from previous testing and (2) a more recent sample collected specifically for BNFL. A portion of the archive sample and all of the BNFL sample were treated to remove Sr-90 and transuranic elements (TRU). All samples had also been Cs decontaminated by ion exchange (IX), and were spiked with a technetium-95m ({sup 95m}Tc) pertechnetate tracer, {sup 95m}TcO{sub 4}{sup -}.The TcO{sub 4}{sup -} and total Tc K{sub d} values, assumed equal to the {sup 95m}Tc and {sup 99}Tc K{sub d}'s, respectively, are shown in Table S1. Values are averages of duplicates, which showed significant scatter. The total Tc K{sub d} for the BNFL sample is much lower than the TcO{sub 4}{sup -}, indicating that a large fraction of the {sup 99}Tc is not pertechnetate.« less

Application of statistical experimental design to the optimisation of microextraction by packed sorbent for the analysis of nonsteroidal anti-inflammatory drugs in human urine by ultra-high pressure liquid chromatography.

PubMed

Magiera, Sylwia; Gülmez, Şefika; Michalik, Aleksandra; Baranowska, Irena

2013-08-23

A new approach based on microextraction by packed sorbent (MEPS) and a reversed-phase ultra-high pressure liquid chromatography (UHPLC) method was developed and validated for the determination and quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) (acetylsalicylic acid, ketoprofen, diclofenac, naproxen and ibuprofen) in human urine. The important factors that could influence the extraction were previously screened using the Plackett-Burman design approach. The optimal MEPS extraction conditions were obtained using C18 phase as a sorbent, small sample volume (20μL) and a short time period (approximately 5min) for the entire sample preparation step. The analytes were separated on a core-shell column (Poroshell 120 EC-C18; 100mm×3.0mm; 2.7μm) using a binary mobile phase composed of aqueous 0.1% trifluoroacetic acid and acetonitrile in the gradient elution mode (4.5min of analysis time). The analytical method was fully validated based on linearity, limits of detection (LOD), limits of quantification (LOQ), inter- and intra-day precision and accuracy, and extraction yield. Under optimised conditions, excellent linearity (R(2)>0.9991), limits of detection (1.07-16.2ngmL(-1)) and precision (0.503-9.15% RSD) were observed for the target drugs. The average absolute recoveries of the analysed compounds extracted from the urine samples were 89.4-107%. The proposed method was also applied to the analysis of NSAIDs in human urine. The new approach offers an attractive alternative for the analysis of selected drugs from urine samples, providing several advantages including fewer sample preparation steps, faster sample throughput and ease of performance compared to traditional methodologies. Copyright © 2013 Elsevier B.V. All rights reserved.

Continuous fluidized-bed contactor with recycle of sorbent

DOEpatents

Scott, Charles D.; Petersen, James N.; Davison, Brian H.

1996-01-01

A continuous fluidized-bed contactor containing sorbent particles is used to remove solutes from liquid solvents. As the sorbent particles, for example gel beads, sorb the solute, for example metal ion species, the sorbent particles tend to decrease in diameter. These smaller loaded sorbent particles rise to the top of the contactor, as larger sorbent particles remain at the bottom of the contactor as a result of normal hydraulic forces. The smaller loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor. Alternatively, the loaded sorbent particles may also slightly increase in diameter, or exhibit no change in diameter but an increase in density. As a result of normal hydraulic forces the larger loaded sorbent particles fall to the bottom of the contactor. The larger loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor.

Continuous fluidized-bed contactor with recycle of sorbent

DOEpatents

Scott, C.D.; Petersen, J.N.; Davison, B.H.

1996-07-09

A continuous fluidized-bed contactor containing sorbent particles is used to remove solutes from liquid solvents. As the sorbent particles, for example gel beads, sorb the solute, for example metal ion species, the sorbent particles tend to decrease in diameter. These smaller loaded sorbent particles rise to the top of the contactor, and larger sorbent particles remain at the bottom of the contactor as a result of normal hydraulic forces. The smaller loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor. Alternatively, the loaded sorbent particles may also slightly increase in diameter, or exhibit no change in diameter but an increase in density. As a result of normal hydraulic forces the larger loaded sorbent particles fall to the bottom of the contactor. The larger loaded sorbent particles are then recovered, regenerated, and reintroduced into the contactor. 8 figs.

Determination of Three Organochlorine Pesticides in Aqueous Samples by Solid-Phase Extraction Based on Natural Nano Diatomite in Packed Syringe Coupled to Gas Chromatography-Mass Spectrometry.

PubMed

Taghani, Abdollah; Goudarzi, Nasser; Bagherian, Ghadamali; Chamjangali, Mansour Arab

2017-01-01

A rapid, simple, and sensitive technique is proposed based on a miniaturized solid-phase extraction method named mictroextraction in a packed syringe coupled with gas chromatography-mass spectrometry for the preconcentration and determination of three organochlorine pesticides. These include hexachlorobenzene, heptachlor and aldrine in aqueous samples. For the first time, the natural nano diatomite is used a sorbent. Based on this technique, 6.0 mg of the nano sorbent is inserted in a syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters, such as the solution pH, type and volume of the organic desorption solvent, and amount of sorbent on the extraction efficiency of the selected pesticides, is investigated. The proposed method shows good linearity in the range of 0.1 - 40.0 μg L -1 , and at low limits of detection in the range of 0.02 - 0.13 μg L -1 using the selected ion-monitoring mode. The reproducibility of this method was found to be in the range of 3.5 - 11.1% for the understudied pesticides. In order to evaluate the matrix effect, the developed method is also applied to the preconcentration and determination of the selected pesticides in different water samples.

Aptamer functionalized magnetic nanoparticles for effective extraction of ultratrace amounts of aflatoxin M1 prior its determination by HPLC.

PubMed

Khodadadi, Mohammad; Malekpour, Akbar; Mehrgardi, Masoud A

2018-06-09

Aptamers, due to the inherently high selectivity towards target analytes, are promising candidate for surface modification of the nanoparticles. Therefore, aptamer-functionalized magnetic nanoparticles (AMNPs) was prepared and used to develop a magnetic solid-phase extraction procedure for clean-up of milk and dairy products samples before measuring the aflatoxin M1 (AFM1) contents by the high-performance liquid chromatography. The prepared sorbent was characterized by different instrumental methods such as FT-IR, FESEM, TEM, EDX and AGFM. The AMNPs was used in extraction and pre-concentration of ultratrace amounts AFM1 from local milk samples. The amount of sorbent, elution volume, extraction time, and salt addition were optimized. Based on the results, calibration plot is linear over the 0.3 to 1 ng·L -1 and 5 to 50 ng·L -1 AFM1 concentration ranges. The limits of detection of the developed method were obtained 0.2 ng·L -1 which is the smallest value that has been reported up to now. The results show that this new superior sorbent has a large potential to simplify the complex matrix of the samples and can used for detection, preconcentration and accurate determination of ultratrace amounts of the AFM1 from milk and dairy products. Copyright © 2018 Elsevier B.V. All rights reserved.

Sample Integrity Evaluation and EPA Method 325b Interlaboratory Comparison for Select Volatile Organic Compounds Collected Diffusively on Carbopack X Sorbent Tubes

EPA Science Inventory

Sample integrity evaluations and inter-laboratory comparisons were conducted in application of U.S. Environmental Protection Agency (EPA) Methods 325A/B for monitoring benzene and additional selected volatile organic compounds (VOCs) usingpassive-diffusive Carbopack X tube sample...

Comparison of different mesoporous silicas for off-line solid phase extraction of 17β-estradiol from waters and its determination by HPLC-DAD.

PubMed

Gañán, Judith; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

2013-09-15

Functionalized (SBA-C₁₈ and SM-C₁₈) and non-functionalized (SBA-15 and SM) mesoporous silicas were then examined as sorbents for solid-phase extraction of 17β-estradiol in aqueous media. Experiments were run in order to test critical factors affecting the procedure extraction efficiency, including the type of sorbent, the analyte concentration, the solvent and volume used for elution and the sample volume. Among the prepared materials, SBA-C₁₈ had the highest adsorption affinity towards 17β-estradiol and under optimized conditions (200mg of sorbent, 150 mL of water sample, elution with 3 × 2 mL of methanol) this sorbent proved good extraction capacity and elution efficiency for this hormone from aqueous media (recovery near 100%). To evaluate the analytical applicability of the proposed method, it was applied to the determination of 17β-estradiol in drinking water by high performance liquid chromatography with a photodiode array detector. Calibration curves were shown to be linear between 1.25 and 100 mg L(-1)with correlation coefficients ≥0.999 (n=5) for 17β-estradiol. The instrumental detection and quantitation limits calculated were 0.38 and 1.25 mg L(-1), respectively. The relative standard deviation obtained values were ≤3% and the mean recoveries obtained were of 82%. The results suggest that SBA-C18 is a promising material for the off-line solid phase extraction of 17β-estradiol from waters. Copyright © 2013 Elsevier B.V. All rights reserved.

Trace Contaminant Testing with the Orion Atmosphere Revitalization Technology

NASA Technical Reports Server (NTRS)

Button, Amy Lin; Sweterlitsch, Jeffrey; Broerman, Craig

2009-01-01

Every spacecraft atmosphere contains trace contaminants resulting from offgassing by cabin materials and human passengers. An amine-based carbon dioxide (CO2) and water vapor sorbent in pressure-swing regenerable beds has been developed by Hamilton Sundstrand and baselined for the Orion Atmosphere Revitalization System (ARS). Part of the risk mitigation effort for this new technology is the study of how atmospheric trace contaminants will affect and be affected by the technology. One particular area of concern is ammonia, which, in addition to the normal spacecraft sources, can also be off-gassed by the amine-based sorbent. In the first half of 2009, tests were performed with typical cabin atmosphere levels of five of the most common trace gases, most of which had not yet been tested with this technology. A subscale sample of the sorbent was exposed to each of the chemicals mixed into a stream of moist, CO2-laden air, and the CO2 adsorption capacity of the sorbent was compared before and after the exposure. After these typical-concentration chemicals were proven to have negligible effect on the subscale sample, tests proceeded on a full-scale test article in a sealed chamber with a suite of eleven contaminants. To isolate the effects of various test rig components, several extended-duration tests were run: without injection or scrubbing, with injection and without scrubbing, with injection and scrubbing by both the test article and dedicated trace contaminant filters, and with injection and scrubbing by only the test article. The high-level results of both the subscale and full-scale tests are examined in this paper.

Quaternary ammonium-functionalized MCM-48 mesoporous silica as a sorbent for the dispersive solid-phase extraction of endocrine disrupting compounds in water.

PubMed

Zhang, Shijuan; Lu, Fengli; Ma, Xiaoyun; Yue, Mingbo; Li, Yanxin; Liu, Jiammin; You, Jinmao

2018-07-06

MCM-48 mesoporous silica was functionalized with dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride, a quaternary ammonium salt with a long hydrophobic chain, to prepare a new sorbent for the dispersive solid-phase extraction (DSPE) of seven endocrine disrupting compounds (EDCs) including 4-hexylphenol, 4-octylphenol, 4-nonylphenol, bisphenol A, estrone, 17β-estradiol and estriol in water. A series of differently functionalized MCM-48 materials were also synthesized, and they served as reference materials to study the mechanism. The developed DSPE method was combined with HPLC with fluorescence detection to evaluate the adsorption performance. The results indicated that the quaternary ammonium-functionalized MCM-48 mesoporous silica can be used as ideal sorbent for EDCs in water with recoveries of higher than 95% due to the electrostatic interactions and hydrophobic effect. Hydrogen bonding and π-π interactions in other synthesized materials could lead to about 25-30% increase in recoveries, but the results for polyhydroxy compounds were still not satisfying. The quaternary ammonium-functionalized MCM-48 mesoporous silica was successfully applied to the DSPE of EDCs in real water samples. The optimum extraction conditions were sorbent amount, 15 mg; desorption time; 5 min; elution volume, 0.8 mL; sample pH 3.0; and salt addition, 5 g/L. The limits of detection were in the range of 1.2-2.6 ng/L, while the limits of quantitation were in the range of 4.3-8.3 ng/L. Copyright © 2018 Elsevier B.V. All rights reserved.

Solid-phase extraction-fluorimetric high performance liquid chromatographic determination of domoic acid in natural seawater mediated by an amorphous titania sorbent.

PubMed

Chan, Ivy O M; Tsang, Vic W H; Chu, K K; Leung, S K; Lam, Michael H W; Lau, T C; Lam, Paul K S; Wu, Rudolf S S

2007-01-30

The feasibility of using sol-gel amorphous titania (TiO2) as a solid-phase sorbent for the pre-concentration of domoic acid (DA), a potent amnesic shellfish poisoning (ASP) toxin, directly from seawater was explored. The sol-gel titania material is able to adsorb DA from seawater, via the formation of ester-linkage between the carboxylic moieties of DA and the Ti-OH groups on the sorbent surface, at low pH and desorb it at high pH. The chemisorption process is not significantly interfered by the seawater matrix. The optimum pH values for the adsorption and desorption of DA were found to be pH 4 and 11, respectively. The optimal sorbent loading for the batch-type solid-phase extraction of DA was 0.67 mg-TiO2 ng-DA(-1) and adsorption equilibrium was achieved in 2 h at room temperature. The desorbed DA in 500 microL of 0.1 M alkaline borate buffer can be directly derviatized by 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) in aqueous media for fluorimetric HPLC quantification. Analyte recovery, repeatability and detection limit of this titania SPE-fluorimetric HPLC determination are 89%, 6.2% and 120 pg-DA mL(-1) (n=7, P<0.05), respectively, for a sample volume of 30 mL. This titania SPE technique should also be applicable to the pre-concentration of other polar carboxylate- and phosphonate-containing biomolecules and pharmaceuticals in complex and interfering environmental sample matrices.

Development of Highly Durable and Reactive Regenerable Magnesium-Based Sorbents for CO2 Separation in Coal Gasification Process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Javad Abbasian; Armin Hassanzadeh Khayyat; Rachid B. Slimane

The specific objective of this project was to develop physically durable and chemically regenerable MgO-based sorbents that can remove carbon dioxide from raw coal gas at operating condition prevailing in IGCC processes. A total of sixty two (62) different sorbents were prepared in this project. The sorbents were prepared either by various sol-gel techniques (22 formulations) or modification of dolomite (40 formulations). The sorbents were prepared in the form of pellets and in granular forms. The solgel based sorbents had very high physical strength, relatively high surface area, and very low average pore diameter. The magnesium content of the sorbentsmore » was estimated to be 4-6 % w/w. To improve the reactivity of the sorbents toward CO{sub 2}, The sorbents were impregnated with potassium salts. The potassium content of the sorbents was about 5%. The dolomite-based sorbents were prepared by calcination of dolomite at various temperature and calcination environment (CO{sub 2} partial pressure and moisture). Potassium carbonate was added to the half-calcined dolomite through wet impregnation method. The estimated potassium content of the impregnated sorbents was in the range of 1-6% w/w. In general, the modified dolomite sorbents have significantly higher magnesium content, larger pore diameter and lower surface area, resulting in significantly higher reactivity compared to the sol-gel sorbents. The reactivities of a number of sorbents toward CO{sub 2} were determined in a Thermogravimetric Analyzer (TGA) unit. The results indicated that at the low CO{sub 2} partial pressures (i.e., 1 atm), the reactivities of the sorbents toward CO{sub 2} are very low. At elevated pressures (i.e., CO{sub 2} partial pressure of 10 bar) the maximum conversion of MgO obtained with the sol-gel based sorbents was about 5%, which corresponds to a maximum CO{sub 2} absorption capacity of less than 1%. The overall capacity of modified dolomite sorbents were at least one order of magnitude higher than those of the sol-gel based sorbents. The results of the tests conducted with various dolomite-based sorbent indicate that the reactivity of the modified dolomite sorbent increases with increasing potassium concentration, while higher calcination temperature adversely affects the sorbent reactivity. Furthermore, the results indicate that as long as the absorption temperature is well below the equilibrium temperature, the reactivity of the sorbent improves with increasing temperature (350-425 C). As the temperature approaches the equilibrium temperature, because of the significant increase in the rate of reverse (i.e., regeneration) reaction, the rate of CO{sub 2} absorption decreases. The results of cyclic tests show that the reactivity of the sorbent gradually decreases in the cyclic process. To improve long-term durability (i.e., reactivity and capacity) of the sorbent, the sorbent was periodically re-impregnated with potassium additive and calcined. The results indicate that, in general, re-treatment improves the performance of the sorbent, and that, the extent of improvement gradually decreases in the cyclic process. The presence of steam significantly enhances the sorbent reactivity and significantly decreases the rate of decline in sorbent deactivation in the cyclic process.« less

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

NASA Astrophysics Data System (ADS)

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.

Flow-injection determination of total organic fluorine with off-line defluorination reaction on a solid sorbent bed.

PubMed

Musijowski, Jacek; Trojanowicz, Marek; Szostek, Bogdan; da Costa Lima, José Luis Fontes; Lapa, Rui; Yamashita, Hiroki; Takayanagi, Toshio; Motomizu, Shoji

2007-09-26

Considering recent reports on widespread occurrence and concerns about perfluoroalkyl substances (PFAS) in environmental and biological systems, analysis of these compounds have gained much attention in recent years. Majority of analyte-specific methods are based on a LC/MS/MS or a GC/MS detection, however many environmental or biological studies would benefit from a total organic fluorine (TOF) determination. Presented work was aimed at developing a method for TOF determination. TOF is determined as an amount of inorganic fluoride obtained after defluorination reaction conducted off-line using sodium biphenyl reagent directly on the sorbent without elution of retained analytes. Recovered fluoride was analyzed using flow-injection system with either fluorimetric or potentiometric detection. The TOF method was tested using perfluorocarboxylic acids (PFCA), including perfluorooctanoic acid (PFOA), as model compounds. Considering low concentrations of PFAS in natural samples, solid-phase extraction as a preconcentration procedure was evaluated. Several carbon-based sorbents were tested, namely multi-wall carbon nanotubes, carbon nanofibres and activated carbon. Good sorption of all analytes was achieved and defluorination reaction was possible to carry out directly on a sorbent bed. Recoveries obtained for PFCAs, adsorbed on an activated carbon sorbent, and measured as TOF, were 99.5+/-1.7, 110+/-9.4, 95+/-26, 120+/-32, 110+/-12 for C4, C6, C8, C10 and C12-PFCA, respectively. Two flow systems that would enable the defluorination reaction and fluoride determination in a single system were designed and tested.

Ozone and Ozone By-Products in the Cabins of Commercial Aircraft

PubMed Central

Weisel, Clifford; Weschler, Charles J.; Mohan, Kris; Vallarino, Jose; Spengler, John D.

2013-01-01

The aircraft cabin represents a unique indoor environment due to its high surface-to-volume ratio, high occupant density and the potential for high ozone concentrations at cruising altitudes. Ozone was continuously measured and air was sampled on sorbent traps, targeting carbonyl compounds, on 52 transcontinental U.S. or international flights between 2008 and 2010. The sampling was predominantly on planes that did not have ozone scrubbers (catalytic converters). Peak ozone levels on aircraft without catalytic convertors exceeded 100 ppb, with some flights having periods of more than an hour when the ozone levels were > 75ppb. Ozone was greatly reduced on relatively new aircraft with catalytic convertors, but ozone levels on two flights whose aircraft had older convertors were similar to those on planes without catalytic convertors. Hexanal, heptanal, octanal, nonanal, decanal and 6-methyl-5-hepten-2-one (6-MHO) were detected in the aircraft cabin at sub- to low ppb levels. Linear regression models that included the log transformed mean ozone concentration, percent occupancy and plane type were statistically significant and explained between 18 and 25% of the variance in the mixing ratio of these carbonyls. Occupancy was also a significant factor for 6-MHO, but not the linear aldehydes, consistent with 6-MHO’s formation from the reaction between ozone and squalene, which is present in human skin oils. PMID:23517299

Sorbents for the oxidation and removal of mercury

DOEpatents

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

2013-08-20

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.

Sorbents for the oxidation and removal of mercury

DOEpatents

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.

Sorbents for the oxidation and removal of mercury

DOEpatents

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

2012-05-01

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.

Sorbents for the oxidation and removal of mercury

DOEpatents

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

2014-09-02

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.

Microextraction by Packed Sorbent (MEPS) and Solid-Phase Microextraction (SPME) as Sample Preparation Procedures for the Metabolomic Profiling of Urine

PubMed Central

Silva, Catarina; Cavaco, Carina; Perestrelo, Rosa; Pereira, Jorge; Câmara, José S.

2014-01-01

For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS) and solid-phase microextraction (SPME), completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones. PMID:24958388

AUDIT MATERIALS FOR SEMIVOLATILE ORGANIC MEASUREMENTS DURING HAZARDOUS WASTE TRIAL BURNS

EPA Science Inventory

Two new performance audit materials utilizing different sorbents have neen developed to assess the overall accuracy and precision of the sampling, desorption, and analysis of semivolatile organic compounds by EPA, SW 846 Method 0010 (i.e., the Modified Method 5 sampling train). h...

Breakthrough of 1,3-dichloropropene and chloropicrin from 600 mg XAD-4 air sampling tubes

USDA-ARS?s Scientific Manuscript database

Accurately measuring air concentrations of agricultural fumigants is important for the regulation of air quality. Understanding the conditions under which sorbent tubes can effectively retain such fumigants during sampling is critical in mitigating chemical breakthrough from the tubes and facilitati...

Evaluation of ionic liquids supported on silica as a sorbent for fully automated online solid-phase extraction with LC-MS determination of sulfonamides in bovine milk samples.

PubMed

da Silva, Meire Ribeiro; Mauro Lanças, Fernando

2018-03-10

Sulfonamides are antibiotics widely used in the treatment of diseases in dairy cattle. However, their indiscriminate use for disease control may lead to their presence in tissues and milk and their determination requires a sample preparation step as part of an analytical approach. Among the several sample preparation techniques available, those based upon the use of sorptive materials have been widely employed. Recently, the application of ionic liquids immobilized on silica surfaces or polymeric materials has been evaluated for such an application. This manuscript addresses the evaluation of silica-based ionic liquid obtained by a sol-gel synthesis process by basic catalysis as sorbent for online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry for sulfonamides determination. Infrared vibrational spectroscopy confirmed the presence of the ionic liquid on the silica surface, suggesting that the ionic liquid was anchored on to the silica surface. Other sorbents varying the ionic liquid alkyl chain were also synthesized and evaluated by off-line solid-phase extraction in the sulfonamide extraction. As the length of the alkyl chain increased, the amount of extracted sulfonamides decreased, possibly due to a decrease in the electrostatic interaction caused by the reduction in the polarity, as well as the presence of a hexafluorophosphate anion that increases the hydrophobic character of the material. The use of 1-butyl-3-methylimidazolium hexafluorophosphate as a selective ionic liquid sorbent enabled the isolation and sulfonamide preconcentration in bovine milk by online solid-phase extraction with liquid chromatography and electrospray ionization time-of-flight mass spectrometry. The limit of quantification for the method developed was 5-7, 5 μg/mL, with extraction recoveries ranging between 74 and 93% and intra- and interassay between 1.5-12.5 and 2.3-13.1, respectively. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Magnetic sporopollenin-cyanopropyltriethoxysilane-dispersive micro-solid phase extraction coupled with high performance liquid chromatography for the determination of selected non-steroidal anti-inflammatory drugs in water samples.

PubMed

Abd Wahib, Siti Munirah; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Kamboh, Muhammad Afzal; Abdul Keyon, Aemi S

2018-01-12

A facile dispersive-micro-solid phase extraction (D-μ-SPE) method coupled with HPLC for the analysis of selected non-steroidal anti-inflammatory drugs (NSAIDs) in water samples was developed using a newly prepared magnetic sporopollenin-cyanopropyltriethoxysilane (MS-CNPrTEOS) sorbent. Sporopollenin homogenous microparticles of Lycopodium clavatum spores possessed accessible functional groups that facilitated surface modification. Simple modification was performed by functionalization with 3-cyanopropyltriethoxysilane (CNPrTEOS) and magnetite was introduced onto the biopolymer to simplify the extraction process. MS-CNPrTEOS was identified by infrared spectrometrywhile the morphology and the magnetic property were confirmed by scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM), respectively. To maximize the extraction performance of ketoprofen, ibuprofen, diclofenac and mefenamic acid using the proposed MS-CNPrTEOS, important D-μ-SPE parameters were comprehensively optimized. The optimum extraction conditions were sorbent amount, 40 mg; extraction time, 5 min; desorption time; 5 min; sample volume, 15 mL; sample pH 2.0; and salt addition, 2.5% (w/v). The feasibility of the developed method was evaluated using spiked tap water, lake water, river water and waste water samples. Results showed that ketoprofen and ibuprofen were linear in the range of 1.0-1000 μg L -1 whilst diclofenac and mefenamic acid were linear in the range 0.8-500 μg L -1 . The results also showed good detection limits for the studied NSAIDs in the range of 0.21-0.51 μg L -1 and good recoveries for spiked water samples in the range of 85.1-106.4%. The MS-CNPrTEOS proved a promising dispersive sorbent and applicable to facile and rapid assay of NSAIDs in water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Analytical method validation for the determination of 2,3,3,3-tetrafluoropropene in air samples using gas chromatography with flame ionization detection.

PubMed

Mawn, Michael P; Kurtz, Kristine; Stahl, Deborah; Chalfant, Richard L; Koban, Mary E; Dawson, Barbara J

2013-01-01

A new low global warming refrigerant, 2,3,3,3-tetrafluoro propene, or HFO-1234yf, has been successfully evaluated for automotive air conditioning, and is also being evaluated for stationary refrigeration and air conditioning systems. Due to the advantageous environmental properties of HFO-1234yf versus HFC-134a, coupled with its similar physical properties and system performance, HFO-1234yf is also being evaluated to replace HFC-134a in refrigeration applications where neat HFC-134a is currently used. This study reports on the development and validation of a sampling and analytical method for the determination of HFO-1234yf in air. Different collection media were screened for desorption and simulated sampling efficiency with three-section (350/350/350 mg) Anasorb CSC showing the best results. Therefore, air samples were collected using two 3-section Anasorb CSC sorbent tubes in series at 0.02 L/min for up to 8 hr for sample volumes of up to 9.6 L. The sorbent tubes were extracted in methylene chloride, and analyzed by gas chromatography with flame ionization detection. The method was validated from 0.1× to 20× the target level of 0.5 ppm (2.3 mg/m(3)) for a 9.6 L air volume. Desorption efficiencies for HFO-1234yf were 88 to 109% for all replicates over the validation range with a mean overall recovery of 93%. Simulated sampling efficiencies ranged from 87 to 104% with a mean of 94%. No migration or breakthrough to the back tube was observed under the sampling conditions evaluated. HFO-1234yf samples showed acceptable storage stability on Anasorb CSC sorbent up to a period of 30 days when stored under ambient, refrigerated, or frozen temperature conditions.

Effect of precursor and preparation method on manganese based activated carbon sorbents for removing H2S from hot coal gas.

PubMed

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.

Bee (Hymenoptera: Apoidea) Diversity and Sampling Methodology in a Midwestern USA Deciduous Forest.

PubMed

McCravy, Kenneth W; Ruholl, Jared D

2017-08-04

Forests provide potentially important bee habitat, but little research has been done on forest bee diversity and the relative effectiveness of bee sampling methods in this environment. Bee diversity and sampling methodology were studied in an Illinois, USA upland oak-hickory forest using elevated and ground-level pan traps, malaise traps, and vane traps. 854 bees and 55 bee species were collected. Elevated pan traps collected the greatest number of bees (473), but ground-level pan traps collected greater species diversity (based on Simpson's diversity index) than did elevated pan traps. Elevated and ground-level pan traps collected the greatest bee species richness, with 43 and 39 species, respectively. An estimated sample size increase of over 18-fold would be required to approach minimum asymptotic richness using ground-level pan traps. Among pan trap colors/elevations, elevated yellow pan traps collected the greatest number of bees (266) but the lowest diversity. Malaise traps were relatively ineffective, collecting only 17 bees. Vane traps collected relatively low species richness (14 species), and Chao1 and abundance coverage estimators suggested that minimum asymptotic species richness was approached for that method. Bee species composition differed significantly between elevated pan traps, ground-level pan traps, and vane traps. Indicator species were significantly associated with each of these trap types, as well as with particular pan trap colors/elevations. These results indicate that Midwestern deciduous forests provide important bee habitat, and that the performance of common bee sampling methods varies substantially in this environment.

Geochemical hosts of solubilized radionuclides in uranium mill tailings

USGS Publications Warehouse

Landa, E.R.; Bush, C.A.

1990-01-01

The solubilization and subsequent resorption of radionuclides by ore components or by reaction products during the milling of uranium ores may have both economic and environmental consequences. Particle-size redistribution of radium during milling has been demonstrated by previous investigators; however, the identification of sorbing components in the tailings has received little experimental attention. In this study, uranium-bearing sandstone ore was milled, on a laboratory scale, with sulfuric acid. At regular intervals, filtrate from this suspension was placed in contact with mixtures of quartz sand and various potential sorbents which occur as gangue in uranium ores; the potential sorbents included clay minerals, iron and aluminum oxides, feldspar, fluorspar, barite, jarosite, coal, and volcanic glass. After equilibration, the quartz sand-sorbent mixtures were separated from the filtrate and radioassayed by gamma-spectrometry to determine the quantities of 238U, 230Th, 226Ra, and 210Pb sorbed, and the radon emanation coefficients. Sorption of 238U was low in all cases, with maximal sorptions of 1-2% by the bentonite- and coal-bearing samples. 230Th sorption also was generally less than 1%; maximal sorption here was observed in the fluorspar-bearing sample and appears to be associated with the formation of gypsum during milling. 226Ra and 210 Pb generally showed higher sorption than the other nuclides - more than 60% of the 26Ra solubilized from the ore was sorbed on the barite-bearing sample. The mechanism (s) for this sorption by a wide variety of substrates is not yet understood. Radon emanation coefficients of the samples ranged from about 5 to 30%, with the coal-bearing samples clearly demonstrating an emanating power higher than any of the other materials. ?? 1990.

Development of hyperbranched polymers with non-covalent interactions for extraction and determination of aflatoxins in cereal samples.

PubMed

Liu, Xiaoyan; Li, Huihui; Xu, Zhigang; Peng, Jialin; Zhu, Shuqiang; Zhang, Haixia

2013-10-03

A novel approach for assembling homogeneous hyperbranched polymers based on non-covalent interactions with aflatoxins was developed; the polymers were used to evaluate the extraction of aflatoxins B1, B2, G1 and G2 (AFB1, AFB2, AFG1 and AFG2) in simulant solutions. The results showed that the extraction efficiencies of three kinds of synthesized polymers for the investigated analytes were not statistically different; as a consequence, one of the representative polymers (polymer I) was used as the solid-phase extraction (SPE) sorbent to evaluate the influences of various parameters, such as desorption conditions, pH, ionic strength, concentration of methanol in sample solutions, and the mass of the sorbent on the extraction efficiency. In addition, the extraction efficiencies for these aflatoxins were compared between the investigated polymer and the traditional sorbent C18. The results showed that the investigated polymer had superior extraction efficiencies. Subsequently, the proposed polymer for the SPE packing material was employed to enrich and analyze four aflatoxins in the cereal powder samples. The limits of detection (LODs) at a signal-to-noise (S/N) ratio of 3 were in the range of 0.012-0.120 ng g(-1) for four aflatoxins, and the limits of quantification (LOQs) calculated at S/N=10 were from 0.04 to 0.40 ng g(-1) for four aflatoxins. The recoveries of four aflatoxins from cereal powder samples were in the range of 82.7-103% with relative standard deviations (RSDs) lower than 10%. The results demonstrate the suitability of the SPE approach for the analysis of trace aflatoxins in cereal powder samples. Copyright © 2013 Elsevier B.V. All rights reserved.

β-CD/ATP composite materials for use in dispersive solid-phase extraction to measure (fluoro)quinolone antibiotics in honey samples.

PubMed

Cui, Xiangqian; Zhang, Panjie; Yang, Xiaoling; Yang, Miyi; Zhou, Wenfeng; Zhang, Sanbin; Gao, Haixiang; Lu, Runhua

2015-06-09

A novel sorbent (β-CD/ATP composite) for dispersive solid-phase extraction (d-SPE) prepared by bonding β-cyclodextrin to modified attapulgite via silane coupling was used to determine the concentrations of four (fluoro)quinolones (Qs) in honey samples. The subsequent quantification of the Qs (ciprofloxacin, norfloxacin, ofloxacin, and gatifloxacin) was accomplished using high-performance liquid chromatography (HPLC) with ultraviolet detection after the d-SPE procedure. Parameters that may influence the extraction efficiency, such as type and volume of the eluent, type and amount of the sorbent, times of the vortex and sonication process, and pH of the sample, were investigated using batch and column procedures. The optimal experimental conditions (5 mL sample at pH 3, 4 mg of β-CD/ATP composite as the sorbent, 200 μL of 40% ammonia in methanol as the eluent, with vortex time 60s and sonication time 6 min, and no addition of salt) were obtained from this statistical evaluation. The limits of detection (LODs) were determined to the range from 0.30 to 3.95 μg L(-1). Good recoveries (83.6-88.6%) were obtained under the optimum conditions, and the relative standard deviations (RSDs), which are used to indicate reproducibility, were less than 7.4%. The method was validated with three real honey samples, and the results demonstrated that β-CD/ATP composite possessed a high adsorption capacity for Qs. Although the LODs were slightly higher than expected, this study confirmed the possibility of using cyclodextrin grafted palygorskite in analytical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of trace levels of benzophenone-type ultra-violet filters in real matrices by bar adsorptive micro-extraction using selective sorbent phases.

PubMed

Almeida, C; Stępkowska, A; Alegre, A; Nogueira, J M F

2013-10-11

Bar adsorptive micro-extraction (BAμE), using selective sorbent phases, followed by liquid desorption in combination with high performance liquid chromatography-diode array detection (BAμE-LD/HPLC-DAD), is proposed for the determination of trace levels of four benzophenone-type UV filters (benzophenone, 2-hydroxy-4-methoxy-benzophenone, 2,4-hydroxybenzophenone and 4-hydroxybenzophenone) in real matrices. By comparing three polymers (P1, P2 and P3) and five activated carbons (AC1, AC2, AC3, AC4 and AC5) phases, P2 (a modified pyrrolidone polymer) and AC4 coatings showed much higher selectivity and capacity through BAμE, where the former offers multiple mechanisms of interaction and faster equilibrium kinetics. Assays performed on 25mL of ultra-pure water samples spiked at the 8.0μg/L level, yielded recoveries ranging from 76.6±8.3% to 103.5±6.4% depending on the sorbent phase used (P2 or AC4), under optimized experimental conditions. The analytical performance showed convenient detection limits (0.3-0.5μg/L) and good linear dynamic ranges (1.0-24.0μg/L) with remarkable determination coefficients (r(2)>0.9969). Excellent repeatability was also achieved through intraday (RSD<13.0%) and interday (RSD<8.9%) experiments. By using the standard addition methodology, the application of the present analytical approach on sea water, wastewater, commercial cosmetic products and urine samples revealed good sensitivity, absence of matrix effects and the occurrence of levels of some benzophenones. The proposed methodology that uses nanostructured particles and operates under the floating sampling technology proved to be a sorption-based static micro-extraction alternative to monitor benzophenone-type UV filters in real matrices. Moreover, is easy to implement, reliable, sensitive, requiring low sample volume and the possibility to choose the most selective sorbent coating according to the target compounds involved. Copyright © 2013. Published by Elsevier B.V.

Optimizations of packed sorbent and inlet temperature for large volume-direct aqueous injection-gas chromatography to determine high boiling volatile organic compounds in water.

PubMed

Yu, Bofan; Song, Yonghui; Han, Lu; Yu, Huibin; Liu, Yang; Liu, Hongliang

2014-08-22

For the expanded application area, fast trace analysis of certain high boiling point (i.e., 150-250 °C) volatile organic compounds (HVOCs) in water, a large volume-direct aqueous injection-gas chromatography (LV-DAI-GC) method was optimized for the following parameters: packed sorbent for sample on-line pretreatment, inlet temperature and detectors configuration. Using the composite packed sorbent self-prepared with lithium chloride and a type of diatomite, the method enabled safe injection of an approximately 50-100 μL sample at an inlet temperature of 150 °C in the splitless mode and separated HVOCs from water matrix in 2 min. Coupled with a flame ionization detector (FID), an electron capture detector (ECD) and a flame photometric detector (FPD), the method could simultaneously quantify 27 HVOCs that belong to seven subclasses (i.e., halogenated aliphatic hydrocarbons, chlorobenzenes, nitrobenzenes, anilines, phenols, polycyclic aromatic hydrocarbons and organic sulfides) in 26 min. Injecting a 50 μL sample without any enrichment step, such as cryotrap focusing, the limits of quantification (LOQs) for the 27 HVOCs was 0.01-3 μg/L. Replicate analyses of the 27 HVOCs spiked source and river water samples exhibited good precision (relative standard deviations ≤ 11.3%) and accuracy (relative errors ≤ 17.6%). The optimized LV-DAI-GC was robust and applicable for fast determination and automated continuous monitoring of HVOCs in surface water. Copyright © 2014 Elsevier B.V. All rights reserved.

The choice of ultrasound assisted extraction coupled with spectrophotometric for rapid determination of gallic acid in water samples: Central composite design for optimization of process variables.

PubMed

Pooralhossini, Jaleh; Ghaedi, Mehrorang; Zanjanchi, Mohammad Ali; Asfaram, Arash

2017-01-01

A sensitive procedure namely ultrasound-assisted (UA) coupled dispersive nano solid-phase microextraction spectrophotometry (DNSPME-UV-Vis) was designed for preconcentration and subsequent determination of gallic acid (GA) from water samples, while the detailed of composition and morphology and also purity and structure of this new sorbent was identified by techniques like field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Energy-dispersive X-ray spectroscopy (EDX) techniques. Among conventional parameters viz. pH, amount of sorbent, sonication time and volume of elution solvent based on Response Surface Methodology (RSM) and central composite design according to statistics based contour the best operational conditions was set at pH of 2.0; 1.5mg sorbent, 4.0min sonication and 150μL ethanol. Under these pre-qualified conditions the method has linear response over wide concentration range of 15-6000ngmL -1 with a correlation coefficient of 0.9996. The good figure of merits like acceptable LOD (S/N=3) and LOQ (S/N=10) with numerical value of 2.923 and 9.744ngmL -1 , respectively and relative recovery between 95.54 and 100.02% show the applicability and efficiency of this method for real samples analysis with RSDs below 6.0%. Finally the method with good performance were used for monitoring under study analyte in various real samples like tap, river and mineral waters. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

PubMed

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.

Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection.

PubMed

Azzouz, Abdelmonaim; Ballesteros, Evaristo

2014-09-19

A novel analytical method using a continuous solid-phase extraction system in combination with gas chromatography-mass spectrometry for the simultaneous separation and determination of endocrine disrupting compounds (EDCs) is reported. The method was applied to major EDCs of various types including parabens, alkylphenols, phenylphenols, bisphenol A and triclosan in water. Samples were preconcentrated by using an automatic solid-phase extraction module containing a sorbent column, and retained analytes eluted with acetonitrile for derivatization with a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane. A number of variables potentially influencing recovery of the target compounds such as the type of SPE sorbent (Silica gel, Florisil, RP-C18, Amberlite XAD-2 and XAD-4, Oasis HLB and LiChrolut EN), eluent and properties of the water including pH and ionic strength, were examined. LiChrolut EN was found to be the most efficient sorbent for retaining the analytes, with ∼100% efficiency. The ensuing method was validated with good analytical results including low limits of detection (0.01-0.08ng/L for 100mL of sample) and good linearity (r(2)>0.997) throughout the studied concentration ranges. The method exhibited good accuracy (recoveries of 90-101%) and precision (relative standard deviations less than 7%) in the determination of EDCs in drinking, river, pond, well, swimming pool and waste water. Waste water samples were found to contain the largest number and highest concentrations of analytes (3.2-390ng/L). Copyright © 2014 Elsevier B.V. All rights reserved.

[Sampling optimization for tropical invertebrates: an example using dung beetles (Coleoptera: Scarabaeinae) in Venezuela].

PubMed

Ferrer-Paris, José Rafael; Sánchez-Mercado, Ada; Rodríguez, Jon Paul

2013-03-01

The development of efficient sampling protocols is an essential prerequisite to evaluate and identify priority conservation areas. There are f ew protocols for fauna inventory and monitoring in wide geographical scales for the tropics, where the complexity of communities and high biodiversity levels, make the implementation of efficient protocols more difficult. We proposed here a simple strategy to optimize the capture of dung beetles, applied to sampling with baited traps and generalizable to other sampling methods. We analyzed data from eight transects sampled between 2006-2008 withthe aim to develop an uniform sampling design, that allows to confidently estimate species richness, abundance and composition at wide geographical scales. We examined four characteristics of any sampling design that affect the effectiveness of the sampling effort: the number of traps, sampling duration, type and proportion of bait, and spatial arrangement of the traps along transects. We used species accumulation curves, rank-abundance plots, indicator species analysis, and multivariate correlograms. We captured 40 337 individuals (115 species/morphospecies of 23 genera). Most species were attracted by both dung and carrion, but two thirds had greater relative abundance in traps baited with human dung. Different aspects of the sampling design influenced each diversity attribute in different ways. To obtain reliable richness estimates, the number of traps was the most important aspect. Accurate abundance estimates were obtained when the sampling period was increased, while the spatial arrangement of traps was determinant to capture the species composition pattern. An optimum sampling strategy for accurate estimates of richness, abundance and diversity should: (1) set 50-70 traps to maximize the number of species detected, (2) get samples during 48-72 hours and set trap groups along the transect to reliably estimate species abundance, (3) set traps in groups of at least 10 traps to suitably record the local species composition, and (4) separate trap groups by a distance greater than 5-10km to avoid spatial autocorrelation. For the evaluation of other sampling protocols we recommend to, first, identify the elements of sampling design that could affect the sampled effort (the number of traps, sampling duration, type and proportion of bait) and their spatial distribution (spatial arrangement of the traps) and then, to evaluate how they affect richness, abundance and species composition estimates.

Grafting the sol-gel based sorbents by diazonium salts: a novel approach toward unbreakable capillary microextraction.

PubMed

Bagheri, Habib; Bayat, Parisa; Piri-Moghadam, Hamed

2013-11-29

The present work deals with a novel approach for grafting a sol-gel based sorbent, using diazonium salts for preparation of an unbreakable capillary microextraction (CME) device in on-line combination with high performance liquid chromatography (HPLC). The use of diazonium salts modifier allowed all types of metallic and non-metallic substrates to be used without any limitation. Substrates including copper, brass, stainless steel and polytetrafluoroethylene (PTFE) were chosen to be functionalized by chemical or electrochemical reduction of 4-amino phenyl acetic acid. Then, 3-(trimethoxysilyl)propylamine (3TMSPA) was selected as the precursor and the only reagent for preparation of the desired surface chemical bonded sorbent. The presence of chemical bond between substrate, diazonium salts and 3TMSPA is more probably responsible for thermal and solvent stability and long lifetime of the prepared sorbent. Characterization of the aryl group formation on the various substrates along with the prepared sorbents was thoroughly investigated by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and thermogravimetry analysis (TGA). Typically, one of the prepared sorbents, deposited on the inner surface of the copper tube, was selected for assessing the developed method. The CME device was used for on-line extraction of atrazine, ametryn and terbutryn, as model compounds, from the aquatic media. After extraction, the HPLC mobile phase was used for on-line desorption and elution of the extracted analytes from the CME loop, containing the grafted sol-gel based sorbent, through the HPLC column. Figures of merit of the developed method were also obtained in which the linearity for the analytes was in the range of 30-1000μgL(-1). The value of LOD (S/N=3) for all analytes was 10μgL(-1) and the RSD% values (n=5) were all below 9.4% at the 500μgL(-1) level. Applicability of the developed method was examined by analyzing some real water samples in which the relative recovery percentage ranged from 75 to 95%. Copyright © 2013 Elsevier B.V. All rights reserved.

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

NASA Technical Reports Server (NTRS)

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.

New high-capacity, calcium-based sorbents, calcium silicate sorbents. Final report, 1993--August 31, 1994

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kenney, M.C.; Chiang, R.K.; Fillgrove, K.L.

1995-02-01

A search is being carried out for new calcium-based S0{sub 2} sorbents for induct injection. More specifically, a search is being carried out for induct injection calcium silicate sorbents that are highly cost effective. The objectives for the current year include the study of sorbents made from Ca(OH){sub 2}, from mixtures of Ca(OH){sub 2} and SiO{sub 2}, and from portland cement. They also include the study of sorbents made from model compounds. During this year, sorbents prepared from Ca(OH){sub 2} and from mixtures of Ca(OH){sub 2} and fumed SiO{sub 2} were investigated. The results show that very good SiO{sub 2}-modifiedmore » Ca(OH){sub 2} sorbents in which the Si-to-Ca reactant ratio is low can be prepared from Ca(OH){sub 2} and fumed SiO{sub 2}. Sorbents prepared from Ca(OH){sub 2} and natural SiO{sub 2} or natural SiO{sub 2} sources were also studied. The results obtained show that very good SiO{sub 2}-modified Ca(OH){sub 2} sorbents and calcium silicate hydrate sorbents, C-S-H sorbents, can be prepared from Ca(OH){sub 2} and diatomite, pumice or perlite, minerals that are readily available. In addition. sorbents prepared from Ca{sub 3}SiO{sub 5} and {beta}-Ca{sub 2}SiO{sub 4} and from mixtures of these compounds and SiO{sub 2} were studied. The results secured demonstrate that very good C-S-H rich sorbents can be prepared from these compounds and from mixtures of them with SiO{sub 2}. They also provide information useful for interpreting the cement sorbent results. Sorbents prepared from cement and from mixtures of cement and natural SiO{sub 2} or SiO{sub 2} sources were investigated as well. The results secured show that cement and mixtures of it with diatomite, pumice or perlite rapidly yield excellent sorbents with the proper reaction conditions.« less

SO 2-Resistant Immobilized Amine Sorbents for CO 2 Capture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tumuluri, Uma

2014-01-01

The solid amine sorbent for CO 2 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 CO 2 capture capacity or low stability in the flue gas environment. This project is aimed at developing a SO 2-resistant solid amine sorbent for capturing CO 2 from coal–fired power plants with SCR/FGD which emits SO 2ranging 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 themore » initial capture capacity in presence of 1% SO 2. This amine sorbent was further modified by coating with polyethyleneglycol (PEG) to increase the SO 2-resistance. Polyethylene glycol (PEG) was found to decrease the SO 2-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 CO 2 capture capacity more than 2.3 mmol/g. The results of this study provided the scientific basis for further development of SO 2-resistant sorbents.« less

Fabrication of magnetite nano particles and modification with metal organic framework of Zn(2+) for sorption of doxycyline.

PubMed

Ghassemi Nooreini, Mahsa; Ahmad Panahi, Homayon

2016-10-15

This study presents a novel method for synthesis and characterization of a metal-organic framework and application in drug delivery. The first step was synthesis of amino functionalized magnetite that was then modified by a metal-organic framework of Zn(2+). This newly developed nano-sorbent was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive x-ray spectroscopy, thermogravimetric analysis, vibrating sample magnetometer and x-ray diffraction. Doxycycline was loaded to the nano-sorbent and effects of the variable parameters, kinetics of adsorption, release and capacity of adsorption were investigated. Test results specified maximum sorption of 21.5mgg(-1) for doxycycline in conditions of nano-sorbent at pH 7 and optimum time of 10min. Equilibrium adsorption data were analyzed by the Langmuir, Freundlich and Temkin models. Results showed that about 40% of doxycycline was released in simulated gastric fluid for the 30min and more than 70% was released in simulated intestinal fluid during 12h. These results were satisfactory and demonstrate that this new nano-sorbent modified with metal-organic framework had a good level of efficiency for drug delivery of doxycycline. Copyright © 2016 Elsevier B.V. All rights reserved.

Verification of diffusive and pumped samplers for volatile organic compounds using a controlled atmosphere test facility

NASA Astrophysics Data System (ADS)

Martin, Nicholas A.; Leming, Edward J.; Henderson, Malcolm H.; Lipscombe, Robert P.; Black, John K.; Jarvis, Scott D.

2010-09-01

There is a requirement to verify the performance of sorbent-based passive or active samplers and to extend their use, where possible, to monitor volatile organic compounds (VOCs) that are known to be photochemical ozone pre-cursors or are relevant to the activities of the petrochemical industry. We report measurements of the 14-day diffusive uptake rates for the VOCs: i-butane (2-methyl propane), n-butane, i-pentane (2-methyl butane), n-pentane, n-hexane, benzene, toluene, and m-xylene (at environmental level concentrations) for industry standard axial samplers (Perkin-Elmer-type samplers) containing the sorbents Carbopack-X, -Z, -B or Tenax-TA. We also present data on back-diffusion, blank levels, and storage for the above sorbents, and describe the simultaneous use of the sorbent Carbopack-X for pumped sampling of certain VOCs. The results were obtained by dosing samplers in a controlled atmosphere test facility (CATFAC) operating under well-defined conditions of concentration, nominal temperature of 20 °C, wind speed of 0.5 m s -1, and relative humidities of 0% and 80%. Field measurements were also obtained to provide supplementary data to support the laboratory study. Results are compared to existing published data, where these are available.

Effect of blend ratio of PP/kapok blend nonwoven fabrics on oil sorption capacity.

PubMed

Lee, Young-Hee; Kim, Ji-Soo; Kim, Do-Hyung; Shin, Min-Seung; Jung, Young-Jin; Lee, Dong-Jin; Kim, Han-Do

2013-01-01

More research and development on novel oil sorbent materials is needed to protect the environmental pollution. New nonwoven fabrics (pads) of polypropylene (PP)/kapok blends (blend ratio: 100/0, 75/25, 50/50, 25/75 and 10/90) were prepared by needle punching process at a fixed (optimized) condition (punch density: 50 punches/cm2 and depth: 4mm). This study focused on the effect of blend ratio of PP/kapok nonwoven fabrics on oil sorption capacities to find the best blend ratio having the highest synergy effect. The PP/kapok blend (50/50) sample has the lowest bulk density and showed the best oil absorption capacity. The oil sorption capacity of PP/kapok blend (50/50) nonwoven fabric for kerosene/soybean oil [21.09/27.01 (g oil/g sorbent)] was 1.5-2 times higher than those of commercial PP pad oil sorbents. The highest synergy effect of PP/kapok blend (50/50) was ascribed to the lowest bulk density of PP/kapok blend (50/50), which might be due to the highest morphologically incompatibility between PP fibre and kapok. These results suggest that the PP/kapok blend (50/50) having the highest synergy effect has a high potential as a new high-performance oil sorbent material.

Preparation of l-phenylalanine-imprinted solid-phase extraction sorbent by Pickering emulsion polymerization and the selective enrichment of l-phenylalanine from human urine.

PubMed

Li, Ji; Hu, Xiaoling; Guan, Ping; Zhang, Xiaoyan; Qian, Liwei; Zhang, Nan; Du, Chunbao; Song, Renyuan

2016-05-01

A novel l-phenylalanine molecularly imprinted solid-phase extraction sorbent was synthesized by the combination of Pickering emulsion polymerization and ion-pair dummy template imprinting. Compared to other polymerization methods, the molecularly imprinted polymers thus prepared exhibit a high specific surface, large pore diameter, and appropriate particle size. The key parameters for solid-phase extraction were optimized, and the result indicated that the molecularly imprinted polymer thus prepared exhibits a good recovery of 98.9% for l-phenylalanine. Under the optimized conditions of the procedure, an analytical method for l-phenylalanine was well established. By comparing the performance of the molecularly imprinted polymer and a commercial reverse-phase silica gel, the obtained molecularly imprinted polymer as an solid-phase extraction sorbent is more suitable, exhibiting high precision (relative standard deviation 3.2%, n = 4) and a low limit of detection (60.0 ± 1.9 nmol·L(-1) ) for the isolation of l-phenylalanine. Based on these results, the combination of the Pickering emulsion polymerization and ion-pair dummy template imprinting is effective for preparing selective solid-phase extraction sorbents for the separation of amino acids and organic acids from complex biological samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

One-pot synthesized functionalized mesoporous silica as a reversed-phase sorbent for solid-phase extraction of endocrine disrupting compounds in milks.

PubMed

Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Marina, María Luisa; Sierra, Isabel

2016-01-08

A new procedure for the determination of 12 naturally occurring hormones and some related synthetic chemicals in milk, commonly used as growth promoters in cattle, is reported. The method is based on liquid-liquid extraction followed by solid-phase extraction (SPE) using a new one-pot synthesized ordered mesoporous silica (of the SBA-15 type) functionalized with octadecyl groups (denoted as SBA-15-C18-CO) as reversed-phase sorbent. The analytes were eluted with methanol and then submitted to HPLC with diode array detection. Under optimal conditions, the method quantification limit for the analytes ranged from 0.023 to 1.36μg/mL. The sorbent affored the extraction of estrone, 17β-estradiol, estriol, progesterone, hexestrol, diethylstilbestrol, 4-androstene-3,17-dione, ethinylestradiol, 17α-methyltestosterone, nandrolone, prednisolone and testosterone with mean recoveries ranging from 72% to 105% (except for diethylstilbestrol) with RSD<11%. These results were comparable and, in some cases, even better than those obtained with other extraction methods, therefore SBA-15-C18-CO mesoporous silica possess a high potential as a reversed-phase sorbent for SPE of the 12 mentioned endocrine disrupting compounds in milk samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Trace Contaminant Testing with the Orion Atmosphere Revitalization Technology

NASA Technical Reports Server (NTRS)

Button, Amy B.; Sweterlitsch, Jeffrey J.; Broerman, Craig D.; Campbell, Melissa L.

2010-01-01

Every spacecraft atmosphere contains trace contaminants resulting from offgassing by cabin materials and human passengers. An amine-based carbon dioxide (CO2) and water vapor sorbent in pressure-swing regenerable beds has been developed by Hamilton Sundstrand and baselined for the Orion Atmosphere Revitalization System (ARS). Part of the risk mitigation effort for this new technology is the study of how atmospheric trace contaminants will affect and be affected by the technology. One particular area of concern is ammonia, which, in addition to the normal spacecraft sources, can also be offgassed by the amine-based sorbent. In the spring of 2009, tests were performed at Johnson Space Center (JSC) with typical cabin atmosphere levels of five of the most common trace gases, most of which had not yet been tested with this technology. A subscale sample of the sorbent was exposed to each of the chemicals mixed into a stream of moist, CO2-laden air, and the CO2 adsorption capacity of the sorbent was compared before and after the exposure. After these typical-concentration chemicals were proven to have negligible effect on the subscale sample, tests proceeded on a full-scale test article in a sealed chamber with a suite of eleven contaminants. To isolate the effects of various test rig components, several extended-duration tests were run: without injection or scrubbing, with injection and without scrubbing, with injection of both contaminants and metabolic CO2 and water vapor loads and scrubbing by both the test article and dedicated trace contaminant filters, and with the same injections and scrubbing by only the test article. The high-level results of both the subscale and full-scale tests are examined in this paper.

Magnetic solid phase extraction of brominated flame retardants and pentachlorophenol from environmental waters with carbon doped Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Yang, Jing; Li, Jia-yuan; Qiao, Jun-qin; Cui, Shi-hai; Lian, Hong-zhen; Chen, Hong-yuan

2014-12-01

Carbon doped Fe3O4 nanoparticles (Fe3O4/C) prepared by a facile hydrothermal reaction of glucose with iron resource have been applied as magnetic solid-phase extraction (MSPE) sorbent, for the first time, to extract trace brominated flame retardants (BFRs) and pentachlorophenol (PCP) from environmental waters. Various MSPE parameters were optimized including amount of Fe3O4/C nanoparticles, pH of sample solution, enrichment factor of analytes and reusability of Fe3O4/C sorbent. The reliability of the MSPE method was evaluated by the recoveries of BFRs and PCP in spiked water samples. Good recoveries (80.0-110.0%) were achieved with the relative standard deviations range from 0.3% to 6.8%. In this paper, the extraction characteristics of Fe3O4/C sorbent were further elucidated. It is found that the adsorption process of Fe3O4/C to analytes predominates the MSPE efficiency. There is hybrid hydrophobic interaction and hydrogen bonding or dipole-dipole attraction between Fe3O4/C and analytes. Notably, the chemical components of carbon layer on the surface of Fe3O4 nanoparticles were identified by X-ray photoelectron spectroscopy and thermogravimetry-mass spectrometry, and in consequence the covalent bonds between Fe3O4 and the coated carbon have been observed. In addition, the straight influence of synthesis condition of Fe3O4/C nanoparticles including glucose concentration and hydrothermal reaction time on extraction performance for BFRs and PCP has been investigated. It is confirmed that the existence of organic carbon containing functional groups over Fe3O4/C sorbent is responsible for the MSPE extraction.

Adsorption and removal of arsenic (V) using crystalline manganese (II,III) oxide: Kinetics, equilibrium, effect of pH and ionic strength.

PubMed

Babaeivelni, Kamel; Khodadoust, Amid P; Bogdan, Dorin

2014-01-01

Manganese (II,III) oxide (Mn3O4) crystalline powder was evaluated as a potential sorbent for removal of arsenic (V) from water. Adsorption isotherm experiments were carried out to determine the adsorption capacity using de-ionized (DI) water, a synthetic solution containing bicarbonate alkalinity, and two natual groundwater samples. Adsorption isotherm data followed the Langmuir and Freundlich equations, indicating favorable adsorption of arsenic (V) onto Mn3O4, while results from the Dubinin-Radushkevich equation were suggestive of chemisorption of arsenic (V). When normalized to the sorbent surface area, the maximum adsorption capacity of Mn3O4 for arsenic (V) was 101 μg m(-2), comparable to that of activated alumina. Arsenic (V) adsorption onto Mn3O4 followed pseudo-second-order kinetics. Adsorption of arsenic (V) was greatest at pH 2, while adsorption at pH 7-9 was within 91% of maximum adsorption, whereas adsorption decreased to 32% of maximum adsorption at pH 10. Surface charge analysis confirmed the adsorption of arsenic (V) onto the acidic surface of the Mn3O4 sorbent with a pHPZC of 7.32. The presence of coexisting ions bicarbonate and phosphate resulted in a decrease in arsenic (V) uptake. Comparable adsorption capacities were obtained for the synthetic solution and both groundwater samples. Overall, crystalline Mn3O4 was an effective and viable sorbent for removal of arsenic (V) from natural water, removing greater than 95% of arsenic (V) from a 1 mg L(-1) solution within 60 min of contact time.

Zero-valent iron/iron oxide-oxyhydroxide/graphene as a magnetic sorbent for the enrichment of polychlorinated biphenyls, polyaromatic hydrocarbons and phthalates prior to gas chromatography-mass spectrometry.

PubMed

Karamani, Anna A; Douvalis, Alexios P; Stalikas, Constantine D

2013-01-04

A composite magnetic material consisting of zero-valent iron, iron oxide-oxyhydroxide and graphene was synthesized and used successfully as a sorbent for the micro solid-phase extraction of PAHs, PCBs and phthalic acid esters. The components endow the composite with multiple characteristics such as adsorption capability and facile removal due to its magnetic properties. Due to the π-π electrostatic stacking property of graphene, the high specific surface area and the adsorption capability of both components, the resulting black flaky Fe(0)/iron oxide-oxyhydroxide/graphene composite showed high extraction efficiency for the target analytes from water samples. Compared with the neat graphene, the composite material has improved properties in terms of microextraction capabilities as both the hydrophobic graphene and zero-valent iron participate in the adsorption of the hydrophobic molecules. The precision from the extraction of all three groups of compounds was lower than 7% and the recoveries were from 90 to 93% from a spiked lake water sample. The high recoveries in relation to the low final volume of the desorption solvent ensure high preconcentration efficiency and a promising sorbent for analytical applications. Copyright © 2012 Elsevier B.V. All rights reserved.

Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

NASA Astrophysics Data System (ADS)

Omidi, Fariborz; Behbahani, Mohammad; Kalate Bojdi, Majid; Shahtaheri, Seyed Jamaleddin

2015-12-01

A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe3O4@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe3O4@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe3O4@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe3O4@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L-1 and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g-1. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results.

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

2015-05-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe3O4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L-1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml-1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results.

Flotation-separation of aluminum from some water samples using powdered marble waste and oleic acid.

PubMed

Ghazy, Shaban el-Sayed; Samra, Salem el-Sayed; Mahdy, Abd el-Fattah Mohammed; el-Morsy, Sherin Mohammed

2003-10-01

Bench-scale experiments were conducted in the laboratory, aiming to remove aluminum from water. They were based on the use of powdered marble wastes (PMW), which are inexpensive and produced in large quantity, and thus potentially cause environmental problems, as an effective inorganic sorbent and oleic acid (HOL) as surfactant. The main parameters (solution pHs, sorbent, surfactant and aluminum concentrations, shaking time, ionic strength and the presence of foreign ions) that influence the sorptive-flotation process were examined. Good results were obtained under the optimum conditions, for which nearly 100% of aluminum at pH 7 and at room temperature (approximately 25 degrees C) was removed. The procedure was successfully applied to the recovery of aluminum spiked to some natural water samples. Moreover, a sorption and flotation mechanism is suggested.

A novel magnetic poly(aniline-naphthylamine)-based nanocomposite for micro solid phase extraction of rhodamine B.

PubMed

Bagheri, Habib; Daliri, Rasoul; Roostaie, Ali

2013-09-10

A novel Fe3O4-poly(aniline-naphthylamine)-based nanocomposite was synthesized by chemical oxidative polymerization process as a magnetic sorbent for micro solid phase extraction. The scanning electron microscopy images of the synthesized nanocomposite revealed that the copolymer posses a porous structure with diameters less than 50nm. The extraction efficiency of this sorbent was examined by isolation of rhodamine B, a mutagenic and carcinogenic dye, from aquatic media in dispersion mode. Among different synthesized polymers, Fe3O4/poly(aniline-naphthylamine) nanocomposite showed a prominent efficiency. Parameters including the desorption solvent, amount of sorbent, desorption time, sample pH, ionic strength, extraction time and stirring rate were optimized. Under the optimum condition, a linear spiked calibration curve in the range of 0.35-5.00μgL(-1) with R(2)=0.9991 was obtained. The limits of detection (3Sb) and limits of quantification (10Sb) of the method were 0.10μgL(-1) and 0.35μgL(-1) (n=3), respectively. The relative standard deviation for water sample with 0.5μgL(-1) of RhB was 4.2% (n=5) and the absolute recovery was 92%. The method was applied for the determination of rhodamine B in dishwashing foam, dishwashing liquid, shampoo, pencil, matches tips and eye shadows samples and the relative recovery percentage were in the range of 94-99%. Copyright © 2013 Elsevier B.V. All rights reserved.

Matrix solid-phase dispersion followed by gas chromatography tandem mass spectrometry for the determination of benzotriazole UV absorbers in sediments.

PubMed

Carpinteiro, I; Abuín, B; Ramil, M; Rodríguez, I; Cela, R

2012-01-01

A cost-effective and low solvent consumption method, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six benzotriazole UV absorbers in sediments is presented. Sieved samples (0.5 g) were first mixed in a mortar with a solid sorbent and then transferred to a polypropylene syringe containing a layer of clean-up co-sorbent. Analytes were eluted with a suitable solvent and further determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Under final conditions, diatomaceous earth and silica, deactivated to 10%, were used as inert dispersant and clean-up co-sorbent, respectively. Analytes were recovered using just 5 mL of dichloromethane, and this extract was concentrated and exchanged to 1 mL of isooctane. Further removal of co-extracted sulphur was achieved adding activated copper powder to final extracts, which were stored overnight, before injection in the GC-MS/MS system. The accuracy of the method was assessed with river and marine sediment samples showing different carbon contents and spiked at different concentrations in the range from 40 to 500 ng g(-1). Recoveries varied between 78% and 110% with associated standard deviations below 14%. The limits of quantification of the method stayed between 3 and 15 ng g(-1). Levels of target compounds in sediment samples ranged from not detected up to a maximum of 56 ng g(-1) for Tinuvin 328.

Novel approach to microwave-assisted extraction and micro-solid-phase extraction from soil using graphite fibers as sorbent.

PubMed

Xu, Li; Lee, Hian Kee

2008-05-30

A single-step extraction-cleanup procedure involving microwave-assisted extraction (MAE) and micro-solid-phase extraction (micro-SPE) has been developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) from soil samples. Micro-SPE is a relatively new extraction procedure that makes use of a sorbent enclosed within a sealed polypropylene membrane envelope. In the present work, for the first time, graphite fiber was used as a sorbent material for extraction. MAE-micro-SPE was used to cleanup sediment samples and to extract and preconcentrate five PAHs in sediment samples prepared as slurries with addition of water. The best extraction conditions comprised of microwave heating at 50 degrees C for a duration of 20 min, and an elution (desorption) time of 5 min using acetonitrile with sonication. Using gas chromatography (GC)-flame ionization detection (FID), the limits of detection (LODs) of the PAHs ranged between 2.2 and 3.6 ng/g. With GC-mass spectrometry (MS), LODs were between 0.0017 and 0.0057 ng/g. The linear ranges were between 0.1 and 50 or 100 microg/g for GC-FID analysis, and 1 and 500 or 1000 ng/g for GC-MS analysis. Granular activated carbon was also used for the micro-SPE device but was found to be not as efficient in the PAH extraction. The MAE-micro-SPE method was successfully used for the extraction of PAHs in river and marine sediments, demonstrating its applicability to real environmental solid matrixes.

Dispersive micro-solid-phase extraction of benzoylurea insecticides in honey samples with a β-cyclodextrin-modified attapulgite composite as sorbent.

PubMed

Zhang, Panjie; Cui, Xiangqian; Yang, Xiaoling; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Lu, Runhua

2016-01-01

A β-cyclodextrin-modified attapulgite composite was prepared and used as a dispersive micro-solid-phase extraction sorbent for the determination of benzoylurea insecticides in honey samples. Parameters that may influence the extraction efficiency, such as the type and volume of the eluent, the amount of the sorbent, the extraction time and the ionic strength were investigated and optimized using batch and column procedures. Under optimized conditions, good linearity was obtained for all of the tested compounds, with R(2) values of at least 0.9834. The limits of detection were determined in the range of 0.2-1.0 μg/L. The recoveries of the four benzoylurea insecticides in vitex honey and acacia honey increased from 15.2 to 81.4% and from 14.2 to 82.0%, respectively. Although the β-cyclodextrin-modified attapulgite composite did not show a brilliant adsorption capacity for the selected benzoylurea insecticides, it exhibited a higher adsorption capacity toward relatively hydrophobic compounds, such as chlorfluazuron and hexaflumuron (recoveries in vitex honey samples ranged from 70.0 to 81.4% with a precision of 1.0-3.7%). It seemed that the logPow of the benzoylurea insecticides is related to their recoveries. The results confirmed the possibility of using cyclodextrin-modified palygorskite in the determination of relatively hydrophobic trace pharmaceutical residues. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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.

Cyclic carbonation calcination studies of limestone and dolomite for CO{sub 2} separation from combustion flue gases - article no. 011801

DOE Office of Scientific and Technical Information (OSTI.GOV)

Senthoorselvan, S.; Gleis, S.; Hartmut, S.

2009-01-15

Naturally occurring limestone and dolomite samples, originating from different geographical locations, were tested as potential sorbents for carbonation/calcination based CO{sub 2} capture from combustion flue gases. Samples have been studied in a thermogravimetric analyzer under simulated flue gas conditions at three calcination temperatures, viz., 750{sup o}C, 875{sup o}C, and 930{sup o}C for four carbonation calcination reaction (CCR) cycles. The dolomite sample exhibited the highest rate of carbonation than the tested limestones. At the third cycle, its CO{sub 2} capture capacity per kilogram of the sample was nearly equal to that of Gotland, the highest reacting limestone tested. At the fourthmore » cycle it surpassed Gotland, despite the fact that the CaCO{sub 3} content of the Sibbo dolomite was only 2/3 of that of the Gotland. Decay coefficients were calculated by a curve fitting exercise and its value is lowest for the Sibbo dolomite. That means, most probably its capture capacity per kilogram of the sample would remain higher well beyond the fourth cycle. There was a strong correlation between the calcination temperature, the specific surface area of the calcined samples, and the degree of carbonation. It was observed that the higher the calcination temperature, the lower the sorbent reactivity. For a given limestone/dolomite sample, sorbents CO{sub 2} capture capacity depended on the number of CCR cycles and the calcination temperature. According to the equilibrium thermodynamics, the CO{sub 2} partial pressure in the calciner should be lowered to lower the calcination temperature. This can be achieved by additional steam supply into the calciner. Steam could then be condensed in an external condenser to single out the CO{sub 2} stream from the exit gas mixture of the calciner. A calciner design based on this concept is illustrated.« less

CO2 Capture Using Electric Fields: Low-Cost Electrochromic Film on Plastic for Net-Zero Energy Building

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

2010-01-01

Broad Funding Opportunity Announcement Project: Two faculty members at Lehigh University created a new technique called supercapacitive swing adsorption (SSA) that uses electrical charges to encourage materials to capture and release CO2. Current CO2 capture methods include expensive processes that involve changes in temperature or pressure. Lehigh University’s approach uses electric fields to improve the ability of inexpensive carbon sorbents to trap CO2. Because this process uses electric fields and not electric current, the overall energy consumption is projected to be much lower than conventional methods. Lehigh University is now optimizing the materials to maximize CO2 capture and minimize themore » energy needed for the process.« less

Reactivity of Metal Oxide Sorbents for Removal of H{sub 2}S

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kwon, K.C.; Crowe, E.R.

1996-12-31

Removal of hydrogen sulfide contained in hot coal gases produced from integrated gasification combined cycle power generation systems is required to protect downstream combustion turbines from being corroded with sulfur compounds. Removal of sulfur compounds from hot coal gas products is investigated by using various metal oxide sorbents and membrane separation methods. The main requirements of these metal oxide sorbents are durability and high sulfur loading capacity during absorption-regeneration cycles. In this research, durable metal oxide sorbents were formulated. Reactivity of the formulated metal oxide sorbents with simulated coal gas mixtures was examined to search for an ideal sorbent formulationmore » with a high-sulfur loading capacity suitable for removal of hydrogen sulfide from coal gases. The main objectives of this research are to formulate durable metal oxide sorbents with high-sulfur loading capacity by a physical mixing method, to investigate reaction kinetics on the removal of sulfur compounds from coal gases at high temperature and pressure, to study reaction kinetics on the regeneration of sulfided sorbents, to identify effects of hydrogen partial pressures and moisture on equilibrium/dynamic absorption of hydrogen sulfide into formulated metal oxide sorbents as well as initial reaction rates of H{sub 2}S with formulated metal oxide sorbents, and to evaluate intraparticular diffusivity of H{sub 2}S into formulated sorbents at various reaction conditions. The metal oxide sorbents such as TU-1, TU-19, TU-24, TU-25 and TU-28 were formulated with zinc oxide powder as an active sorbent ingredient, bentonite as a binding material and titanium oxide as a supporting metal oxide.« less

Hydroxyapatite-based sorbents: elaboration, characterization and application for the removal of catechol from the aqueous phase.

PubMed

Sebei, Haroun; Pham Minh, Doan; Lyczko, Nathalie; Sharrock, Patrick; Nzihou, Ange

2017-10-01

Hydroxyapatite (HAP) is highly considered as good sorbent for the removal of metals from the aqueous phase. However, soluble metals co-exist with organic pollutants in wastewaters. But little work has been devoted to investigate the reactivity of HAP for the removal of organic compounds. The main objective of this work is to study the reactivity of HAP-based sorbents for the removal of catechol as a model organic pollutant from an aqueous solution. Thus, HAP sorbents were firstly synthesized using calcium carbonate and potassium dihydrogen phosphate under moderate conditions (25-80°C, atmospheric pressure). A zinc-doped HAP was also used as sorbent, which was obtained from the contact of HAP with an aqueous solution of zinc nitrate. All the sorbents were characterized by different standard physico-chemical techniques. The sorption of catechol was carried out in a batch reactor under stirring at room temperature and pressure. Zinc-doped HAP sorbent was found to be more reactive than non-doped HAP sorbents for the fixation of catechol. The highest sorption capacity was of 15 mg of C per gram of zinc-doped HAP sorbent. The results obtained suggest the reaction scheme of HAP sorbents with metals and organic pollutants when HAP sorbents were used for the treatment of complex wastewaters.

Characteristics and reactivity of rapidly hydrated sorbent for semidry flue gas desulfurization.

PubMed

Zhang, Jie; You, Changfu; Zhao, Suwei; Chen, Changhe; Qi, Haiying

2008-03-01

Semidry flue gas desulfurization with a rapidly hydrated sorbent was studied in a pilot-scale circulating fluidized bed (CFB) experimental facility. The desulfurization efficiency was measured for various operating parameters, including the sorbent recirculation rate and the water spray method. The experimental results show that the desulfurization efficiencies of the rapidly hydrated sorbent were 1.5-3.0 times higher than a commonly used industrial sorbent for calcium to sulfur molar ratios from 1.2 to 3.0, mainly due to the higher specific surface area and pore volume. The Ca(OH)2 content in the cyclone separator ash was about 2.9% for the rapidly hydrated sorbent and was about 0.1% for the commonly used industrial sorbent, due to the different adhesion between the fine Ca(OH)2 particles and the fly ash particles, and the low cyclone separation efficiency for the fine Ca(OH)2 particles that fell off the sorbent particles. Therefore the actual recirculation rates of the active sorbent with Ca(OH)2 particles were higher for the rapidly hydrated sorbent, which also contributed to the higher desulfurization efficiency. The high fly ash content in the rapidly hydrated sorbent resulted in good operating stability. The desulfurization efficiency with upstream water spray was 10-15% higher than that with downstream water spray.

Efficiency of malaise traps and colored pan traps for collecting flower visiting insects from three forested ecosystems

Treesearch

Joshua W. Campbell; J.L. Hanula

2007-01-01

Pan and Malaise traps have been used widely to sample insect abundance and diversity, but no studies have compared their performance for sampling pollinators in forested ecosystems. Malaise trap design and color of pan traps are important parameters that influence insect pollinator catches. We compared pan trap (blue, yellow, white, and red) and Malaise trap catches...

Solid-phase extraction sorbent consisting of alkyltrimethylammonium surfactants immobilized onto strong cation-exchange polystyrene resin.

PubMed

Reid, Kendra R; Kennedy, Lonnie J; Crick, Eric W; Conte, Eric D

2002-10-25

Presented is a solid-phase extraction sorbent material composed of cationic alkyltrimethylammonium surfactants attached to a strong cation-exchange resin via ion-exchange. The original hydrophilic cation-exchange resin is made hydrophobic by covering the surface with alkyl chains from the hydrophobic portion of the surfactant. The sorbent material now has a better ability to extract hydrophobic molecules from aqueous samples. The entire stationary phase (alkyltrimethylammonium surfactant) is removed along with the analyte during the elution step. The elution step requires a mild elution solvent consisting of 0.25 M Mg2+ in a 50% 2-propanol solution. The main advantage of using a removable stationary phase is that traditionally utilized toxic elution solvents such as methylene chloride, which are necessary to efficiently release strongly hydrophobic species from SPE stationary phases, may now be avoided. Also, the final extract is directly compatible with reversed-phase liquid chromatography. The performance of this procedure is presented using pyrene as a test molecule.

[The progress in speciation analysis of trace elements by atomic spectrometry].

PubMed

Wang, Zeng-Huan; Wang, Xu-Nuo; Ke, Chang-Liang; Lin, Qin

2013-12-01

The main purpose of the present work is to review the different non-chromatographic methods for the speciation analysis of trace elements in geological, environmental, biological and medical areas. In this paper, the sample processing methods in speciation analysis were summarized, and the main strategies for non-chromatographic technique were evaluated. The basic principles of the liquid extractions proposed in the published literatures recently and their advantages and disadvantages were discussed, such as conventional solvent extraction, cloud point extraction, single droplet microextraction, and dispersive liquid-liquid microextraction. Solid phase extraction, as a non-chromatographic technique for speciation analysis, can be used in batch or in flow detection, and especially suitable for the online connection to atomic spectrometric detector. The developments and applications of sorbent materials filled in the columns of solid phase extraction were reviewed. The sorbents include chelating resins, nanometer materials, molecular and ion imprinted materials, and bio-sorbents. Other techniques, e. g. hydride generation technique and coprecipitation, were also reviewed together with their main applications.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Magnetic adsorbents for the removal of Hg (II) and phenanthrene from aqueous solutions

NASA Astrophysics Data System (ADS)

Isari, Ekavi; Karapanagioti, Hrissi K.; Manariotis, Ioannis D.; Werner, David

2015-04-01

Activated carbon (AC) acts as a strong binding agent that lowers the pollutant concentration and, thus its toxicity. Another promising sorbent material in environmental applications is biochar (BC) which is obtained from the incomplete combustion of carbon-rich biomass under oxygen-limited conditions. Both of these materials could be used as soil or sediment amendments that would lower the toxicity in the aqueous phase. A draw back of this technique is that although the pollutant will remain non- bioavailable for many years being sorbed into these sorbents, it actually stays into the system. The objective of this study was (a) to synthesize a magnetic powdered activated carbon (AC/Fe) and magnetic powdered biochar (BC/Fe) produced from commercial AC1 and AC2 samples and biochar respectively and (b) to evaluate the potential use of AC/Fe and BIO/Fe to remove aqueous Hg (II) or phenanthrene while being magnetically recoverable. The BC was produced from olive pomace. The surface area, the pore volume, and the average pore size of each sorbent were determined using gas (N2) adsorption-desorption cycles and the Brunauer, Emmett, and Teller (BET) equation. Isotherms with 30 adsorption and 20 desorption points were conducted at liquid nitrogen temperature (77K). Open surface area and micropore volume were determined using t-plot method and Harkins & Jura equation. For both AC/Fe, surface area measurements resulted in 66% those of corresponding AC. For BC/Fe, the surface area was 82% that of BC. Batch experiments with all sorbent samples and mercury solutions were conducted at room temperature (25oC) and at pH 5 in order to compare the sorption properties of the materials. Similar tests were performed with phenanthrene solutions. Based on mercury isotherm data, AC/Fe and BC/Fe are effective sorbents but with lower sorption capacity compared to the initial materials (50-75% lower). All these properties point to promising materials that can effectively be used for in-situ environmental remediation and also be recovered.

Highly Attrition Resistant Zinc Oxide-Based Sorbents for H2S Removal by Spray Drying Technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ryu, C.K.; Lee, J.B.; Ahn, D.H.

2002-09-19

Primary issues for the fluidized-bed/transport reactor process are high attrition resistant sorbent, its high sorption capacity and regenerability, durability, and cost. The overall objective of this project is the development of a superior attrition resistant zinc oxide-based sorbent for hot gas cleanup in integrated coal gasification combined cycle (IGCC). Sorbents applicable to a fluidized-bed hot gas desulfurization process must have a high attrition resistance to withstand the fast solid circulation between a desulfurizer and a regenerator, fast kinetic reactions, and high sulfur sorption capacity. The oxidative regeneration of zinc-based sorbent usually initiated at greater than 600 C with highly exothermicmore » nature causing deactivation of sorbent as well as complication of sulfidation process by side reaction. Focusing on solving the sorbent attrition and regenerability of zinc oxide-based sorbent, we have adapted multi-binder matrices and direct incorporation of regeneration promoter. The sorbent forming was done with a spray drying technique that is easily scalable to commercial quantity.« less

Spatio-temporal optimization of sampling for bluetongue vectors (Culicoides) near grazing livestock

PubMed Central

2013-01-01

Background Estimating the abundance of Culicoides using light traps is influenced by a large variation in abundance in time and place. This study investigates the optimal trapping strategy to estimate the abundance or presence/absence of Culicoides on a field with grazing animals. We used 45 light traps to sample specimens from the Culicoides obsoletus species complex on a 14 hectare field during 16 nights in 2009. Findings The large number of traps and catch nights enabled us to simulate a series of samples consisting of different numbers of traps (1-15) on each night. We also varied the number of catch nights when simulating the sampling, and sampled with increasing minimum distances between traps. We used resampling to generate a distribution of different mean and median abundance in each sample. Finally, we used the hypergeometric distribution to estimate the probability of falsely detecting absence of vectors on the field. The variation in the estimated abundance decreased steeply when using up to six traps, and was less pronounced when using more traps, although no clear cutoff was found. Conclusions Despite spatial clustering in vector abundance, we found no effect of increasing the distance between traps. We found that 18 traps were generally required to reach 90% probability of a true positive catch when sampling just one night. But when sampling over two nights the same probability level was obtained with just three traps per night. The results are useful for the design of vector monitoring programmes on fields with grazing animals. PMID:23705770

A New Enzyme-linked Sorbent Assay (ELSA) to Quantify Syncytiotrophoblast Extracellular Vesicles in Biological Fluids.

PubMed

Göhner, Claudia; Weber, Maja; Tannetta, Dionne S; Groten, Tanja; Plösch, Torsten; Faas, Marijke M; Scherjon, Sicco A; Schleußner, Ekkehard; Markert, Udo R; Fitzgerald, Justine S

2015-06-01

The pregnancy-associated disease preeclampsia is related to the release of syncytiotrophoblast extracellular vesicles (STBEV) by the placenta. To improve functional research on STBEV, reliable and specific methods are needed to quantify them. However, only a few quantification methods are available and accepted, though imperfect. For this purpose, we aimed to provide an enzyme-linked sorbent assay (ELSA) to quantify STBEV in fluid samples based on their microvesicle characteristics and placental origin. Ex vivo placenta perfusion provided standards and samples for the STBEV quantification. STBEV were captured by binding of extracellular phosphatidylserine to immobilized annexin V. The membranous human placental alkaline phosphatase on the STBEV surface catalyzed a colorimetric detection reaction. The described ELSA is a rapid and simple method to quantify STBEV in diverse liquid samples, such as blood or perfusion suspension. The reliability of the ELSA was proven by comparison with nanoparticle tracking analysis. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Novel magnetic hollow zein nanoparticles for preconcentration of chlorpyrifos from water and soil samples prior to analysis via high-performance liquid chromatography (HPLC).

PubMed

Rahimi Moghadam, Mojtaba; Zargar, Behrooz; Rastegarzadeh, Saadat

2018-04-30

Herein, magnetically hollow zein nanoparticles were synthesized and used as a magnetic sorbent for the preconcentration of chlorpyrifos and its analysis by high-performance liquid chromatography (HPLC). Morphology of the sorbent was characterized by transmission electron microscopy (TEM). In this study, the effects of important parameters such as pH of the solution, adsorption and desorption time, type and volume of desorption solvent, and salt addition were investigated. Under optimized experimental conditions, the linear range was from 50 to 2000 μg mL-1, and an LOD of 25 μg L-1 was calculated. The relative standard deviations (RSD) varied from 3.8 to 5.1% (n = 5). The enrichment factors for 50 and 100 μg L-1 samples were calculated as 187 and 210, respectively. The developed method was successfully applied in soil and water samples and showed good extraction recoveries.

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

PubMed

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.

Sorbents for the oxidation and removal of mercur

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

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 sorbentmore » into the mercury contaminated gas stream are described.« less

Recovery of Rare Earths, Precious Metals and Other Critical Materials from Geothermal Waters with Advanced Sorbent Structures

DOE Data Explorer

Pamela M. Kinsey

2015-09-30

The work evaluates, develops and demonstrates flexible, scalable mineral extraction technology for geothermal brines based upon solid phase sorbent materials with a specific focus upon rare earth elements (REEs). The selected organic and inorganic sorbent materials demonstrated high performance for collection of trace REEs, precious and valuable metals. The nanostructured materials typically performed better than commercially available sorbents. Data contains organic and inorganic sorbent removal efficiency, Sharkey Hot Springs (Idaho) water chemsitry analysis, and rare earth removal efficiency from select sorbents.

Process and system for removing impurities from a gas

DOEpatents

Henningsen, Gunnar; Knowlton, Teddy Merrill; Findlay, John George; Schlather, Jerry Neal; Turk, Brian S

2014-04-15

A fluidized reactor system for removing impurities from a gas and an associated process are provided. The system includes a fluidized absorber for contacting a feed gas with a sorbent stream to reduce the impurity content of the feed gas; a fluidized solids regenerator for contacting an impurity loaded sorbent stream with a regeneration gas to reduce the impurity content of the sorbent stream; a first non-mechanical gas seal forming solids transfer device adapted to receive an impurity loaded sorbent stream from the absorber and transport the impurity loaded sorbent stream to the regenerator at a controllable flow rate in response to an aeration gas; and a second non-mechanical gas seal forming solids transfer device adapted to receive a sorbent stream of reduced impurity content from the regenerator and transfer the sorbent stream of reduced impurity content to the absorber without changing the flow rate of the sorbent stream.

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

DOEpatents

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.

Ultrafast and Stable CO2 Capture Using Alkali Metal Salt-Promoted MgO-CaCO3 Sorbents.

PubMed

Cui, Hongjie; Zhang, Qiming; Hu, Yuanwu; Peng, Chong; Fang, Xiangchen; Cheng, Zhenmin; Galvita, Vladimir V; Zhou, Zhiming

2018-06-20

As a potential candidate for precombustion CO 2 capture at intermediate temperatures (200-400 °C), MgO-based sorbents usually suffer from low kinetics and poor cyclic stability. Herein, a general and facile approach is proposed for the fabrication of high-performance MgO-based sorbents via incorporation of CaCO 3 into MgO followed by deposition of a mixed alkali metal salt (AMS). The AMS-promoted MgO-CaCO 3 sorbents are capable of adsorbing CO 2 at an ultrafast rate, high capacity, and good stability. The CO 2 uptake of sorbent can reach as high as above 0.5 g CO 2 g sorbent -1 after only 5 min of sorption at 350 °C, accounting for vast majority of the total uptake. In addition, the sorbents are very stable even under severe but more realistic conditions (desorption in CO 2 at 500 °C), where the CO 2 uptake of the best sorbent is stabilized at 0.58 g CO 2 g sorbent -1 in 20 consecutive cycles. The excellent CO 2 capture performance of the sorbent is mainly due to the promoting effect of molten AMS, the rapid formation of CaMg(CO 3 ) 2 , and the plate-like structure of sorbent. The exceptional ultrafast rate and the good stability of the AMS-promoted MgO-CaCO 3 sorbents promise high potential for practical applications, such as precombustion CO 2 capture from integrated gasification combined cycle plants and sorption-enhanced water gas shift process.

[Comparison of different sampling traps for Dermanyssus gallinae (Acari: Dermanyssidae) (de Geer, 1778)].

PubMed

Cunha, Lucas M; Cunha, Mariana M; Leite, Romário C; Silva, Israel J; Oliveira, Paulo R de

2009-01-01

This work aims to compare the performance of corrugated paper and "taquaril" bamboo (Phyllostachys sp.) straw traps for collecting (in sampling) Dermanyssus gallinae in a metal cages battery laying hens. The presence of eggs in the two trap models were compared using a Qui-square test and a proportion confidence interval test. Total daily values of mobile instars gathered in each type of trap were compared using the Wilcoxon's test. The amount of traps containing eggs was not different in neither of the traps (p < 0,05). The number of mobile instars sampled at every two days per trap model was different (p

Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

PubMed

Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

2016-09-15

Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria. Copyright © 2016 Elsevier Ltd. All rights reserved.

A novel aptamer-based online magnetic solid phase extraction method for the selective determination of 8-hydroxy-2'-deoxyguanosine in human urine.

PubMed

Gan, Haijiao; Xu, Hui

2018-05-30

In this work, an innovative magnetic aptamer adsorbent (Fe 3 O 4 -aptamer MNPs) was synthesized for the selective extraction of 8-hydroxy-2'-deoxyguanosine (8-OHdG). Amino-functionalized-Fe 3 O 4 was crosslinked with 8-OHdG aptamer by glutaraldehyde and fixed into a steel stainless tube as the sorbent of magnetic solid phase extraction (MSPE). After selective extraction by the aptamer adsorbent, the adsorbed 8-OHdG was desorbed dynamically and online analyzed by high performance liquid chromatography-mass spectrometry (HPLC-MS). The synthesized sorbent presented outstanding features, including specific selectivity, high enrichment capacity, stability and biocompatibility. Moreover, this proposed MSPE-HPLC-MS can achieve adsorption and desorption operation integration, greatly simplify the analysis process and reduce human errors. When compared with offline MSPE, a sensitivity enhancement of 800 times was obtained for the online method. Some experimental parameters such as the amount of the sorbent, sample flow rate and sample volume, were optimized systematically. Under the optimal conditions, low limit of detection (0.01 ng mL -1 , S/N = 3), limit of quantity (0.03 ng mL -1 , S/N = 10) and wide linear range with a satisfactory correlation coefficient (R 2  ≥ 0.9992) were obtained. And the recoveries of 8-OHdG in the urine samples varied from 82% to 116%. All these results revealed that the method is simple, rapid, selective, sensitive and automated, and it could be expected to become a potential approach for the selective determination of trace 8-OHdG in complex urinary samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Matrix solid-phase dispersion extraction followed by high performance liquid chromatography-diode array detection and ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometer method for the determination of the main compounds from Carthamus tinctorius L. (Hong-hua).

PubMed

Hong, Bo; Wang, Zhe; Xu, Tianjiao; Li, Chengchong; Li, Wenjing

2015-03-25

A simple and low-cost method based on matrix solid-phase dispersion (MSPD) extraction, HPLC separation, diode array detection and UPLC-Q-TOF-MS have been developed for the determination of Hydroxysafflor yellow A (HSYA), Kaempferol and other main compounds in Carthamus tinctorius. The experimental parameters that may affect the MSPD method, including dispersing sorbent, ratio of dispersing sorbent to sample, elution solvent, and volume of the elution solvent were examined and optimized. The optimized conditions were determined to be that silica gel was used as dispersing sorbent, the ratio of silica gel to sample mass was selected to be 3:1, and 10 mL of methanol: water (1:3, v:v) was used as elution solvent. The highest extraction yields of the two compounds were obtained under the optimized conditions. The method showed good linearity (r(2)≥0.999 2) and precision (RSD≤3.4%) for HSYA and Kaempferol, with the limits of detection of 35.2 and 14.5 ng mL(-1), respectively. The recoveries were in the range of 92.62-101.7% with RSD values ranging from 1.5 to 3.5%. At the meanwhile, there were 21 compounds in the extraction by MSPD method were identified by TOF-MS method to improve the quality control for safflower. Comparing to ultrasonic and soxhlet methods, the proposed MSPD procedure was more convenient and less time-consuming with reduced requirements on sample and solvent amounts. The proposed procedure was applied to analyze four real samples that were collected from different localities. Copyright © 2015 Elsevier B.V. All rights reserved.

Application of Nanofiber-packed SPE for Determination of Urinary 1-Hydroxypyrene Level Using HPLC.

PubMed

Ifegwu, Okechukwu Clinton; Anyakora, Chimezie; Chigome, Samuel; Torto, Nelson

2014-01-01

It is always desirable to achieve maximum sample clean-up, extraction, and pre-concentration with the minimum possible organic solvent. The miniaturization of sample preparation devices was successfully demonstrated by packing 10 mg of 11 electrospun polymer nanofibers into pipette tip micro column and mini disc cartridges for efficient pre-concentration of 1-hydroxypyrene in urine samples. 1-hydroxypyrene is an extensively studied biomarker of the largest class of chemical carcinogens. Excretory 1-hydroxypyrene was monitored with HPLC/fluorescence detector. Important parameters influencing the percentage recovery such as fiber diameter, fiber packing amount, eluent, fiber packing format, eluent volume, surface area, porosity, and breakthrough parameters were thoroughly studied and optimized. Under optimized condition, there was a near perfect linearity of response in the range of 1-1000 μg/L with a coefficient of determination (r (2)) between 0.9992 and 0.9999 and precision (% RSD) ≤7.64% (n = 6) for all the analysis (10, 25, and 50 μg/L). The Limit of detection (LOD) was between 0.022 and 0.15 μg/L. When compared to the batch studies, both disc packed nanofiber sorbents and pipette tip packed sorbents exhibited evident dominance based on their efficiencies. The experimental results showed comparable absolute recoveries for the mini disc packed fibers (84% for Nylon 6) and micro columns (80% for Nylon 6), although the disc displayed slightly higher recoveries possibly due to the exposure of the analyte to a larger reacting surface. The results also showed highly comparative extraction efficiencies between the nanofibers and conventional C-18 SPE sorbent. Nevertheless, miniaturized SPE devices simplified sample preparation, reducing back pressure, time of the analysis with acceptable reliability, selectivity, detection levels, and environmental friendliness, hence promoting green chemistry.

Nanofibers mat-based solid-phase extraction method for the pretreatment of urine samples and its application in the primary study on the disposition of nonylphenol after long-term low-level exposure in rats.

PubMed

Qian, Liangliang; Li, Ruixian; Di, Qiannan; Shen, Yang; Xu, Qian; Li, Jian

2017-09-01

A method was established for the analysis of nonylphenol (NP) in rat urine samples based on a solid-phase extraction (SPE) procedure with an amino functionalized polyacrylonitrile nanofibers mat (NH 2 -PAN NF S M) as sorbent coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The calibration curves prepared in three different days showed good linearity over a wide range of NP concentrations from 0.1 to 100.0ng/mL. It was remarkable that the proposed NH 2 -PAN NFsM based SPE method showed superior extraction efficiency with the consumption of only 4mg of sorbent and 500μL of eluent. The eluent without any further concentration was directly analyzed by HPLC-MS/MS. As a result, a simple and effective sample preparation was achieved. In addition, the notable lower detection limit (LOD) of 0.03ng/mL revealed the excellent sensitivity of the proposed method in comparison with that in literatures. The recoveries ranged from 85.0% to 114.8% with the relative standard deviations (RSDs) ranging from 7.5% to 13.7%, which were better than or comparable to those from the published methods, suggesting high accuracy of the proposed method. The proposed method was applied in primary study on the disposition of nonylphenol after long-term low-level exposure in rats, providing information for health risk assessment on the real scenarios of NP exposure. NH 2 -PAN NFsM shows great potential as a novel SPE sorbent for the analysis of biological samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Zeolite/iron oxide composite as sorbent for magnetic solid-phase extraction of benzene, toluene, ethylbenzene and xylenes from water samples prior to gas chromatography⬜mass spectrometry.

PubMed

Fernández, Elena; Vidal, Lorena; Canals, Antonio

2016-08-05

This study reports a new composite based on ZSM-5 zeolite decorated with iron oxide magnetic nanoparticles as a valuable sorbent for magnetic solid-phase extraction (MSPE). A proposal is made to determine benzene, toluene, ethylbenzene and xylenes (BTEX) as model analytes in water samples using gas chromatography-mass spectrometry. A two-step multivariate optimization strategy, using Plackett⬜Burman and circumscribed central composite designs, was employed to optimize experimental parameters affecting MSPE. The method was evaluated under optimized extraction conditions (i.e., amount of sorbent, 138mg; extraction time, 11min; sample pH, pH of water (i.e., 5.5⬜6.5); eluent solvent volume, 0.5mL; and elution time, 5min), obtaining a linear response from 1 to 100μgL(↙1) for benzene; from 10 to 100μgL(↙1) for toluene, ethylbenzene and o-xylene; and from 10 to 75μgL(↙1) for m,p-xylene. The repeatability of the proposed method was evaluated at a 40μgL(↙1) spiking level and coefficients of variation ranged between 8 and 11% (n=5). Limits of detection were found to be 0.3μgL(↙1) for benzene and 3μgL(↙1) for the other analytes. These values satisfy the current normative of the Environmental Protection Agency and European Union for BTEX content in waters for human consumption. Finally, drinking water, wastewater and river water were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 85% and 114% showing negligible matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

Chromium(III)-imprinted silica gel for speciation analysis of chromium in environmental water samples with ICP-MS detection.

PubMed

Zhang, Nan; Suleiman, Jibrin Sabo; He, Man; Hu, Bin

2008-04-15

A new chromium(III)-imprinted 3-(2-aminoethylamino) propyltrimethoxysilane (AAPTS)-functionalized silica gel sorbent was synthesized by a surface imprinting technique and was employed as a selective solid-phase extraction material for speciation analysis of chromium in environmental water samples prior to its determination by inductively coupled plasma mass spectrometry (ICP-MS). The prepared Cr(III)-imprinted silica gel shows the selectivity coefficient of more than 700 for Cr(III) in the presence of Mn(II). The static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cr(III) were 30.5 mg g(-1) and 13.4 mg g(-1). It was also found that Cr(VI) could be adsorbed at low pH by the prepared imprinted silica gel, and this finding makes it feasible to enrich and determine Cr(VI) at low pH without adding reducing reagents. The imprinted silica gel sorbent offered a fast kinetics for the adsorption and desorption of both chromium species. Under the optimized conditions, the detection limits of 4.43 pg mL(-1) and 8.30 pg mL(-1) with the relative standard deviations (R.S.D.s) of 4.44% and 4.41% (C=0.5 ng mL(-1), n=7) for Cr(III) and Cr(VI) were obtained, respectively. The proposed method was successfully applied to the speciation of trace chromium in environmental water samples. To validate the proposed method, two certified reference materials were analyzed and the determined values were in a good agreement with the certified values. The developed method is rapid, selective, sensitive and applicable for the speciation of trace chromium in environmental water samples.

Development of a procedure for the isolation and enrichment of modified nucleosides and nucleobases from urine prior to their determination by capillary electrophoresis-mass spectrometry.

PubMed

Rodríguez-Gonzalo, Encarnación; Hernández-Prieto, Raquel; García-Gómez, Diego; Carabias-Martínez, Rita

2014-01-01

A sample treatment step based on solid-phase extraction (SPE) with polymeric sorbents has been developed for the simultaneous isolation and preconcentration of nucleosides and nucleobases from urine prior to analyses by CE-ESI-MS. In most reported methods nucleosides are isolated from urine by SPE in affinity mode, using an immobilized phenylboronic acid group, which specifically binds cis-diols. However, this is not applicable to non-cis-diol compounds. Here, different types of polymeric sorbents were evaluated for the simultaneous extraction of nucleosides and nucleobases from urine. The best results were obtained with Isolute ENV+, a hydroxylated styrene-divylbenzene polymer, whose retention capacity can be attributed mainly to hydrophobic interactions, and thus it can be applied to a broad range of compounds, regardless of whether they present or not to the cis-diol group in their structure. Other parameters such as the elution solvent and sample volume were optimized. We also studied the influence of the addition of isotopically labeled internal standards (ILISs) before or after the extraction step. The detection limits achieved were in the 0.04-0.17μg/mL range for a sample size of 2.0mL and relative standard deviations were 4-22%. The whole method developed, SPE prior to CE-ESI-MS, was applied to human urine samples from healthy volunteers. We conclude that SPE with polymeric sorbents prior to the electrophoretic CE-ESI-MS methodology constitutes a fast, valid and reliable approach for the simultaneously extraction of urinary nucleosides and nucleobases. Copyright © 2013 Elsevier B.V. All rights reserved.

Point sources of emerging contaminants along the Colorado River Basin: Source water for the arid Southwestern United States

USGS Publications Warehouse

Jones-Lepp, Tammy L.; Sanchez, Charles; Alvarez, David A.; Wilson, Doyle C.; Taniguchi-Fu, Randi-Laurant

2012-01-01

Emerging contaminants (ECs) (e.g., pharmaceuticals, illicit drugs, personal care products) have been detected in waters across the United States. The objective of this study was to evaluate point sources of ECs along the Colorado River, from the headwaters in Colorado to the Gulf of California. At selected locations in the Colorado River Basin (sites in Colorado, Utah, Nevada, Arizona, and California), waste stream tributaries and receiving surface waters were sampled using either grab sampling or polar organic chemical integrative samplers (POCIS). The grab samples were extracted using solid-phase cartridge extraction (SPE), and the POCIS sorbents were transferred into empty SPEs and eluted with methanol. All extracts were prepared for, and analyzed by, liquid chromatography–electrospray-ion trap mass spectrometry (LC–ESI-ITMS). Log DOW values were calculated for all ECs in the study and compared to the empirical data collected. POCIS extracts were screened for the presence of estrogenic chemicals using the yeast estrogen screen (YES) assay. Extracts from the 2008 POCIS deployment in the Las Vegas Wash showed the second highest estrogenicity response. In the grab samples, azithromycin (an antibiotic) was detected in all but one urban waste stream, with concentrations ranging from 30 ng/L to 2800 ng/L. Concentration levels of azithromycin, methamphetamine and pseudoephedrine showed temporal variation from the Tucson WWTP. Those ECs that were detected in the main surface water channels (those that are diverted for urban use and irrigation along the Colorado River) were in the region of the limit-of-detection (e.g., 10 ng/L), but most were below detection limits.

Single solid phase extraction method for the simultaneous analysis of polar and non-polar pesticides in urine samples by gas chromatography and ultra high pressure liquid chromatography coupled to tandem mass spectrometry.

PubMed

Cazorla-Reyes, Rocío; Fernández-Moreno, José Luis; Romero-González, Roberto; Frenich, Antonia Garrido; Vidal, José Luis Martínez

2011-07-15

A new multiresidue method has been developed and validated for the simultaneous extraction of more than two hundred pesticides, including non-polar and polar pesticides (carbamates, organochlorine, organophosphorous, pyrethroids, herbicides and insecticides) in urine at trace levels by gas and ultra high pressure liquid chromatography coupled to ion trap and triple quadrupole mass spectrometry, respectively (GC-IT-MS/MS, UHPLC-QqQ-MS/MS). Non-polar and polar pesticides were simultaneously extracted from urine samples by a simple and fast solid phase extraction (SPE) procedure using C(18) cartridges as sorbent, and dichloromethane as elution solvent. Recovery was in the range of 60-120%. Precision values expressed as relative standard deviation (RSD) were lower than 25%. Identification and confirmation of the compounds were performed by the use of retention time windows, comparison of spectra (GC-amenable compounds) or the estimation of the ion ratio (LC-amenable compounds). For GC-amenable pesticides, limits of detection (LODs) ranged from 0.001 to 0.436 μg L(-1) and limits of quantification (LOQs) from 0.003 to 1.452 μg L(-1). For LC-amenable pesticides, LODs ranged from 0.003 to 1.048 μg L(-1) and LOQs ranged from 0.011 to 3.494 μg L(-1). Finally, the optimized method was applied to the analysis of fourteen real samples of infants from agricultural population. Some pesticides such as methoxyfenozide, tebufenozide, piperonyl butoxide and propoxur were found at concentrations ranged from 1.61 to 24.4 μg L(-1), whereas methiocarb sulfoxide was detected at trace levels in two samples. Copyright © 2011 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khare, G.P.; Delzer, G.A.; Kubicek, D.H.

Phillips Z-Sorb sorbents have been evaluated successfully as regenerable sorbents for hydrogen sulfide in the fuel gas that is produced in a clean coal technology power plant. Tests have been carried out in fixed-,moving-, and fluid-bed applications. The fixed-bed tests completed at the Morgantown Energy Technology Center showed that Phillips Z-Sorb sorbent performed better than zinc titanate. The performance of Phillips Z-Sorb sorbent in a moving-bed application was very encouraging. The sorbent flowed well, H{sub 2}S was reduced to less than 50 ppm at the absorber outlet over long periods and post-test analysis of the sorbent indicated very low sulfatemore » levels at the regenerator exit. The fluidizable version of Phillips Z-Sorb sorbent was tested in Research Triangle Institutes`s high temperature, high pressure, semi-bath, fluidized-bed reactor system. in a life cycle test consisting of 50 cycles of sulfidation and regeneration, this sorbent exhibited excellent activity and regenerability. The sulfur loading was observed to be 90 + percent of the theoretical capacity. The sorbent consistently demonstrated a sharp regeneration profile with no evidence of sulfate accumulation. 7 refs., 7 fig., 5 tabs.« less

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

NASA Technical Reports Server (NTRS)

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.

Synthesis and properties of nanostructured sol-gel sorbents for simultaneous removal of sulfur dioxide and nitrogen oxides from flue gas

NASA Astrophysics Data System (ADS)

Buelna Quijada, Genoveva

2001-07-01

Regenerative, alumina-supported, copper-based sorbent/catalysts provide a promising technique for simultaneous removal of SO2 and NO x from flue gas. These sorbents can remove over 90% of SO2 and 70+% of NOx while generating no wastes, reducing energy consumption, and producing valuable by-products. The lack of a cost-effective sorbent with low attrition rate and good reactivity has been the main hurdle to commercialization of this copper oxide process. Developing such a sorbent is the focus of this dissertation. This work examines using sol-gel techniques rather than traditional processes to produce gamma-alumina and copper coated 7-alumina granular sorbents. Important modifications to the established sol-gel synthesis process were made, which minimized generated wastes and reduced preparation time and sorbent cost. A laboratory scale semi-continuous process providing a basis for large-scale synthesis was developed. The effect of the copper content on the surface area and dispersion of the active species on sol-gel-derived sorbents coated by the one step and wet-impregnation methods was studied. The sol-gel-derived sorbents showed superior sulfation and regeneration properties than the existing commercial sorbents used in the copper oxide process in terms of sulfation capacity, fast regeneration, recovery of sorption capacity, and SO2 concentration in the regenerated effluent. The optimum temperature for NO reduction by NH3 over sol-gel-derived CuO/gamma-Al2O3 was found to be 350°C for both fresh and sulfated catalysts. This was also the optimum operating temperature for simultaneous removal of SO2 and NOx from simulated flue gas. At 350°C, the adsorption capacity of the sol-gel sorbent/catalyst was higher than UOP's sorbent, and very close to the capacity of ALCOA's sorbent, while the catalytic activity for NO reduction of the sol-gel-derived CuO/gamma-Al 2O3 sorbent fell between the commercial sorbents. The new mesoporous sol-gel-derived materials showed larger surface area, better mechanical strength, and more uniform dispersion of the copper species than existing commercially available sorbents. The superior mechanical properties, better cost effectiveness, and comparable efficiency for simultaneous removal of SO2 and NOx of the sol-gel-derived CuO/gamma-Al 2O3 sorbents with respect to the commercial ones make them a good option for use in the copper oxide process for combined removal of SO2 and NOx from flue gas.

Aerogel sorbents

DOEpatents

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.

Aerogel sorbents

DOEpatents

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

2016-04-05

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.

Use of biomass sorbents for oil removal from gas station runoff.

PubMed

Khan, Eakalak; Virojnagud, Wanpen; Ratpukdi, Thunyalux

2004-11-01

The use of biomass sorbents, which are less expensive and more biodegradable than synthetic sorbents, for oil removal from gas station runoff was investigated. A bench-scale flume experiment was conducted to evaluate the oil removal and retention capabilities of the biomass sorbents which included kapok fiber, cattail fiber, Salvinia sp., wood chip, rice husk, coconut husk, and bagasse. Polyester fiber, a commercial synthetic sorbent, was also experimented for comparison purpose. Oil sorption and desorption tests were performed at a water flow rate of 20 lmin-1. In the oil sorption tests, a 50 mgl(-1) of used engine oil-water mixture was synthesized to simulate the gas station runoff. The mass of oil sorbed for all sorbents, except coconut husk and bagasse, was greater than 70%. Cattail fiber and polyester fiber were the sorbents that provided the least average effluent oil concentrations. Oil selectivity (hydrophobic properties) and physical characteristics of the sorbents are the two main factors that influence the oil sorption capability. The used sorbents from the sorption tests were employed in the desorption tests. Results indicated that oil leached out of all the sorbents tested. Polyester fiber released the highest amount of oil, approximately 4% (mass basis) of the oil sorbed. copyright 2004 Elsevier Ltd.

Multicomponent gas sorption Joule-Thomson refrigeration

NASA Technical Reports Server (NTRS)

Jones, Jack A. (Inventor); Petrick, S. Walter (Inventor); Bard, Steven (Inventor)

1991-01-01

The present invention relates to a cryogenic Joule-Thomson refrigeration capable of pumping multicomponent gases with a single stage sorption compressor system. Alternative methods of pumping a multicomponent gas with a single stage compressor are disclosed. In a first embodiment, the sorbent geometry is such that a void is defined near the output of the sorption compressor. When the sorbent is cooled, the sorbent primarily adsorbs the higher boiling point gas such that the lower boiling point gas passes through the sorbent to occupy the void. When the sorbent is heated, the higher boiling point gas is desorbed at high temperature and pressure and thereafter propels the lower boiling point gas out of the sorption compressor. A mixing chamber is provided to remix the constituent gases prior to expansion of the gas through a Joule-Thomson valve. Other methods of pumping a multicomponent gas are disclosed. For example, where the sorbent is porous and the low boiling point gas does not adsorb very well, the pores of the sorbent will act as a void space for the lower boiling point gas. Alternatively, a mixed sorbent may be used where a first sorbent component physically adsorbs the high boiling point gas and where the second sorbent component chemically absorbs the low boiling point gas.

Analysis Study of Stevioside and Rebaudioside A from Stevia rebaudiana Bertoni by Normal Phase SPE and RP-HPLC

NASA Astrophysics Data System (ADS)

Martono, Y.; Rohman, A.; Riyanto, S.; Martono, S.

2018-04-01

Solid Phase Extraction (SPE) method using silica as sorbent for stevioside and rebaudiosida A analysis in Stevia rebaudiana Bertoni leaf have not been performed. The aim of this study is to develop SPE method using silica as sorbent for Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) analysis of stevioside and rebaudiosida A in S. rebaudiana leaf. The results of this study indicate that the optimal conditions for normal phase SPE (silica) are conditioned with 3.0 mL of hexane. The sample loading volume is 0.1 mL. Cartridge is eluted with 1.0 mL acetonitrile: water (80: 20, v/v) to separate both analytes. The cartridge is washed with chloroform and water of 0.3 mL respectively. The developed SPE sample preparation method meets the accuracy and precision test and can be used for the analysis of stevioside and rebaudioside A by RP-HPLC.

Chemically-modified activated carbon with ethylenediamine for selective solid-phase extraction and preconcentration of metal ions.

PubMed

Li, Zhenhua; Chang, Xijun; Zou, Xiaojun; Zhu, Xiangbing; Nie, Rong; Hu, Zheng; Li, Ruijun

2009-01-26

A new method that utilizes ethylenediamine-modified activated carbon (AC-EDA) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III), Fe(III), Hg(II) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The new sorbent was prepared by oxidative surface modification. Experimental conditions for effective adsorption of trace levels of Cr(III), Fe(III), Hg(II) and Pb(II) were optimized with respect to different experimental parameters using batch and column procedures in detail. The optimum pH value for the separation of metal ions simultaneously on the new sorbent was 4.0. Complete elution of absorbed metal ions from the sorbent surface was carried out using 3.0 mL of 2% (%w/w) thiourea and 0.5 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation and determination of target metal ions. The maximum static adsorption capacity of the sorbent at optimum conditions was found to be 39.4, 28.9, 60.5 and 49.9 mg g(-1) for Cr(III), Fe(III), Hg(II) and Pb(II), respectively. The time for 94% adsorption of target metal ions was less than 2 min. The detection limits of the method was found to be 0.28, 0.22, 0.09 and 0.17 ng mL(-1) for Cr(III), Fe(III), Hg(II) and Pb(II), respectively. The precision (R.S.D.) of the method was lower 4.0% (n=8). The prepared sorbent as solid-phase extractant was successfully applied for the preconcentration of trace Cr(III), Fe(III), Hg(II) and Pb(II) in natural and certified samples with satisfactory results.

EVALUATION OF SORBENTS FOR INDUSTRIAL SLUDGE LEACHATE TREATMENT

EPA Science Inventory

A laboratory and outdoor pilot-scale investigation was conducted on the use of selected sorbents for removing leachate contaminants from three industrial sludges. The laboratory results indicated that, rather than a single sorbent, a combination of acidic and basic sorbents is re...

Performance of a novel synthetic Ca-based solid sorbent suitable for desulfurizing flue gases in a fluidized bed

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pacciani, R.; Muller, C.R.; Davidson, J.F.

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 wasmore » 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.« less

The selective cleanup of complex matrices and simultaneous separation of benzo[a]pyrene by solid-phase extraction with MgO microspheres as sorbents.

PubMed

Jin, Jing; Li, Yun; Zhang, Zhiping; Su, Fan; Qi, Peipei; Lu, Xianbo; Chen, Jiping

2011-12-23

A new method for the selective cleanup of complex matrices and simultaneous separation of benzo[a]pyrene (BaP) was developed in this study. This method was based on solid-phase extraction (SPE) using magnesium oxide microspheres as sorbents, and it eliminated interferences from various impurities, such as lipids, sulphur, pigments, halobenzenes, polychlorodibenzo-p-dioxins and polychlorodibenzofurans. Several parameters, including the volume of rinsing and eluting solvents, the type of loading solvents and SPE sorbents, were optimized systematically. The capability for impurity removal was verified by gel permeation chromatography, gas chromatography, and liquid chromatography. Compared to commercial sorbents (silica gel, florisil and alumina), MgO microspheres exhibited excellent performance in the selective isolation of BaP and removal of impurities. The proposed method was applied to detect BaP in complex samples (sediments, soils, fish, and porcine liver). The limit of quantification (LOQ) was 1.04 ngL(-1), and the resulting regression coefficient (r(2)) was greater than 0.999 over a broad concentration range (9.5-7600 ngL(-1)). In contrast to traditional methods, the proposed method can give rise to higher recovery (85.1-100.8%) and better selectivity with simpler operation and less consumption of organic solvents (20-40 mL). Copyright © 2011 Elsevier B.V. All rights reserved.

Peat hybrid sorbents for treatment of wastewaters and remediation of polluted environment

NASA Astrophysics Data System (ADS)

Klavins, Maris; Burlakovs, Juris; Robalds, Artis; Ansone-Bertina, Linda

2015-04-01

For remediation of soils and purification of polluted waters, wastewaters, sorbents might be considered as an prospective group of materials and amongst them peat have a special role due to low cost, biodegradability, high number of functional groups, well developed surface area and combination of hydrophilic/hydrophobic structural elements. Peat as sorbent have good application potential for removal of trace metals, and we have demonstrated peat sorption capacities, sorption kinetics, thermodynamics in respect to metals with different valencies - Tl(I), Cu(II), Cr(III). However peat sorption capacity in respect to nonmetallic (anionic species) elements is low. Also peat mechanical properties do not support application in large scale column processes. To expand peat application possibilities the approach of biomass based hybrid sorbents has been elaborated. The concept "hybrid sorbent" in our understanding means natural, biomass based sorbent modified, covered with another sorbent material, thus combining two types of sorbent properties, sorbent functionalities, surface properties etc. As the "covering layer" both inorganic substances, mineral phases (iron oxohydroxides, oxyapatite) both organic polymers (using graft polymerization) were used. The obtained sorbents were characterised by their spectral properties, surface area, elemental composition. The obtained hybrid sorbents were tested for sorption of compounds in anionic speciation forms, for example of arsenic, antimony, tellurium and phosphorous compounds in comparison with weakly basic anionites. The highest sorption capacity was observed when peat sorbents modified with iron compounds were used. Sorption of different arsenic speciation forms onto iron-modified peat sorbents was investigated as a function of pH and temperature. It was established that sorption capacity increases with a rise in temperature, and the calculation of sorption process thermodynamic parameters indicates the spontaneity of sorption process and its endothermic nature. The recycling options of obtained compounds after their saturation with metal or non-metallic species are suggested. Acknowledgement: Support from a project 2014/0009/1DP/1.1.1.2.0/13/APIA/VIAA/044

Sampling small mammals in southeastern forests: the importance of trapping in trees

Treesearch

Susan C. Loeb; Gregg L. Chapman; Theodore R. Ridley

2001-01-01

Because estimates of small mammal species richness and diversity are strongly influenced by sampling methodology, 2 or more trap types are often used in studies of small mammal communities. However, in most cases, all traps are placed at ground level. In contrast, we used Sherman live traps placed at 1.5 m in trees in addition to Sherman live traps and Mosby box traps...

Space-filling polyhedral sorbents

DOEpatents

Haaland, Peter

2016-06-21

Solid sorbents, systems, and methods for pumping, storage, and purification of gases are disclosed. They derive from the dynamics of porous and free convection for specific gas/sorbent combinations and use space filling polyhedral microliths with facial aplanarities to produce sorbent arrays with interpenetrating interstitial manifolds of voids.

Circulating moving bed system for CO.sub.2 separation, and method of same

DOEpatents

Elliott, Jeannine Elizabeth; Copeland, Robert James

2016-12-27

A circulating moving bed and process for separating a carbon dioxide from a gas stream is disclosed. The circulating moving bed can include an adsorption reactor and a desorption reactor, and a sorbent that moves through the two reactors. The sorbent can enter the adsorptive reactor and one end and move to an exit point distal to its entry point, while a CO.sub.2 feed stream can enter near the distal point and move countercurrently through the sorbent to exit at a position near the entry point of the sorbent. The sorbent can adsorb the CO.sub.2 by concentration swing adsorption and adsorptive displacement. The sorbent can then transfer to a regeneration reactor and can move countercurrently against a flow of steam through the regeneration reactor. The sorbent can be regenerated and the carbon dioxide recaptured by desorbing the carbon dioxide from the sorbent using concentration swing desorption and desorptive displacement with steam.

Highly sensitive analysis of polycyclic aromatic hydrocarbons in environmental water with porous cellulose/zeolitic imidazolate framework-8 composite microspheres as a novel adsorbent coupled with high-performance liquid chromatography.

PubMed

Liang, Xiaotong; Liu, Shengquan; Zhu, Rong; Xiao, Lixia; Yao, Shouzhuo

2016-07-01

In this work, novel cellulose/zeolitic imidazolate frameworks-8 composite microspheres have been successfully fabricated and utilized as sorbent for environmental polycyclic aromatic hydrocarbons efficient extraction and sensitive analysis. The composite microspheres were synthesized through the in situ hydrothermal growth of zeolitic imidazolate frameworks-8 on cellulose matrix, and exhibited favorable hierarchical structure with chemical composition as assumed through scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction patterns, and Brunauer-Emmett-Teller surface areas characterization. A robust and highly efficient method was then successfully developed with as-prepared composite microspheres as novel solid-phase extraction sorbent with optimum extraction conditions, such as sorbent amount, sample volume, extraction time, desorption conditions, volume of organic modifier, and ionic strength. The method exhibited high sensitivity with low limit of detection down to 0.1-1.0 ng/L and satisfactory linearity with correlation coefficients ranging from 0.9988 to 0.9999, as well as good recoveries of 66.7-121.2% with relative standard deviations less than 10% for environmental polycyclic aromatic hydrocarbons analysis. Thus, our method was convenient and efficient for polycyclic aromatic hydrocarbons extraction and detection, potential for future environmental water samples analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Selective solid-phase extraction using a molecularly imprinted polymer for the analysis of patulin in apple-based foods.

PubMed

Lucci, Paolo; Moret, Sabrina; Bettin, Sara; Conte, Lanfranco

2017-01-01

The aim of this work was to evaluate the use of a molecularly imprinted polymer as a selective solid-phase extraction sorbent for the clean-up and pre-concentration of patulin from apple-based food products. Ultra high pressure liquid chromatography coupled to ultraviolet absorbance detection was used for the analysis of patulin. The molecularly imprinted polymer was applied, for the first time, to the determination of patulin in apple juice, puree and jam samples spiked within the maximum levels specified by the European Commission No. 1881/2006. High recoveries (>77%) were obtained. The method was validated and found to be linear in the range 2-100 μg/kg with correlation coefficients greater than 0.965 and repeatability relative standard deviation below 11% in all cases. Compared with dispersive solid-phase extraction (QuEChERS method) and octadecyl sorbent, the molecularly imprinted polymer showed higher recoveries and selectivity for patulin. The application of Affinisep molecularly imprinted polymer as a selective sorbent material for detection of patulin fulfilled the method performance criteria required by the Commission Regulation No. 401/2006, demonstrating the suitability of the technique for the control of patulin at low ppb levels in different apple-based foods such as juice, puree and jam samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

DOEpatents

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.

Method of burning sulfur-containing fuels in a fluidized bed boiler

DOEpatents

Jones, Brian C.

1982-01-01

A method of burning a sulfur-containing fuel in a fluidized bed of sulfur oxide sorbent wherein the overall utilization of sulfur oxide sorbent is increased by comminuting the bed drain solids to a smaller average particle size, preferably on the order of 50 microns, and reinjecting the comminuted bed drain solids into the bed. In comminuting the bed drain solids, particles of spent sulfur sorbent contained therein are fractured thereby exposing unreacted sorbent surface. Upon reinjecting the comminuted bed drain solids into the bed, the newly-exposed unreacted sorbent surface is available for sulfur oxide sorption, thereby increasing overall sorbent utilization.

Reactivity of metal oxide sorbents for removal of sulfur compounds from coal gases at high temperature and pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kwon, K.C.; Crowe, E.R.; Gangwal, S.K.

1997-01-01

Hot-gas desulfurization for the integrated gasification combined cycle (IGCC) process has been investigated to effectively remove hydrogen sulfide with various metal oxide sorbents at high temperatures and pressures. Metal oxide sorbents such as zinc titanate oxide, zinc ferrite oxide, copper oxide, manganese oxide and calcium oxide were found to be promising sorbents in comparison with other removal methods such as membrane separation and reactive membrane separation. The removal reaction of H{sub 2}S from coal gas mixtures with zinc titanate oxide sorbents was conducted in a batch reactor. The main objectives of this research are to formulate promising metal oxide sorbentsmore » for removal of hydrogen sulfide from coal gas mixtures, to compare reactivity of a formulated sorbent with a sorbent supplied by the Research Triangle Institute at high temperatures and pressures, and to determine effects of concentrations of moisture contained in coal gas mixtures on equilibrium absorption of H{sub 2}S into metal oxide sorbents. Promising durable metal oxide sorbents with high-sulfur-absorbing capacity were formulated by mixing active metal oxide powders with inert metal oxide powders and calcining these powder mixtures.« less

Tc-99 Decontamination From Heat Treated Gaseous Diffusion Membrane -Phase I

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L.; Wilmarth, B.; Restivo, M.

2017-03-13

Uranium gaseous diffusion cascades represent a significant environmental challenge to dismantle, containerize and dispose as low-level radioactive waste. Baseline technologies rely on manual manipulations involving direct access to technetium-contaminated piping and materials. There is a potential to utilize novel thermal decontamination technologies to remove the technetium and allow for on-site disposal of the very large uranium converters. Technetium entered these gaseous diffusion cascades as a hexafluoride complex in the same fashion as uranium. Technetium, as the isotope Tc-99, is an impurity that follows uranium in the first cycle of the Plutonium and Uranium Extraction (PUREX) process. The technetium speciation ormore » exact form in the gas diffusion cascades is not well defined. Several forms of Tc-99 compounds, mostly the fluorinated technetium compounds with varying degrees of volatility have been speculated by the scientific community to be present in these cascades. Therefore, there may be a possibility of using thermal desorption, which is independent of the technetium oxidation states, to perform an in situ removal of the technetium as a volatile species and trap the radionuclide on sorbent traps which could be disposed as low-level waste.« less

Identification and quantification of volatile organic compounds using systematic single-ion chromatograms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsuchiya, Yoshio; Kanabus-Kaminska, J.M.

1996-12-31

In order to determine the background level of volatile organic compounds (VOCs) in Canadian indoor air, a method of identification and quantification at a level of 0.3 {micro}g/m{sup 3} using systematic single-ion chromatograms (SICs) has been developed. The compounds selected for measurement included several halogenated compounds, oxygen compounds, terpenes, and C8 to C16 n-alkanes. Air samples were taken in 3-layered sorbent tubes and trapped compounds were thermally desorbed into the helium stream of a gas chromatograph/mass spectrometer (GC/MS) analytical system. Total quantities of volatile organic compounds (TVOCs) were measured using a flame ionization detector (FID). Individual compounds were analyzed bymore » a GC/MS. For the identification of compounds in the main stream GC effluent, both the specific GC retention and mass spectra were used. About 50 selected SICs were routinely extracted from a total ion chromatogram (TIC) to detect and quantify compounds. For each compound, a single representative ion was selected. The specific retention was calculated from the elution time on the SIC. For quantification, ion counts under a peak in the SIC were measured. The single-ion MS response factor for some of the compounds was experimentally determined using a dynamic reference procedure.« less

New Sorbents for Removing Arsenic From Water

NASA Astrophysics Data System (ADS)

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 concentration in leachate water from 35 mg/L to less than 0.005 mg/L; the concentrations of trace metals were also lowered to environmentally acceptable levels and leachate acidity was neutralized. Arsenic concentrations in the leachate water have remained below 0.005 mg/L for the four years since the treatment was carried out and the concentrations of trace metals have remained well below regulatory limits. In another example, the use of BauxsolT blended with a small amount of jarosite successfully reduced the total arsenic concentration in an industrial processing water from 16.4 mg/L to less than 0.001 mg/L; the treatment also reduced the concentrations of Cd, Cr, Ni, Pb and Zn to environmentally acceptable values. In a final example, activated BauxsolT used in simple flow through columns reduced the arsenic concentration in potable water from about 2 mg/L to less than 0.001 mg/L. In all three trials the spent BauxsolT residue released almost no arsenic in a TCLP leaching test and easily met the criteria for classification as an inert solid so that there were no special requirements for the disposal of water treatment residues. In all three studies the BauxsolT-based products compared very favorably with other more costly sorbents that are available.

Selective removal of 2,4-dichlorophenoxyacetic acid from water by molecularly-imprinted amino-functionalized silica gel sorbent.

PubMed

Han, Deman; Jia, Wenping; Liang, Huading

2010-01-01

A molecularly-imprinted amino-functionalized sorbent for selective removal of 2,4-dichlorophenoxyacetic acid (2,4-D) was prepared by a surface imprinting technique in combination with a sol-gel process. The 2,4-D-imprinted amino-functionalized silica sorbent was characterized by FT-IR, nitrogen adsorption and static adsorption experiments. The selectivity of the sorbent was investigated by a batch competitive binding experiment using an aqueous 2,4-D and 2,4-dichlorophenol (2,4-DCP) mixture or using an aqueous 2,4-D and 2,4-dichlorophenylacetic acid (DPAC) mixture. The largest selectivity coefficient for 2,4-D in the presence of 2,4-DCP was found to be over 18, the largest relative selectivity coefficient between 2,4-D and 2,4-DCP over 9. The static uptake capacity and selectivity coefficient of the 2,4-D-imprinted functionalized sorbent are higher than those of the non-imprinted sorbent. The imprinted functionalized silica gel sorbent offered a fast kinetics for the extraction/stripping of 2,4-D, 73% of binding capacity (200 mg/L 2,4-D onto 20 mg of imprinted sorbent) was obtained within 5 min and the adsorbed 2,4-D can be easily stripped by the mixture solution of ethanol and 6 mol/L HCl (V:V = 1:1). In a test of five extraction/stripping cycles, the adsorption capacity of the sorbent was all above 93% of that of the fresh sorbent. Experimental result showed the potential of molecularly-imprinted amino-functionalized sorbent for selective removal of 2,4-D.

Trapping of Individual Airborne Absorbing Particles Using a Counterflow Nozzle and Photophoretic Trap for Continuous Sampling and Analysis

DTIC Science & Technology

2014-03-19

particles from air. The key parts of the system are a conical photophoretic optical trap and a counter-flow coaxial-double- nozzle that concentrates and then...distribution is unlimited. Trapping of individual airborne absorbing particles using a counterflow nozzle and photophoretic trap for continuous...airborne absorbing particles using a counterflow nozzle and photophoretic trap for continuous sampling and analysis Report Title We describe an

Carbon sorbent based on flax boon

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abramov, M.V.; Tyulina, R.M.; Yaroslavtsev, V.T.

1994-11-10

Flax-fiber production wastes such as boon can be used effectively as the starting material for producing carbon sorbents. Activated carbons are among the most widely used sorbents in industrial wastewater and waste gas treatment. A single-stage process has been developed for producing an efficient, cheap carbon sorbent based on flax boon.

Regenerable solid imine sorbents

DOEpatents

Gray, McMahan; Champagne, Kenneth J.; Fauth, Daniel; Beckman, Eric

2013-09-10

Two new classes of amine-based sorbents are disclosed. The first class comprises new polymer-immobilized tertiary amine sorbents; the second class new polymer-bound amine sorbents. Both classes are tailored to facilitate removal of acid anhydrides, especially carbon dioxide (CO.sub.2), from effluent gases. The amines adsorb acid anhydrides in a 1:1 molar ratio. Both classes of amine sorbents adsorb in the temperature range from about 20.degree. C. upwards to 90.degree. C. and can be regenerated by heating upwards to 100.degree. C.

Sulfur tolerant highly durable CO.sub.2 sorbents

DOEpatents

Smirniotis, Panagiotis G [Cincinnati, OH; Lu, Hong [Urbana, IL

2012-02-14

A sorbent for the capture of carbon dioxide from a gas stream is provided, the sorbent containing calcium oxide (CaO) and at least one refractory dopant having a Tammann temperature greater than about 530.degree. C., wherein the refractory dopant enhances resistance to sintering, thereby conserving performance of the sorbent at temperatures of at least about 530.degree. C. Also provided are doped CaO sorbents for the capture of carbon dioxide in the presence of SO.sub.2.

Application of zirconium dioxide nanoparticle sorbent for the clean-up step in post-harvest pesticide residue analysis.

PubMed

Uclés, Ana; Herrera López, Sonia; Dolores Hernando, Maria; Rosal, Roberto; Ferrer, Carmen; Fernández-Alba, Amadeo R

2015-11-01

The use of yttria-stabilized zirconium dioxide nanoparticles as d-SPE clean-up sorbent for a rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the determination of post-harvest fungicides (carbaryl, carbendazim, chlorpropham, diphenylamine, ethoxyquin, flutriafol, imazalil, iprodione, methomyl, myclobutanil, pirimiphos-methyl, prochloraz, pyrimethanil, thiabendazole, thiophanate-methyl and tolclofos-methyl) in orange and pear samples has been evaluated and validated. The sample preparation was a modification of the QuEChERS extraction method using yttria-stabilized zirconium dioxide and multi-walled carbon nanotubes (MWCNTs) nanoparticles as the solid phase extraction (d-SPE) clean-up sorbents prior to injecting the ten-fold diluted extracts into the LC system. By using the yttria-stabilized zirconium dioxide extraction method, more recoveries in the 70-120% range were obtained - thus this method was used for the validation. Quantification was carried out using a matrix-matched calibration curve which was linear in the 1-500 µg kg(-1) range for almost all the pesticides studied. The validated limit of quantification was 10 µg kg(-1) for most of the studied compounds, except chlorpropham, ethoxyquin and thiophanate-methyl. Pesticide recoveries at the 10 and 100 µg kg(-1) concentration levels were satisfactory, with values between 77% and 120% and relative standard deviations (RSD) lower than 10% (n=5). The developed method was applied for the determination of selected fungicides in 20 real orange and pear samples. Four different pesticide residues were detected in 10 of these commodities; 20% of the samples contained pesticide residues at a quantifiable level (equal to or above the LOQs) for at least one pesticide residue. The most frequently-detected pesticide residues were: carbendazim, thiabendazole and imazalil-all were below the MRL. The highest concentration found was imazalil at 1175 µg kg(-1) in a pear sample. Copyright © 2015 Elsevier B.V. All rights reserved.

A comparison of solids collected in sediment traps and automated water samplers

USGS Publications Warehouse

Bartsch, L.A.; Rada, R.G.; Sullivan, J.F.

1996-01-01

Sediment traps are being used in some pollution monitoring programs in the USA to sample suspended solids for contaminant analyses. This monitoring approach assumes that the characteristics of solids obtained in sediment traps are the same as those collected in whole-water sampling devices. We tested this assumption in the upper Mississippi River, based on the inorganic particle-size distribution (determined with a laser particle- analyzer) and volatile matter content of solids (a surrogate for organic matter). Cylindrical sediment traps (aspect ratio 3) were attached to a rigid mooring device and deployed in a flowing side channel in Navigation Pool 7 of the upper Mississippi River. On each side of the mooring device, a trap was situated adjacent to a port of an autosampler that collected raw water samples hourly to form 2-d composite samples. Paired samples (one trap and one raw water, composite sample) were removed from each end of the mooring device at 2-d intervals during the 30-d study period and compared. The relative particle collection efficiency of paired samplers did not vary temporally. Particle-size distributions of inorganic solids from sediment traps and water samples were not significantly different. The volatile matter content of solids was lesser in sediment traps (mean, 9.5%) than in corresponding water samples (mean, 22.7%). This bias may have been partly due to under-collection of phytoplankton (mainly cyanobacteria), which were abundant in the water column during the study. The positioning of water samplers and sediment traps in the mooring device did not influence the particle-size distribution or total solids of samples. We observed a small difference in the amount of organic matter collected by water samplers situated at opposite ends of the mooring device.

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

NASA Technical Reports Server (NTRS)

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.

New materials for solid-phase extraction and multiclass high-performance liquid chromatographic analysis of pesticides in grapes.

PubMed

Melo, Lucio F C; Collins, Carol H; Jardim, Isabel C S F

2004-04-02

Sample preparation procedures which included the use of new aminopropyl (NH2) and octadecyl (C18) solid-phase extraction (SPE) sorbents are proposed for the simultaneous multiclass determination of the fungicide benomyl and of the herbicides tebuthiuron, diuron, simazine, atrazine, and ametryn in grapes, using single wavelength high-performance liquid chromatography. Sorbent preparation uses a fast, easy, and effective procedure to obtain silica-based materials, made by depositing polysiloxanes on a silica support followed by thermal immobilization. Recovery results of the compounds, after elution from the SPE cartridges, indicate that the most efficient system employed silica loaded with 40% of an aminofunctional polydimethylsiloxane as sorbent, using dichloromethane:methanol (95:5, v/v) as eluent. Method validation, carried out in agreement with International Conference on Harmonization directives, was performed at three fortification levels (100, 200, and 1000 microg kg(-1)). Limits of detection and quantification show that the method developed can be used to detect the pesticides at concentrations below the maximum residue levels established by Codex Alimentarius, the US Environmental Protection Agency, the European Union, and Brazilian legislation.

Hydrogen sulfide capture by limestone and dolomite at elevated pressure. 2: Sorbent particle conversion modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zevenhoven, C.A.P.; Yrjas, K.P.; Hupa, M.M.

1996-03-01

The physical structure of a limestone or dolomite to be used in in-bed sulfur capture in fluidized bed gasifiers has a great impact on the efficiency of sulfur capture and sorbent use. In this study an unreacted shrinking core model with variable effective diffusivity is applied to sulfidation test data from a pressurized thermogravimetric apparatus (P-TGA) for a set of physically and chemically different limestone and dolomite samples. The particle size was 250--300 {micro}m for all sorbents, which were characterized by chemical composition analysis, particle density measurement, mercury porosimetry, and BET internal surface measurement. Tests were done under typical conditionsmore » for a pressurized fluidized-bed gasifier, i.e., 20% CO{sub 2}, 950 C, 20 bar. At these conditions the limestone remains uncalcined, while the dolomite is half-calcined. Additional tests were done at low CO{sub 2} partial pressures, yielding calcined limestone and fully calcined dolomite. The generalized model allows for determination of values for the initial reaction rate and product layer diffusivity.« less

Critical evaluation and comparison of enrichment efficiency of multi-walled carbon nanotubes, C18 silica and activated carbon towards some pesticides from environmental waters.

PubMed

El-Sheikh, Amjad H; Sweileh, Jamal A; Al-Degs, Yahya S; Insisi, Ahmad A; Al-Rabady, Nancy

2008-02-15

In this work, optimization of multi-residue solid phase extraction (SPE) procedures coupled with high-performance liquid chromatography for the determination of Propoxur, Atrazine and Methidathion from environmental waters is reported. Three different sorbents were used in this work: multi-walled carbon nanotubes (MWCNTs), C18 silica and activated carbon (AC). The three optimized SPE procedures were compared in terms of analytical performance, application to environmental waters, cartridge re-use, adsorption capacity and cost of adsorbent. Although the adsorption capacity of MWCNT was larger than AC and C18, however, the analytical performance of AC could be made close to the other sorbents by appropriate optimization of the SPE procedures. A sample of AC was then oxidized with various oxidizing agents to show that ACs of various surface properties has different enrichment efficiencies. Thus researchers are advised to try AC of various surface properties in SPE of pollutants prior to using expensive sorbents (such as MWCNT and C18 silica).

Phytic acid-stabilized super-amphiphilic Fe3O4-graphene oxide for extraction of polycyclic aromatic hydrocarbons from vegetable oils.

PubMed

Ji, Wenhua; Zhang, Mingming; Duan, Wenjuan; Wang, Xiao; Zhao, Hengqiang; Guo, Lanping

2017-11-15

Phytic acid-stabilized Fe 3 O 4 -graphene oxide (GOPA@Fe 3 O 4 ) was assembled by microwave-enhanced hydrothermal synthesis and super-amphipathicity was demonstrated by measurement of dynamic oil and water contact angles. GOPA@Fe 3 O 4 was used as a sorbent for enrichment of eight polycyclic aromatic hydrocarbons (PAHs) from vegetable oils by magnetic solid-phase extraction (MSPE). The extraction-desorption factors were systematically investigated and, under optimum conditions, the super-amphiphilic sorbent achieved wide linear ranges (0.2-200ngg -1 ), satisfactory precision (3.44-6.64% for intra-day and 5.39-8.41% for inter-day) and low limits of detection (LODs, 0.06-0.15ngg -1 ) for PAHs. Excellent recoveries (85.6-102.3%) for spiked PAHs were obtained with genuine vegetable oil samples. These results indicate that MSPE using GOPA@Fe 3 O 4 as the sorbent, coupled with high performance liquid chromatography (HPLC), is an efficient and simple method for the detection of low concentrations of PAHs in vegetable oils. Copyright © 2017 Elsevier Ltd. All rights reserved.

Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

PubMed

Muhamad, Halimah; Zainudin, Badrul Hisyam; Abu Bakar, Nor Kartini

2012-10-15

Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia. Copyright © 2012 Elsevier Ltd. All rights reserved.

Sorbents with high efficiency for CO2 capture based on amines-supported carbon for biogas upgrading.

PubMed

Pino, Lidia; Italiano, Cristina; Vita, Antonio; Fabiano, Concetto; Recupero, Vincenzo

2016-10-01

Sorbents for CO 2 capture have been prepared by wet impregnation of a commercial active carbon (Ketjen-black, Akzo Nobel) with two CO 2 -philic compounds, polyethylenimine (PEI) and tetraethylenepentamine (TEPA), respectively. The effects of amine amount (from 10 to 70wt.%), CO 2 concentration in the feed, sorption temperature and gas hourly space velocity on the CO 2 capture performance have been investigated. The sorption capacity has been evaluated using the breakthrough method, with a fixed bed reactor equipped with on line gas chromatograph. The samples have been characterized by N 2 adsorption-desorption, scanning electron microscopy and energy dispersive X-ray (SEM/EDX). A promising CO 2 sorption capacity of 6.90 mmol/g sorbent has been obtained with 70wt.% of supported TEPA at 70°C under a stream containing 80vol% of CO 2 . Sorption tests, carried out with simulated biogas compositions (CH 4 /CO 2 mixtures), have revealed an appreciable CO 2 separation selectivity; stable performance was maintained for 20 adsorption-desorption cycles. Copyright © 2016. Published by Elsevier B.V.

CO2 Capacity Sorbent Analysis Using Volumetric Measurement Approach

NASA Technical Reports Server (NTRS)

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.

Toward in situ monitoring of water contamination by nitroenergetic compounds.

PubMed

Johnson, Brandy J; Leska, Iwona A; Medina, Alejandro; Dyson, Norris F; Nasir, Mansoor; Melde, Brian J; Taft, Jenna R; Charles, Paul T

2012-11-06

We have previously described the application of novel porous organosilicate materials to the preconcentration of nitroenergetic targets from aqueous solution prior to HPLC analysis. The performance of the sorbents and the advantages of these types of materials over commercially available solid phase extraction sorbents have been demonstrated. Here, the development of systems for application of those sorbents to in situ monitoring is described. Considerations such as column pressure, particulate filtration, and component durability are discussed. The diameter of selected column housings, the sorbent bed depth, and the frits utilized significantly impact the utility of the sorbent columns in the prototype system. The impact of and necessity for improvements in the morphological characteristics of the sorbents as they relate to reduction in column pressure are detailed. The results of experiments utilizing a prototype system are presented. Data demonstrating feasibility for use of the sorbents in preconcentration prior to ion mobility spectrometry is also presented.

CO2 Capacity Sorbent Analysis Using Volumetric Measurement Approach

NASA Technical Reports Server (NTRS)

Huang, Roger; Richardson, Tra-My Justine; Belancik, Grace; Jan, Darrell; Knox, James; Cmarik, Gregory E.; Ebner, Armin; Ritter, James

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 0 C, 10 C, 25 C, 50 C, and 75 C 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.

Method of removing hydrogen sulfide from gases utilizing a zinc oxide sorbent and regenerating the sorbent

DOEpatents

Jalan, Vinod M.; Frost, David G.

1984-01-01

A spent solid sorbent resulting from the removal of hydrogen sulfide from a fuel gas flow is regenerated with a steam-air mixture. The mixture of steam and air may also include additional nitrogen or carbon dioxide. The gas mixture contacts the spent sorbent containing metal sulfide at a temperature above 500.degree. C. to regenerate the sulfide to metal oxide or carbonate. Various metal species including the period four transition metals and the lanthanides are suitable sorbents that may be regenerated by this method. In addition, the introduction of carbon dioxide gas permits carbonates such as those of strontium, barium and calcium to be regenerated. The steam permits regeneration of spent sorbent without formation of metal sulfate. Moreover, the regeneration will proceed with low oxygen concentrations and will occur without the increase in temperature to minimize the risk of sintering and densification of the sorbent.

A semi-automatic microextraction in packed sorbent, using a digitally controlled syringe, combined with ultra-high pressure liquid chromatography as a new and ultra-fast approach for the determination of prenylflavonoids in beers.

PubMed

Gonçalves, João L; Alves, Vera L; Rodrigues, Fátima P; Figueira, José A; Câmara, José S

2013-08-23

In this work a highly selective and sensitive analytical procedure based on semi-automatic microextraction by packed sorbents (MEPS) technique, using a new digitally controlled syringe (eVol(®)) combined with ultra-high pressure liquid chromatography (UHPLC), is proposed to determine the prenylated chalcone derived from the hop (Humulus lupulus L.), xanthohumol (XN), and its isomeric flavonone isoxanthohumol (IXN) in beers. Extraction and UHPLC parameters were accurately optimized to achieve the highest recoveries and to enhance the analytical characteristics of the method. Important parameters affecting MEPS performance, namely the type of sorbent material (C2, C8, C18, SIL, and M1), elution solvent system, number of extraction cycles (extract-discard), sample volume, elution volume, and sample pH, were evaluated. The optimal experimental conditions involves the loading of 500μL of sample through a C18 sorbent in a MEPS syringe placed in the semi-automatic eVol(®) syringe followed by elution using 250μL of acetonitrile (ACN) in a 10 extractions cycle (about 5min for the entire sample preparation step). The obtained extract is directly analyzed in the UHPLC system using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and ACN (eluent B) in the gradient elution mode (10min total analysis). Under optimized conditions good results were obtained in terms of linearity within the established concentration range with correlation coefficients (R) values higher than 0.986, with a residual deviation for each calibration point below 12%. The limit of detection (LOD) and limit of quantification (LOQ) obtained were 0.4ngmL(-1) and 1.0ngmL(-1) for IXN, and 0.9ngmL(-1) and 3.0ngmL(-1) for XN, respectively. Precision was lower than 4.6% for IXN and 8.4% for XN. Typical recoveries ranged between 67.1% and 99.3% for IXN and between 74.2% and 99.9% for XN, with relative standard deviations %RSD no larger than 8%. The applicability of the proposed analytical procedure in commercial beers, revealed the presence of both target prenylchalcones in all samples being IXN the most abundant with concentration of between 0.126 and 0.200μgmL(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Attrition resistant, zinc titanate-containing, reduced sulfur sorbents

DOEpatents

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

2004-11-02

The disclosure is directed to sorbent compositions for removing reduced sulfur species (e.g., H.sub.2 S, COS and CS.sub.2) a feed stream. The sorbent is formed from a multi-phase composition including a zinc titanate phase and a zinc oxide-aluminate phase. The sorbent composition is substantially free of unreacted alumina.

40 CFR Table 3 to Subpart Jjjjjj... - Operating Limits for Boilers With Emission Limits

Code of Federal Regulations, 2012 CFR

2012-07-01

... performance test demonstrating compliance with the PM emission limitation. 4. Dry sorbent or carbon injection control Maintain the sorbent or carbon injection rate at or above the lowest 2-hour average sorbent flow... emissions limitation. When your boiler operates at lower loads, multiply your sorbent or carbon injection...

40 CFR Table 7 to Subpart Jjjjjj... - Demonstrating Continuous Compliance

Code of Federal Regulations, 2013 CFR

2013-07-01

... § 63.11211. 4. Dry Scrubber Sorbent or Activated Carbon Injection Rate a. Collecting the sorbent or activated carbon injection rate monitoring system data for the dry scrubber according to §§ 63.11224 and 63... average sorbent or activated carbon injection rate at or above the minimum sorbent or activated carbon...

40 CFR Table 7 to Subpart Jjjjjj... - Demonstrating Continuous Compliance

Code of Federal Regulations, 2014 CFR

2014-07-01

... § 63.11211. 4. Dry Scrubber Sorbent or Activated Carbon Injection Rate a. Collecting the sorbent or activated carbon injection rate monitoring system data for the dry scrubber according to §§ 63.11224 and 63... average sorbent or activated carbon injection rate at or above the minimum sorbent or activated carbon...

Development and evaluation of a silver mordenite composite sorbent for the partitioning of xenon from krypton in gas compositions

DOE PAGES

Garn, Troy G.; Greenhalgh, Mitchell; Law, Jack D.

2015-12-22

A new engineered form composite sorbent for the selective separation of xenon from krypton in simulant composition off-gas streams resulting from the reprocessing of used nuclear fuel has been developed and evaluated. A sodium mordenite powder was incorporated into a macroporous polymer binder, formed into spherical beads and successfully converted to a 9 wt.% silver form composite sorbent. The final engineered form sorbent retained the characteristic surface area indicative of sodium mordenite powder. The sorbent was evaluated for xenon adsorption potential with capacities measured as high as 30 millimoles of xenon per kilogram of sorbent achieved at ambient temperature andmore » 460 millimoles of xenon per kilogram sorbent at 220 K. Xenon/krypton selectivity was calculated to be 22.4 with a 1020 µL/L xenon, 150 µL/L krypton in a balance of air feed gas at 220 K. Furthermore, adsorption/desorption thermal cycling effects were evaluated with results indicating sorbent performance was not significantly impacted while undergoing numerous adsorption/desorption thermal cycles.« less

Polymeric ionic liquid bucky gels as sorbent coatings for solid-phase microextraction.

PubMed

Zhang, Cheng; Anderson, Jared L

2014-05-30

Novel cross-linked polymeric ionic liquid (PIL) bucky gels were formed by free-radical polymerization of polymerizable ionic liquids gelled with multi-walled carbon nanotubes (MWCNT) and used as sorbent coatings for solid-phase microextraction (SPME). The combination of PIL with MWCNTs significantly enhanced the π-π interaction between the sorbent coatings and the aromatic analytes. Compared to the neat PIL-based sorbent coating, the PIL bucky gel sorbent coatings demonstrated higher extraction efficiency for the extraction of polycyclic aromatic hydrocarbons (PAHs). A partitioning extraction mechanism was observed for the PIL/MWCNT-based sorbent coatings indicating that the addition of MWCNTs did not seem to affect the extraction mechanism of the sorbent coating. The analyte-to-coating partition coefficients (logKfs) were estimated and the limits of detection (LOD) for selected PIL bucky gel sorbent coating were determined to be in the range of 1-2.5 ng L(-1). Recovery studies were also performed for PAHs in river and tap water to validate the applicability of the developed method. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

Wilson, Lee D; Mohamed, Mohamed H; Berhaut, Christopher L

2011-08-29

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.

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

PubMed Central

Wilson, Lee D.; Mohamed, Mohamed H.; Berhaut, Christopher L.

2011-01-01

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. PMID:28824156

Carrageenan-grafted magnetite nanoparticles as recyclable sorbents for dye removal

NASA Astrophysics Data System (ADS)

Daniel-da-Silva, Ana L.; Salgueiro, Ana M.; Creaney, Bianca; Oliveira-Silva, Rui; Silva, Nuno J. O.; Trindade, Tito

2015-07-01

The efforts dedicated to improving water decontamination procedures have prompted the interest in the development of efficient, inexpensive, and reusable sorbents for the uptake of dye pollutants. In this work, novel sorbents consisting of carrageenan polysaccharides grafted to magnetic iron oxide nanoparticles were prepared. κ- and ι-carrageenan were first chemically modified by carboxymethylation and then covalently attached via amide bond to the surface of aminated silica-coated magnetite nanoparticles, both steps monitored using infrared spectroscopy (FTIR) analysis. The kinetics and the equilibrium behavior of the cationic dye methylene blue (MB) adsorption onto the carrageenan sorbents were investigated. ι-carrageenan sorbents displayed higher MB adsorption capacity that was ascribed to high content of sulfonate groups. Overall, the pseudo-second order equation provided a good description of the adsorption kinetics. The κ-carrageenan sorbents followed an unusual Z-type equilibrium adsorption isotherm whereas the isotherm of ι-carrageenan sorbents, although displaying a conventional shape, could not be successfully predicted by isotherm models commonly used. Noteworthy, both sorbents were long-term stable and could easily be recycled by simply rinsing with KCl aqueous solution. The removal efficiency of κ-carrageenan sorbents was 92 % in the first adsorption cycle and kept high (>80 %) even after six consecutive adsorption/desorption cycles.

JV Task 107- Pilot-Scale Emission Control Technology Testing for Constellation Energy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Michael Jones; Brandon Pavlish; Stephen Sollom

2007-06-30

An Indonesian, Colombian, and Russian coal were tested in the Energy & Environmental Research Center's combustion test facility for their performance and an evaluation of mercury release and capture with selected additives in both electrostatic precipitator and baghouse configurations. Sorbents included the carbon-based materials NORIT DARCO Hg, Sorbent Technologies B-PAC and B-PAC LC, STI Rejects provided by Constellation Energy, and Envergex e-Sorb, along with ChemMod's high-temperature additive. Each coal was evaluated over several days and compared. Ash-fouling tests were conducted, and mercury levels were monitored using continuous mercury monitors (CMMs). The Ontario Hydro mercury sampling method was also utilized. Themore » Indonesian coal had the lowest ash content, lowest sulfur content, and lowest energy content of the three coals tested. The Colombian coal had the highest mercury content and did contain a significant level of selenium which can interfere with the ability of a CMM to monitor mercury in the gas stream. All sorbents displayed very favorable results. In most cases, mercury removal greater than 86% could be obtained. The Indonesian coal displayed the best mercury removal with sorbent addition. A maximum removal of 97% was measured with this coal using Envergex's carbon-based sorbent at a rate of 4 lb/Macf across an electrostatic precipitator. The high ash and selenium content of the Colombian coal caused it to be a problematic fuel, and ash plugging of the test furnace was a real concern. Problems with the baghouse module led to limited testing. Results indicated that native capture across the baghouse for each coal type was significant enough not to warrant sorbent addition necessary. The fouling potential was the lowest for the Indonesian coal. Low sulfur content contributes to the poor potential for fouling, as witnessed by the lack of deposits during testing. The Russian and Colombian coals had a much higher potential for fouling primarily because of their high ash contents, but the potential was highest for the Colombian coal. Of the three coals tested, the Colombian would be the least desirable.« less

KINETICS OF Mn-BASED SORBENTS FOR HOT COAL GAS DESULFURIZATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

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 ofmore » 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 induration temperature. Sorbent also showed 30 to 53% loss of its strength over four cycles of sulfidation and regeneration. The former being sorbent indurated at 1115 o C and the prior being sorbent indurated at 1100 o C. A mathematical model was developed to describe the reaction of H 2 S with the mixed metal oxide in a fixed-bed reactor, where the individual pellets react according to the shrinking core model. The effective diffusivity within a single pellet was estimated by adjusting its value until a good match between the experimental and model H 2 S breakthrough curves was obtained. Predicted sorbent conversion at the conclusion of test FB3A compared well with experimental sulfur analysis.« less

Evaluation of Solid Sorbents as a Retrofit Technology for CO 2 Capture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sjostrom, Sharon

2016-06-02

ADA completed a DOE-sponsored program titled Evaluation of Solid Sorbents as a Retrofit Technology for CO 2 Capture under program DE-FE0004343. During this program, sorbents were analyzed for use in a post-combustion CO 2 capture process. A supported amine sorbent was selected based upon superior performance to adsorb a greater amount of CO 2 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 sorbentmore » CO 2 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 CO 2 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 CO 2 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 CO 2 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 primarily the result of sorbent circulation limitations at operating temperatures combined with pre-loading of the sorbent with CO 2 prior to entering the adsorber. Specifically, CO 2-rich gas was utilized to convey sorbent from the regenerator to the adsorber. This gas was nominally 45°C below the regenerator temperature during testing. ADA’s post-combustion capture system with modifications to overcome pilot constraints, in conjunction with incorporating a sorbent with CO 2 working capacity of 15 g CO 2/100 g sorbent and a contact time of 10 to 15 minutes or less with flue gas could provide significant cost and performance benefits when compared to an MEA system.« less

Optimization of sample preparation by central composite design for multi-class determination of veterinary drugs in bovine muscle, kidney and liver by ultra-high-performance liquid chromatographic-tandem mass spectrometry.

PubMed

Rizzetti, Tiele M; de Souza, Maiara P; Prestes, Osmar D; Adaime, Martha B; Zanella, Renato

2018-04-25

In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver. Copyright © 2017 Elsevier Ltd. All rights reserved.

Dispersive Solid Phase Extraction for the Analysis of Veterinary Drugs Applied to Food Samples: A Review

PubMed Central

Islas, Gabriela; Hernandez, Prisciliano

2017-01-01

To achieve analytical success, it is necessary to develop thorough clean-up procedures to extract analytes from the matrix. Dispersive solid phase extraction (DSPE) has been used as a pretreatment technique for the analysis of several compounds. This technique is based on the dispersion of a solid sorbent in liquid samples in the extraction isolation and clean-up of different analytes from complex matrices. DSPE has found a wide range of applications in several fields, and it is considered to be a selective, robust, and versatile technique. The applications of dispersive techniques in the analysis of veterinary drugs in different matrices involve magnetic sorbents, molecularly imprinted polymers, carbon-based nanomaterials, and the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method. Techniques based on DSPE permit minimization of additional steps such as precipitation, centrifugation, and filtration, which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique and how it has been applied to food analysis. PMID:29181027

Fabrication and characterization of buckypapers for use in air sampling

NASA Astrophysics Data System (ADS)

Oh, Jonghwa

Occupational exposure to volatile organic compounds (VOCs) is a concern from a public health perspective. In many industrial activities, workers' exposure to VOCs can be sufficiently high to induce adverse health effects, so their monitoring is necessary. In exposure assessment, post sampling extraction and quantification are the typical analytical procedures. Recently, our group developed the photothermal desorption (PTD) technique in which a pulse of light thermally desorbs an analyte directly from a sorbent. Advantages of this technique are; it is solvent free, repeated analysis is possible, sorbents are reusable, and no high cost of equipment is required. PTD overcomes almost all drawbacks of current extraction methods. This study was aimed to develop and test a new sorbent which will efficiently work with PTD. Single-walled carbon nanotubes (SWNTs) were examined as potential sorbents because of their high surface area, great thermal conductivity, and efficient light absorption. SWNTs were fabricated into a self-supporting form (i.e., buckypaper (BP)) which will preserve its physical integrity under normal working conditions. Largely two types of SWNTs were used, arc discharge (AD) and high-pressure carbon monoxide (HiPco), and different fabrication methods were examined. Upon fabrication, their adsorption properties were characterized in terms of Brunauer, Emmett, and Teller (BET) surface area, pore size, and toluene adsorption capacity. HiPco BP and methanol-cleaned AD BP (suspended/rinsed with methanol) were the top two materials, showing the highest surface area (649 and 387 m²/g, respectively) and adsorption capacity (106 and 46 mg/g, respectively) with relatively small mean pore diameter (7.7 and 8.8 nm, respectively). To further improve the adsorption properties, specific heat treatment conditions for each type of BPs were employed. After initial treatments only HiPco BP and acetone-cleaned AD BP (suspended/rinsed with acetone) were selected for further investigations based on obtained surface area (933 and 970 m²/g, respectively) and physical integrity. These two BPs were then examined for PTD and the AD BP showed higher recovery rate (0.016 - 0.431 %) at all energy levels examined (1.84 - 7.37 J). The AD BP has been shown to be an efficient sorbent for toluene and possibly a good candidate for PTD.

Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

Treesearch

Martha J.M. Wells; Jerry L. Michael

1987-01-01

Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Holly Krutka; Sharon Sjostrom

2011-07-31

Through a U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL) funded cooperative agreement DE-NT0005649, ADA Environmental Solutions (ADA) has begun evaluating the use of solid sorbents for CO{sub 2} capture. The project objective was to address the viability and accelerate development of a solid-based CO{sub 2} capture technology. To meet this objective, initial evaluations of sorbents and the process/equipment were completed. First the sorbents were evaluated using a temperature swing adsorption process at the laboratory scale in a fixed-bed apparatus. A slipstream reactor designed to treat flue gas produced by coal-fired generation of nominally 1 kWe was designedmore » and constructed, which was used to evaluate the most promising materials on a more meaningful scale using actual flue gas. In a concurrent effort, commercial-scale processes and equipment options were also evaluated for their applicability to sorbent-based CO{sub 2} capture. A cost analysis was completed that can be used to direct future technology development efforts. ADA completed an extensive sorbent screening program funded primarily through this project, DOE NETL cooperative agreement DE-NT0005649, with support from the Electric Power Research Institute (EPRI) and other industry participants. Laboratory screening tests were completed on simulated and actual flue gas using simulated flue gas and an automated fixed bed system. The following types and quantities of sorbents were evaluated: 87 supported amines; 31 carbon based materials; 6 zeolites; 7 supported carbonates (evaluated under separate funding); and 10 hydrotalcites. Sorbent evaluations were conducted to characterize materials and down-select promising candidates for further testing at the slipstream scale. More than half of the materials evaluated during this program were supported amines. Based on the laboratory screening four supported amine sorbents were selected for evaluation at the 1 kW scale at two different 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 diffusion limitations related to the CO{sub 2} uptake rate. Three additional supported amine materials, sorbents AX, F, and BN, were selected for evaluation using the 1 kW pilot at Sherco. Sorbent AX was operated in batch mode and performed similarly to sorbent R (i.e. could achieve up to 90% removal when given adequate regeneration time). Sorbent BN was not expected to be subject to the same mass diffusion limitations as experienced with sorbent R. When sorbent BN was used in continuous mode the steady state CO{sub 2} removal was approximately double that of sorbent R, which highlighted the importance of sorbents without kinetic limitations.« less

Screening of cocaine and its metabolites in human urine samples by direct analysis in real-time source coupled to time-of-flight mass spectrometry after online preconcentration utilizing microextraction by packed sorbent.

PubMed

Jagerdeo, Eshwar; Abdel-Rehim, Mohamed

2009-05-01

Microextraction by packed sorbent (MEPS) has been evaluated for fast screening of drugs of abuse with mass spectrometric detection. In this study, C8 (octyl-silica, useful for nonpolar to moderately polar compounds), ENV(+) (hydroxylated polystyrene-divinylbenzene copolymer, for extraction of aliphatic and aromatic polar compounds), Oasis MCX (sulfonic-poly(divinylbenzene-co-N-polyvinyl-pyrrolidone) copolymer), and Clean Screen DAU (mixed mode, ion exchanger for acidic and basic compounds) were used as sorbents for the MEPS. The focus was on fast extraction and preconcentration of the drugs with rapid analysis using a time-of-flight (TOF) mass spectrometer as the detector with direct analysis in a real-time (DART) source. The combination of an analysis time of less than 1 min and accurate mass of the first monoisotopic peak of the analyte and the relative abundances of the peaks in the isotopic clusters provided reliable information for identification. Furthermore, the study sought to demonstrate that it is possible to quantify the analyte of interest using a DART source when an internal standard is used. Of all the sorbents used in the study, Clean Screen DAU performed best for extraction of the analytes from urine. Using Clean Screen DAU to extract spiked samples containing the drugs, linearity was demonstrated for ecgonine methyl ester, benzoylecgonine, cocaine, and cocaethylene with average ranges of: 65-910, 75-1100, 95-1200, and 75-1100 ng/mL (n = 5), respectively. The limits of detection (LOD) for ecgonine methyl ester, benzoylecgonine, cocaine, and cocaethylene were 22.9 ng/mL, 23.7 ng/mL, 4.0 ng/mL, and 9.8 ng/mL respectively, using a signal-to-noise ratio of 3:1.

Matrix molecularly imprinted mesoporous sol-gel sorbent for efficient solid-phase extraction of chloramphenicol from milk.

PubMed

Samanidou, Victoria; Kehagia, Maria; Kabir, Abuzar; Furton, Kenneth G

2016-03-31

Highly selective and efficient chloramphenicol imprinted sol-gel silica based inorganic polymeric sorbent (sol-gel MIP) was synthesized via matrix imprinting approach for the extraction of chloramphenicol in milk. Chloramphenicol was used as the template molecule, 3-aminopropyltriethoxysilane (3-APTES) and triethoxyphenylsilane (TEPS) as the functional precursors, tetramethyl orthosilicate (TMOS) as the cross-linker, isopropanol as the solvent/porogen, and HCl as the sol-gel catalyst. Non-imprinted sol-gel polymer (sol-gel NIP) was synthesized under identical conditions in absence of template molecules for comparison purpose. Both synthesized materials were characterized by Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR) and nitrogen adsorption porosimetry, which unambiguously confirmed their significant structural and morphological differences. The synthesized MIP and NIP materials were evaluated as sorbents for molecularly imprinted solid phase extraction (MISPE) of chloramphenicol in milk. The effect of critical extraction parameters (flow rate, elution solvent, sample and eluent volume, selectivity coefficient, retention capacity) was studied in terms of retention and desorption of chloramphenicol. Competition and cross reactivity tests have proved that sol-gel MIP sorbent possesses significantly higher specific retention and enrichment capacity for chloramphenicol compared to its non-imprinted analogue. The maximum imprinting factor (IF) was found as 9.7, whereas the highest adsorption capacity of chloramphenicol by sol-gel MIP was 23 mg/g. The sol-gel MIP was found to be adequately selective towards chloramphenicol to provide the necessary minimum required performance limit (MRPL) of 0.3 μg/kg set forth by European Commission after analysis by LC-MS even without requiring time consuming solvent evaporation and sample reconstitution step, often considered as an integral part in solid phase extraction work-flow. Intra and inter-assay RSD values were less than 13% and accuracy expressed as relative recovery ranged from 85 to 106%. Copyright © 2016 Elsevier B.V. All rights reserved.

Multi-Column Experimental Test Bed Using CaSDB MOF for Xe/Kr Separation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Welty, Amy Keil; Greenhalgh, Mitchell Randy; Garn, Troy Gerry

Processing of spent nuclear fuel produces off-gas from which several volatile radioactive components must be separated for further treatment or storage. As part of the Off-gas Sigma Team, parallel research at INL and PNNL has produced several promising sorbents for the selective capture of xenon and krypton from these off-gas streams. In order to design full-scale treatment systems, sorbents that are promising on a laboratory scale must be proven under process conditions to be considered for pilot and then full-scale use. To that end, a bench-scale multi-column system with capability to test multiple sorbents was designed and constructed at INL.more » This report details bench-scale testing of CaSDB MOF, produced at PNNL, and compares the results to those reported last year using INL engineered sorbents. Two multi-column tests were performed with the CaSDB MOF installed in the first column, followed with HZ-PAN installed in the second column. The CaSDB MOF column was placed in a Stirling cryocooler while the cryostat was employed for the HZ-PAN column. Test temperatures of 253 K and 191 K were selected for the first column while the second column was held at 191 K for both tests. Calibrated volume sample bombs were utilized for gas stream analyses. At the conclusion of each test, samples were collected from each column and analyzed for gas composition. While CaSDB MOF does appear to have good capacity for Xe, the short time to initial breakthrough would make design of a continuous adsorption/desorption cycle difficult, requiring either very large columns or a large number of smaller columns. Because of the tenacity with which Xe and Kr adhere to the material once adsorbed, this CaSDB MOF may be more suitable for use as a long-term storage solution. Further testing is recommended to determine if CaSDB MOF is suitable for this purpose.« less

Signal enhancement using a switchable magnetic trap

DOEpatents

Beer, Neil Reginald [Pleasanton, CA

2012-05-29

A system for analyzing a sample including providing a microchannel flow channel; associating the sample with magnetic nanoparticles or magnetic polystyrene-coated beads; moving the sample with said magnetic nanoparticles or magnetic polystyrene-coated beads in the microchannel flow channel; holding the sample with the magnetic nanoparticles or magnetic polystyrene-coated beads in a magnetic trap in the microchannel flow channel; and analyzing the sample obtaining an enhanced analysis signal. An apparatus for analysis of a sample includes magnetic particles connected to the sample, a microchip, a flow channel in the microchip, a source of carrier fluid connected to the flow channel for moving the sample in the flow channel, an electromagnet trap connected to the flow line for selectively magnetically trapping the sample and the magnetic particles, and an analyzer for analyzing the sample.

Trap configuration and spacing influences parameter estimates in spatial capture-recapture models

USGS Publications Warehouse

Sun, Catherine C.; Fuller, Angela K.; Royle, J. Andrew

2014-01-01

An increasing number of studies employ spatial capture-recapture models to estimate population size, but there has been limited research on how different spatial sampling designs and trap configurations influence parameter estimators. Spatial capture-recapture models provide an advantage over non-spatial models by explicitly accounting for heterogeneous detection probabilities among individuals that arise due to the spatial organization of individuals relative to sampling devices. We simulated black bear (Ursus americanus) populations and spatial capture-recapture data to evaluate the influence of trap configuration and trap spacing on estimates of population size and a spatial scale parameter, sigma, that relates to home range size. We varied detection probability and home range size, and considered three trap configurations common to large-mammal mark-recapture studies: regular spacing, clustered, and a temporal sequence of different cluster configurations (i.e., trap relocation). We explored trap spacing and number of traps per cluster by varying the number of traps. The clustered arrangement performed well when detection rates were low, and provides for easier field implementation than the sequential trap arrangement. However, performance differences between trap configurations diminished as home range size increased. Our simulations suggest it is important to consider trap spacing relative to home range sizes, with traps ideally spaced no more than twice the spatial scale parameter. While spatial capture-recapture models can accommodate different sampling designs and still estimate parameters with accuracy and precision, our simulations demonstrate that aspects of sampling design, namely trap configuration and spacing, must consider study area size, ranges of individual movement, and home range sizes in the study population.

Apparatus for hot-gas desulfurization of fuel gases

DOEpatents

Bissett, Larry A.

1992-01-01

An apparatus for removing sulfur values from a hot fuel gas stream in a fdized bed contactor containing particulate sorbent material by employing a riser tube regeneration arrangement. Sulfur-laden sorbent is continuously removed from the fluidized bed through a stand pipe to the riser tube and is rapidly regenerated in the riser tube during transport of the sorbent therethrough by employing an oxygen-containing sorbent regenerating gas stream. The riser tube extends from a location below the fluidized bed to an elevation above the fluidized bed where a gas-solid separating mechanism is utilized to separate the regenerated particulate sorbent from the regeneration gases and reaction gases so that the regenerated sorbent can be returned to the fluidized bed for reuse.

Multistage open-tube trap for enrichment of part-per-trillion trace components of low-pressure (below 27-kPa) air samples

NASA Technical Reports Server (NTRS)

Ohara, D.; Vo, T.; Vedder, J. F.

1985-01-01

A multistage open-tube trap for cryogenic collection of trace components in low-pressure air samples is described. The open-tube design allows higher volumetric flow rates than densely packed glass-bead traps commonly reported and is suitable for air samples at pressures below 27 kPa with liquid nitrogen as the cryogen. Gas blends containing 200 to 2500 parts per trillion by volume each of ethane and ethene were sampled and hydrocarbons were enriched with 100 + or - 4 percent trap efficiency. The multistage design is more efficient than equal-length open-tube traps under the conditions of the measurements.

Quadrupole ion traps and trap arrays: geometry, material, scale, performance.

PubMed

Ouyang, Z; Gao, L; Fico, M; Chappell, W J; Noll, R J; Cooks, R G

2007-01-01

Quadrupole ion traps are reviewed, emphasizing recent developments, especially the investigation of new geometries, guided by multiple particle simulations such as the ITSIM program. These geometries include linear ion traps (LITs) and the simplified rectilinear ion trap (RIT). Various methods of fabrication are described, including the use of rapid prototyping apparatus (RPA), in which 3D objects are generated through point-by-point laser polymerization. Fabrication in silicon using multilayer semi-conductor fabrication techniques has been used to construct arrays of micro-traps. The performance of instruments containing individual traps as well as arrays of traps of various sizes and geometries is reviewed. Two types of array are differentiated. In the first type, trap arrays constitute fully multiplexed mass spectrometers in which multiple samples are examined using multiple sources, analyzers and detectors, to achieve high throughput analysis. In the second, an array of individual traps acts collectively as a composite trap to increase trapping capacity and performance for a single sample. Much progress has been made in building miniaturized mass spectrometers; a specific example is a 10 kg hand-held tandem mass spectrometer based on the RIT mass analyzer. The performance of this instrument in air and water analysis, using membrane sampling, is described.

Comparison of carbon dioxide-baited trapping systems for sampling outdoor mosquito populations in Tanzania.

PubMed

Mboera LEG; Knols BGJ; Braks MAH; Takken, W

2000-09-01

For collecting mosquitoes (Diptera: Culicidae) the outdoor catching efficiency of four types of trapping devices baited with carbon dioxide (CO2, 300 ml/ min) was evaluated and compared in two areas of Tanzania. The types of traps employed were: the CDC miniature trap with the incandescent light bulb switched on or off; electric nets (ENT) and a Counterflow Geometry (CFG) trap. In Njage, southeast Tanzania, Anopheles gambiae Giles sensu stricto was the most abundant of the seven mosquito species obtained, comprising of 74.3% of the total number caught (n=2,171). In Muheza, north-east Tanzania, Culex quinquefasciatus Say was the predominant species (90.9%) among 1,080 caught. At both localities the CFG trap was superior to the CDC trap with light-on or light-off for sampling both An. gambiae and Cx. quinquefasciatus. Efficiency of the CFG trap and ENT were similar for sampling these species of mosquitoes (P > 0.05). However, ENT was superior to the CDC trap with light-off for collecting both species. Significantly more (P < 0.05) Cx. quinquefasciatus were obtained by the CDC trap with light-off than with light-on, especially outdoors. It is concluded that both ENT and the CFG are effective tools for sampling populations of An. gambiae and Cx. quinquefasciatus outdoors.

Variation in Baiting Intensity Among CO2-Baited Traps Used to Collect Hematophagous Arthropods

PubMed Central

Springer, Yuri P.; Taylor, Jeffrey R.; Travers, Patrick D.

2015-01-01

Hematophagous arthropods transmit the etiological agents of numerous diseases and as a result are frequently the targets of sampling to characterize vector and pathogen populations. Arguably, the most commonly used sampling approach involves traps baited with carbon dioxide. We report results of a laboratory study in which the performance of carbon dioxide-baited traps was evaluated using measures of baiting intensity, the amount of carbon dioxide released per unit time during trap deployment. We evaluated the effects of trap design, carbon dioxide source, and wind speed on baiting intensity and documented significant effects of these factors on the length of sampling (time to baiting intensity = 0), maximum baiting intensity, and variation in baiting intensity during experimental trials. Among the three dry ice-baited trap types evaluated, traps utilizing insulated beverage coolers as dry ice containers sampled for the longest period of time, had the lowest maximum but most consistent baiting intensity within trials and were least sensitive to effects of wind speed and dry ice form (block vs. pellet) on baiting intensity. Results of trials involving traps baited with carbon dioxide released from pressurized cylinders suggested that this trap type had performance comparable to dry ice-baited insulated cooler traps but at considerably higher cost. PMID:26160803

The role of humic acids and biochar as specific sorbents of pesticides in soil

NASA Astrophysics Data System (ADS)

Ćwieląg-Piasecka, Irmina; Dębicka, Magdalena; Medyńska-Jureszek, Agnieszka; Weber, Jerzy; Jamroz, Elżbieta

2017-04-01

Pesticides are widely used in agriculture to prevent or control different pests and increase yield as well as products quality. Despite of the strict regulations concerning sustainable use of plant protection products, their residues are very often present in soil. Depending on their chemical and physical properties, they undergo various transformations in the soil. This results in their retention on different sorbents, degradation by microorganisms or leaching to the groundwater. Biochar is a carbon-rich byproduct of thermal biomass conversion, and due to its high sorption properties can be an efficient sorbent for pesticides in soil. The aim of the research was to compare the effect of two types of organic sorbents - humic acids (HA) and biochar (BC) - in sorption-desorption processes of different pesticides, which residues are commonly present in arable soils and thus are potentially harmful for the environment. The humic acids were extracted from topsoil horizon of arable cambisoil derived from loam (Lower Silesia, Poland) by Shnitzer's method, then purified using XAD resin and freeze-dried. Biochar was produced from wheat straw in gasification process at 550˚C, remaining 30 minutes in the reactor. Investigated pesticides belong to three different chemical classes: carbamates (carbaryl and carbofuran), phenoxyacetic acids (2,4-D and MCPA) and aniline derivatives (metolachlor), and are active substances of commonly used plant protection products in agriculture. To obtain the experimental goal the sorption experiment was conducted. To the investigated organic matter samples (HA or BC) aliquots of pesticides solutions in 10M CaCl2 were added and the mixtures were shaken for 24h. Afterwards the samples were centrifuged and supernatants analyzed by LC-MS/MS for the pesticides content. After that the same samples were refilled with CaCl2 and analyzed in the same way for desorption studies. Humic acids exhibited strong affinity for the ionic substances (2,4-D, MCPA), for which high percentage uptake was obtained (about 70% of the compound sorbed). Retention of carbamates on HA were much weaker, on contrary to their behavior towards BC - the uptake of carbamates on BC was nearly total (in the range from 90 to nearly 100%). Metolachlor was sorbed comparably strong both by HA and BC. Noticeable desorption occurred only in case of 2,4-D bound to HA, which might suggest the moderately strong bonding type. On the other hand, in case of BC desorption was completely inhibited due to stronger type of interaction with investigated substances. The obtained results indicate that the sorption behaviour of HA and BC is completely different, depending on the chemical structure both of the organic sorbents and pesticides used. Hydrophobic surface of adopted BC may preferentially attract pesticides of nonpolar and nonionic structural features. Soil humic acids, which are main sorbents of organic pollutants in soil, bind chemicals through the ionic, hydrogen and covalent bonding as well as hydrophobic bonding or van der Waals forces, which in some cases may result in a weaker pesticide retention.

Characterizing odors from cattle feedlots with different odor techniques

USDA-ARS?s Scientific Manuscript database

Odors from cattle feedlots negatively affect local communities. The purpose of this study was to characterize odors and odorants using different odor sampling techniques. Odors were characterized with field olfactometers (Nasal Ranger®), sensory techniques (GC-O) and analytical techniques (sorbent t...

Phototaxis of larval and juvenile northern pike

USGS Publications Warehouse

Zigler, S.J.; Dewey, M.R.

1995-01-01

Age- Phi northern pike Esox lucius prefer vegetated habitats that are difficult to sample with standard towed gears. Light traps can be effective for sampling larval fishes in dense vegetation, given positive phototaxis of fish. We evaluated the phototactic response of young northern pike by comparing the catches of larvae and juveniles obtained with plexiglass traps deployed with a chemical light stick versus traps deployed without a light source (controls) in a laboratory raceway and in a vegetated pond. In the laboratory tests, catches of protolarvae and mesolarvae in lighted traps were 11-35 times greater than catches in control traps. The catches of juvenile northern pike in field and laboratory experiments were 3-15 times greater in lighted traps than in control traps, even though the maximum body width of the larger juveniles was similar to the width of the entrance slots of the traps (5 mm). Larval and juvenile northern pike were photopositive; thus, light traps should effectively sample age-0 northern pike for at least 6 weeks after hatching.

Sorbent Scoping Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chancellor, Christopher John

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 thatmore » 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.« less

Ecologically friendly ways to clean up oil spills in harbor water areas: crude oil and diesel sorption behavior of natural sorbents.

PubMed

Paulauskiene, Tatjana

2018-04-01

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.

Performance of Zn-Fe-Mn/MCM-48 sorbents for high temperature H2S removal and analysis of regeneration process

NASA Astrophysics Data System (ADS)

Huang, Z. B.; Liu, B. S.; Wang, F.; Amin, R.

2015-10-01

MCM-48 was synthesized using a rapid and facile process at room temperature. A series of 50%Zn-Fe-Mn/MCM-48 sorbents were prepared and their performance of hot coal gas desulfurization was investigated. High breakthrough sulfur capacity (13.2 g-S/100 g sorbent) and utilization (66.1%) of 50%1Zn2Fe2Mn/MCM-48 sorbent at 550 °C was achieved. The characterization results of XRD, BET, TPR and FT-IR revealed that MCM-48 had excellent thermal stability at less than 700 °C, ZnMn2O4 and (Mn, Zn)Fe2O4 were mainly active particles in fresh sorbents which were highly dispersed on support. The MCM-48 mesoporous structure remained intact after eight successive desulfurization/regeneration cycles. The regeneration process of 50%1Zn2Fe2Mn/MCM-48 sorbent was analyzed, it indicated that the breakthrough sulfur capacity decline of sorbent was due to the migration of Zn onto the sorbent surface and Zn accumulated on the surface and vaporized to the exterior from the surface. In the TPO test, the oxidation of Zn was different for 50%Zn/MCM-48 at 700 °C. It revealed that the temperature of regeneration for ZnO sorbent should be higher than 700 °C.

High copper level comulled and impregnated sulfur sorbent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bishop, K.C.

A porous sulfur sorbent is disclosed which has principal use in desulfurizing reformer feedstreams. The sorbent is prepared by peptizing alumina with acid and mulling the peptized alumina with a copper compound to form an extrudable dough. The dough is extruded, dried and impregnated with additional copper. The resulting sorbent has a higher capacity for adsorbing sulfur compounds than conventional prior art materials.

Molecularly imprinted polymer cartridges coupled on-line with high performance liquid chromatography for simple and rapid analysis of dextromethorphan in human plasma samples.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Akbari-Adergani, Behrouz

2011-04-01

In this paper, a novel method is described for automated determination of dextromethorphan in biological fluids using molecularly imprinted solid-phase extraction (MISPE) as a sample clean-up technique combined with high performance liquid chromatography (HPLC). The water-compatible molecularly imprinted polymers (MIPs) were prepared using methacrylic acid as functional monomer, ethylene glycol dimethacrylate as cross-linker, chloroform as porogen and dextromethorphan as template molecule. These imprinted polymers were used as solid-phase extraction sorbent for the extraction of dextromethorphan from human plasma samples. Various parameters affecting the extraction efficiency of the MIP cartridges were evaluated. The high selectivity of the sorbent coupled to the high performance liquid chromatographic system permitted a simple and rapid analysis of this drug in plasma samples with limits of detection (LOD) and quantification (LOQ) of 0.12 ng/mL and 0.35 ng/mL, respectively. The MIP selectivity was evaluated by analyzing of the dextromethorphan in presence of several substances with similar molecular structures and properties. Results from the HPLC analyses showed that the recoveries of dextromethorphan using MIP cartridges from human plasma samples in the range of 1-50 ng/mL were higher than 87%. Copyright © 2011 Elsevier B.V. All rights reserved.

An improved analytical strategy combining microextraction by packed sorbent combined with ultra high pressure liquid chromatography for the determination of fluoxetine, clomipramine and their active metabolites in human urine.

PubMed

Alves, Vera; Gonçalves, João; Conceição, Carlota; Teixeira, Helena M; Câmara, José S

2015-08-21

A powerful and sensitive method, by microextraction packed sorbent (MEPS), and ultra-high performance liquid chromatography (UHPLC) with a photodiode array (PDA) detection, is described for the determination of fluoxetine, clomipramine and their active metabolites in human urine samples. The MEPS variables, such as sample volume, pH, number of extraction cycles (draw-eject), and desorption conditions (solvent and solvent volume of elution) were optimized. The analysis were carried out using small sample volumes (500μL) and in a short time period (5min for the entire sample preparation step). Good linearity was obtained for all antidepressants with the correlation coefficients (R(2)) above 0.9965. The limits of detection (LOD) ranged from 0.068 to 0.087μgmL(-1). The recoveries were from 93% to 98%, with relative standard deviations less than 6%. The inter-day precision, expressed as the relative standard deviation, varied between 3.8% and 8.5% while the intra-day precision between 3.0% and 7.1%. In order to evaluate the proposed method for clinical use, the MEPS/UHPLC-PDA method was applied to analysis of urine samples from depressed patients. Copyright © 2015 Elsevier B.V. All rights reserved.

Reversible Ammonia Sorption for the Primary Life Support System (PLSS)

NASA Technical Reports Server (NTRS)

Wojtowicz, Marek A.; Cosgrove, Joseph E.; Serio, Michael A.; Jennings, Mallory A.

2012-01-01

Results are presented on the development of regenerable trace-contaminant (TC) sorbent for use in Extravehicular Activities (EVAs), and more specifically in the Primary Life Support System (PLSS). Since ammonia is the most important TC to be captured, data presented in this paper are limited to ammonia sorption, with results relevant to other TCs to be reported at a later time. The currently available TC-control technology involves the use of a packed bed of acid-impregnated granular charcoal. The sorbent is non-regenerable, and its use is associated with appreciable pressure drop, i.e. power consumption. The objective of this work is to demonstrate the feasibility of using vacuum-regenerable sorbents for PLSS application. In this study, several carbon sorbent monoliths were fabricated and tested. Multiple adsorption/vacuum-regeneration cycles were demonstrated at room temperature, as well as carbon surface conditioning that enhances ammonia sorption without impairing sorbent regeneration. Depending on sorbent monolith geometry, the reduction in pressure drop with respect to granular sorbent was found to be between 50% and two orders of magnitude. Resistive heating of the carbon sorbent monolith was demonstrated by applying voltage to the opposite ends of the monolith.

Removal of sulphur dioxide from flue gases

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ersoy-Mericboyu, A.

1999-08-01

Mixtures of Ca(OH){sub 2} and different siliceous materials such as fly ash, bentonite, silica fume, and diatomite were hydrated to produce reactive SO{sub 2} sorbents. It was observed that these sorbents showed a better reactivity toward SO{sub 2} than the Ca(OH){sub 2} itself. This behavior is closely related to the pozzolanic nature of the hydrated sorbents and to the greater surface area. The reactivity of the sorbents was strongly influenced by the source of siliceous material and the hydration conditions. The total sulphation capacities of the sorbents were determined at 338 K with a synthetic gaseous mixture containing 5,000 ppmmore » SO{sub 2} and 55% relative humidity. Depending on the chemical and physical properties of the sorbents, the SO{sub 2} captures ranged from 1.20 to 5.58 mmol SO{sub 2}/g sorbent. The amount of SO{sub 2} capture increased with the increasing surface area of the sorbent. The utilization of Ca(OH){sub 2} with SO{sub 2} improved significantly when Ca(OH){sub 2} was hydrated with siliceous materials first and later exposed to SO{sub 2}.« less

Near-Resonant Imaging of Trapped Cold Atomic Samples

PubMed Central

You, L.; Lewenstein, Maciej

1996-01-01

We study the formation of diffraction patterns in the near-resonant imaging of trapped cold atomic samples. We show that the spatial imaging can provide detailed information on the trapped atomic clouds. PMID:27805110

Simulation-assisted design of microfluidic sample traps for optimal trapping and culture of non-adherent single cells, tissues, and spheroids.

PubMed

Rousset, Nassim; Monet, Frédéric; Gervais, Thomas

2017-03-21

This work focuses on modelling design and operation of "microfluidic sample traps" (MSTs). MSTs regroup a widely used class of microdevices that incorporate wells, recesses or chambers adjacent to a channel to individually trap, culture and/or release submicroliter 3D tissue samples ranging from simple cell aggregates and spheroids, to ex vivo tissue samples and other submillimetre-scale tissue models. Numerous MST designs employing various trapping mechanisms have been proposed in the literature, spurring the development of 3D tissue models for drug discovery and personalized medicine. Yet, there lacks a general framework to optimize trapping stability, trapping time, shear stress, and sample metabolism. Herein, the effects of hydrodynamics and diffusion-reaction on tissue viability and device operation are investigated using analytical and finite element methods with systematic parametric sweeps over independent design variables chosen to correspond to the four design degrees of freedom. Combining different results, we show that, for a spherical tissue of diameter d < 500 μm, the simplest, closest to optimal trap shape is a cube of dimensions w equal to twice the tissue diameter: w = 2d. Furthermore, to sustain tissues without perfusion, available medium volume per trap needs to be 100× the tissue volume to ensure optimal metabolism for at least 24 hours.

Analytical procedure for the determination of very volatile organic compounds (C3-C6) in indoor air.

PubMed

Schieweck, Alexandra; Gunschera, Jan; Varol, Deniz; Salthammer, Tunga

2018-05-01

The substance group of very volatile organic compounds (VVOCs) is moving into the focus of indoor air analysis, facing ongoing regulations at international and European levels targeting on indoor air quality and human health. However, there exists at present no validated analysis for the identification and quantification of VVOCs in indoor air. Therefore, the present study targeted on the development of an analytical method in order to sample the maximum possible quantity of VVOCs in indoor air on solid sorbents with subsequent analysis by thermal desorption and coupled gas chromatography/mass spectrometry (TDS-GC/MS). For this purpose, it was necessary to investigate the performance of available sorbents and to optimize the parameters of GC/MS analysis. Stainless steel tubes filled with Carbograph 5TD were applied successfully for low-volume sampling (2-4 l) with minimal breakthrough (< 1%). With the developed method, VVOCs between C 3 and C 6 of different volatility and polarity  can be detected even in trace quantities with low limits of quantitation (LOQ; 1-3 μg m -3 ). Limitations occur for low molecular weight compounds ≤C 3 , especially for polar substances, such as carboxylic acids and for some aldehydes and alcohols. Consequently, established methods for the quantification of these compounds in indoor air cannot be fully substituted yet. At least three different analytical techniques are needed to cover the large spectrum of relevant VVOCs in indoor air. In addition, unexpected reaction products might occur and need to be taken into account to avoid misinterpretation of chromatographic signals. Graphical abstract Solid sorbent sampling of VVOCs (C 3 -C 6 ) in indoor air with subsequent TDS-GC/MS analysis.

Synthesis of sintering-resistant sorbents for CO2 capture.

PubMed

Liu, Wenqiang; Feng, Bo; Wu, Yueqin; Wang, Guoxiong; Barry, John; da Costa, João C Diniz

2010-04-15

Sorbents for high temperature CO2 capture are under intensive development owing to their potential applications in advanced zero emission power, sorption-enhanced steam methane reforming for hydrogen production and energy storage systems in chemical heat pumps. One of the challenges in the development is the prevention of sintering of the sorbent (normally a calcium oxide derivative) which causes the CO2 capture capacity of the material to deteriorate rapidly after a few cycles of utilization. Here we show that a simple wet mixing method can produce sintering-resistant sorbents from calcium and magnesium salts of d-gluconic acid. It was found that calcium oxide was well distributed in the sorbents with metal oxide nanoparticles on the surface acting as physical barriers, and the CO2 capture capacity of the sorbents was largely maintained over multiple cycles of utilization. This method was also applied to other organometallic salts of calcium and magnesium/aluminum and the produced sorbents showed similarly high reversibility.

Multiphase flow simulations of a moving fluidized bed regenerator in a carbon capture unit

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sarkar, Avik; Pan, Wenxiao; Suh, Dong-Myung

2014-10-01

To accelerate the commercialization and deployment of carbon capture technologies, computational fluid dynamics (CFD)-based tools may be used to model and analyze the performance of carbon capture devices. This work presents multiphase CFD-based flow simulations for the regeneration device responsible for extracting CO 2 from CO 2-loaded sorbent particles before the particles are recycled. The use of solid particle sorbents in this design is a departure from previously reported systems, where aqueous sorbents are employed. Another new feature is the inclusion of a series of perforated plates along the regenerator height. The influence of these plates on sorbent distribution ismore » examined for varying sorbent holdup, fluidizing gas velocity, and particle size. The residence time distribution of sorbents is also measured to classify the low regime as plug flow or well-mixed flow. The purpose of this work is to better understand the sorbent flow characteristics before reaction kinetics of CO 2 desorption can be implemented.« less

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

DOEpatents

Gangwal, S.; Jothimurugesan, K.

1999-07-27

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 process, such as catalysts for Fischer-Tropsh Synthesis, and sorbents for removal of sulfur gases 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.

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

DOEpatents

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.

Using Malaise traps to sample ground beetles (Coleoptera: Carabidae)

Treesearch

Michael D. Ulyshen; James L. Hanula; Scott Horn

2005-01-01

Pitfall traps provide an easy and inexpensive way to sample ground-dwelling arthropods (Spence and Niemela 1994; Spence et al. 1997; Abildsnes and Tommeras 2000) and have been used exclusively in many studies of the abundance and diversity of ground beetles (Coleoptera: Carabidae). Despite the popularity of this trapping technique, pitfall traps have many disadvantages...

Collection and identification of human remains volatiles by non-contact, dynamic airflow sampling and SPME-GC/MS using various sorbent materials.

PubMed

DeGreeff, Lauryn E; Furton, Kenneth G

2011-09-01

Human remains detection canines are used in locating deceased humans in diverse scenarios and environments based on odor produced during the decay process of the human body. It has been established that human remains detection canines are capable of locating human remains specifically, as opposed to living humans or animal remains, thus suggesting a difference in odor between the different sources. This work explores the collection and determination of such odors using a dynamic headspace concentration device. The airflow rate and three sorbent materials-Dukal cotton gauze, Johnson & Johnson cotton-blend gauze, and polyester material-used for odor collection were evaluated using standard compounds. It was determined that higher airflow rates and openly woven material, e.g., Dukal cotton gauze, yielded significantly less total volatile compounds due to compound breakthrough through the sorbent material. Collection from polymer- and cellulose-based materials demonstrated that the molecular backbone of the material is a factor in compound collection as well. Volatiles, including cyclic and straight-chain hydrocarbons, organic acids, sulfides, aldehydes, ketones, and alcohols, were collected from a population of 27 deceased bodies from two collection locations. The common compounds between the subjects were compared and the odor profiles were determined. These odor profiles were compared with those of animal remains and living human subjects collected in the same manner. Principal component analysis showed that the odor profiles of the three sample types were distinct.

Alternative sorbents for the dispersive solid-phase extraction step in quick, easy, cheap, effective, rugged and safe method for extraction of pesticides from rice paddy soils with determination by liquid chromatography tandem mass spectrometry.

PubMed

Arias, Jean Lucas de Oliveira; Rombaldi, Caroline; Caldas, Sergiane Souza; Primel, Ednei Gilberto

2014-09-19

The clean-up step is essential to reduce interferences, improve quantification and help to maintain the integrity of the chromatographic system when working with complex matrices. In this study, alternative materials were evaluated as sorbents in the dispersive solid-phase extraction (D-SPE) for the determination and extraction of seventeen pesticides from rice paddy soil samples by the quick, easy, cheap, effective, rugged and safe (QuEChERS) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chitin, chitosan, diatomaceous earth and PSA were compared in terms of extraction efficiency and matrix effect. The best results were achieved when chitosan was used. Quantification limits ranged from 0.1 to 100μgkg(-1). Calibration curves showed correlation coefficient values higher than 0.98. Results of accuracy and precision in the spiked soil samples between 60% and 120%, with a relative standard deviation lower than 20%, were reached for 15 out of 17 pesticides. The matrix effect was evaluated and only one compound was influenced by the matrix components, showing medium effect. Results showed that alternative materials are more effective and less expensive than traditional sorbents which have been usually employed, i.e., they may be used in the D-SPE step during the extraction of pesticides from rice paddy soils. Copyright © 2014 Elsevier B.V. All rights reserved.

One-pot synthesis of a multi-template molecularly imprinted polymer for the extraction of six sulfonamide residues from milk before high-performance liquid chromatography with diode array detection.

PubMed

Kechagia, Maria; Samanidou, Victoria; Kabir, Abuzar; Furton, Kenneth G

2018-02-01

A highly selective molecularly imprinted polymer sorbent was synthesized and employed for the simultaneous determination of six sulfonamide antibiotic residues (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, and sulfamethizole) in milk samples. Multi-analyte imprinted particles were used as a sorbent in solid-phase extraction. Sulfonamides were separated on a high-performance liquid chromatography column (Merck-Lichrospher RP18e, 5 μm 250 × 4 mm) and further identified and quantified by diode array detection. Several parameters including required loading of the molecularly imprinted polymer sorbent, mass of milk, volume, and type of elution solvent, as well as time for absorption and elution were investigated to obtain optimal experimental conditions. For comparison purpose, a non-imprinted polymer was applied under the optimum conditions. The validation study according to the European Union Decision 2002/657/EC was based on the investigation of linearity, selectivity, stability, limits of detection and quantitation, decision limit, detection capability, trueness, precision, and ruggedness according to Youden's approach. The decision limit and detection capability values in the milk were achieved from 101.9 to 113.5 μg/kg and from 114.4 to 135.4 μg/kg, respectively, depending on the target sulfonamide drug. Finally, the optimized protocol was successfully applied to commercial milk samples and human breast milk. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

PubMed

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.

Zeolite Linde Type L as micro-solid phase extraction sorbent for the high performance liquid chromatography determination of ochratoxin A in coffee and cereal.

PubMed

Lee, Tien Ping; Saad, Bahruddin; Ng, Eng Poh; Salleh, Baharuddin

2012-05-11

Zeolite Linde Type L (LTL) crystals with different length, diameter and particle size (nanosized LTL, rod LTL, cylinder LTL and needle LTL) were synthesized, characterized and were used as sorbent in the micro-solid phase extraction of ochratoxin A (OTA) before the high performance liquid chromatography detection. Under the optimized conditions, the detection limits of OTA for coffee and cereal were 0.09 ng g(-1) and 0.03 ng g(-1), respectively, while the quantification limits were 0.28 ng g(-1) and 0.08 ng g(-1), respectively. The recoveries of OTA of coffee and cereal spiked at 0.5, 10 and 25 ng g(-1) ranged from 91.7 to 101.0%. The proposed method was applied to forty-five samples of coffee and cereal. The presence of OTA was found in twenty-five samples, ranging from 0.28 to 9.33 ng g(-1). Copyright © 2012 Elsevier B.V. All rights reserved.

Pyridine-functionalized Fe₃O₄ nanoparticles as a novel sorbent for the preconcentration of lead and cadmium ions in tree leaf as a bioindicator of urban traffic pollution.

PubMed

Sayar, Omid; Zhad, Hamid Reza Lotfi Zadeh; Sadeghi, Omid; Amani, Vahid; Najafi, Ezzatolla; Tavassoli, Najmeh

2012-12-01

We have developed a facile and highly sensitive sorbent for cadmium and lead ions. It is based on Fe₃O₄ nanoparticles functionalized with a derivative of picoline and was characterized by scanning electron microscopy, differential thermographic analysis, and elemental analysis. The material can be applied to the preconcentration of lead and cadmium ions. Factors such as the type, concentration and volume of eluent, the pH of the sample solution, the time for extraction, and the volume of the sample were studied. The effects of a variety of ions on preconcentration and recovery of these ions were also investigated. The ions were determined by FAAS, and the limits of detection are <0.8 and <0.061 μg L⁻¹ for lead and cadmium, respectively. Recoveries and precisions are >98.0 % and <1.3 %, respectively. The method was validated by analyzing several certified leaf reference materials.

Laboratory Sampling Guide

DTIC Science & Technology

2012-05-11

their uses: Table 10. Types of Solid Sorbent Tubes Tube Type Typical Uses Anasorb® 747 Methyl Ethyl Ketone , Ethylene Oxide Charcoal Tube...Silica Gel Aliphatic Amines, Methanol, Aldehydes , Acid Mist 2.5.3 Passive Samplers. Passive samplers do not require a sampling pump (Figure 9). They...often encountered within the first 6 inches of soil. Water-soluble contaminants such as metals, acids, ketones , and alcohols will be encountered at

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.

PubMed

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.

Determination of metoprolol enantiomers in human plasma and saliva samples utilizing microextraction by packed sorbent and liquid chromatography-tandem mass spectrometry.

PubMed

Elmongy, Hatem; Ahmed, Hytham; Wahbi, Abdel-Aziz; Amini, Ahmad; Colmsjö, Anders; Abdel-Rehim, Mohamed

2016-08-01

A sensitive, accurate and reliable bioanalytical method for the enantioselective determination of metoprolol in plasma and saliva samples utilizing liquid chromatography-electrospray ionization tandem mass spectrometry was developed and validated. Human plasma and saliva samples were pretreated by microextraction by packed sorbent (MEPS) prior to analysis. A new MEPS syringe form with two inputs was used. Metoprolol enantiomers and internal standard pentycaine (IS) were eluted from MEPS sorbent using isopropanol after removal of matrix interferences using aliquots of 5% methanol in water. Complete separation of metoprolol enantiomers was achieved on a Cellulose-SB column (150 × 4.6 mm, 5 μm) using isocratic elution with mobile phase 0.1% ammonium hydroxide in hexane-isopropanol (80:20, v/v) with a flow rate of 0.8 mL/min. A post-column solvent-assisted ionization was applied to enhance metoprolol ionization signal in positive mode monitoring (+ES) using 0.5% formic acid in isopropanol at a flow rate of 0.2 mL/min. The total chromatographic run time was 10 min for each injection. The detection of metoprolol in plasma and saliva samples was performed using triple quadrupole tandem mass spectrometer in +ES under the following mass transitions: m/z 268.08 → 72.09 for metoprolol and m/z 303.3 → 154.3 for IS. The linearity range was 2.5-500 ng/mL for both R- and S-metoprolol in plasma and saliva. The limits of detection and quantitation for both enantiomers were 0.5 and 2.5 ng/mL respectively, in both matrices (plasma and saliva). The intra- and inter-day precisions were presented in terms of RSD values for replicate analysis of quality control samples and were <5%; the accuracy of determinations varied from 96 to 99%. The method was able to determine the therapeutic levels of metoprolol enantiomers in both human plasma and saliva samples successfully, which can aid in therapeutic drug monitoring in clinical laboratories. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Polar organic chemical integrative samplers for pesticides monitoring: impacts of field exposure conditions.

PubMed

Lissalde, Sophie; Mazzella, Nicolas; Mazellier, Patrick

2014-08-01

This study focuses on how Polar Organic Chemical Integrative Samplers (POCIS) work in real environmental conditions. A selection of 23 polar pesticides and 8 metabolites were investigated by exposure of triplicates of integrative samplers in two rivers in France for successive 14-day periods. The pesticides and metabolites were trapped not only in Oasis HLB sorbent but also in the polyethersulfone (PES) membrane of the POCIS. The distribution of pesticides depended on the molecular structure. The use of the Performance Reference Compound (PRC) is also discussed here. The impact of some environmental parameters and exposure setup on the transfer of pesticides in POCIS sorbent was studied: river flow rate, biofouling on membranes, sampler holding design and position in the stream. Results show a significant impact of river flow velocity on PRC desorption, especially for values higher than 4 cm·s(-1). Some fouling was observed on the PES membrane which could potentially have an impact on molecule accumulation in the POCIS. Finally, the positioning of the sampler in the river did not have significant effects on pesticide accumulation, when perpendicular exposures were used (sampler positioning in front of the water flow). The POCIS with PRC correction seems to be a suitable tool for estimating time-weighted average (TWA) concentrations, for all the molecules except for one of the nine pesticides analyzed in these two French rivers. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of stable tetraethylenepentamine-modified ordered mesoporous silica sorbents by recycling natural Equisetum ramosissimum.

PubMed

Liu, Shou-Heng; Kuok, Chi-Hong

2018-01-01

It is well-known that global warming of the earth is caused by the progressive increase of CO 2 concentration in the environment due to the huge utilization of fossil fuels. As a result, the development of an efficient and economic method to capture CO 2 from large stationary sources, such as coal-fired power plants, cement and steel factories, and so on is urgent. In this study, ordered mesoporous silicas (E-SBA-15) have been prepared by using Equisetum ramosissimum plants as the silica sources and their subsequently incorporating with amino-containing compounds (tetraethylenepentamine, TEPA) and stabilizers (titanium isopropoxide, TIP). A variety of different spectroscopic and analytical techniques, such as nitrogen adsorption-desorption isotherms, low-angle X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transformed infrared (FTIR) spectroscopy, and thermogravimetric analysis (TGA) are used to characterize the physicochemical properties of various materials. CO 2 adsorption capacities of prepared sorbents at 75 °C are obtained by TGA at atmospheric pressure. Among all sorbents, TEPA impregnated E-SBA-15 sorbents possess the highest CO 2 sorption capacity (1.60 mmol CO 2 g -1 sorbent ) under ambient pressure using dry 15% CO 2 . However, TEPA/TIP incorporated E-SBA-15 sorbents exhibit enhanced durability during repeated sorption-desorption cycles compared to the above-mentioned sorbents. This significant enhancement in the stability of CO 2 sorption-desorption process is most likely due to the decreased decomposition/leaching of TEPA which is restricted via the steric effect of TIP. These synthesized sorbents from inexpensive resources (agricultural waste) exhibit good sorbent capacity and surpassing regenerability, revealing a promising CO 2 sorbent for the cost-effective applications in a cyclic adsorption process. Copyright © 2017 Elsevier Ltd. All rights reserved.

Variation in Baiting Intensity Among CO2-Baited Traps Used to Collect Hematophagous Arthropods.

PubMed

Springer, Yuri P; Taylor, Jeffrey R; Travers, Patrick D

2015-01-01

Hematophagous arthropods transmit the etiological agents of numerous diseases and as a result are frequently the targets of sampling to characterize vector and pathogen populations. Arguably, the most commonly used sampling approach involves traps baited with carbon dioxide. We report results of a laboratory study in which the performance of carbon dioxide-baited traps was evaluated using measures of baiting intensity, the amount of carbon dioxide released per unit time during trap deployment. We evaluated the effects of trap design, carbon dioxide source, and wind speed on baiting intensity and documented significant effects of these factors on the length of sampling (time to baiting intensity = 0), maximum baiting intensity, and variation in baiting intensity during experimental trials. Among the three dry ice-baited trap types evaluated, traps utilizing insulated beverage coolers as dry ice containers sampled for the longest period of time, had the lowest maximum but most consistent baiting intensity within trials and were least sensitive to effects of wind speed and dry ice form (block vs. pellet) on baiting intensity. Results of trials involving traps baited with carbon dioxide released from pressurized cylinders suggested that this trap type had performance comparable to dry ice-baited insulated cooler traps but at considerably higher cost. © The Author 2015. Published by Oxford University Press on behalf of the Entomological Society of America.

Method for reducing sulfate formation during regeneration of hot-gas desulfurization sorbents

DOEpatents

Bissett, Larry A.; Strickland, Larry D.; Rockey, John M.

1994-01-01

The regeneration of sulfur sorbents having sulfate forming tendencies and used for desulfurizing hot product gas streams such as provided by coal gasification is provided by employing a two-stage regeneration method. Air containing a sub-stoichiometric quantity of oxygen is used in the first stage for substantially fully regenerating the sorbent without sulfate formation and then regeneration of the resulting partially regenerated sorbent is completed in the second stage with air containing a quantity of oxygen slightly greater than the stoichiometric amount adequate to essentially fully regenerate the sorbent. Sulfate formation occurs in only the second stage with the extent of sulfate formation being limited only to the portion of the sulfur species contained by the sorbent after substantially all of the sulfur species have been removed therefrom in the first stage.

Advanced Sorbent Structure Recovery of REEs, Precious Metals and Other Valuable Metals from Geothermal Waters and Its Associated Technoeconomics

DOE Data Explorer

Addleman, Shane; Chouyyok, Wilaiwan; Palo, Daniel; Dunn, Brad M.; Brann, Michelle; Billingsley, Gary; Johnson, Darren; Nell, Kara M.

2017-05-25

This work evaluates, develops and demonstrates flexible, scalable mineral extraction technology for geothermal brines based upon solid phase sorbent materials with a specific focus upon rare earth elements (REEs). The selected organic and inorganic sorbent materials demonstrated high performance for collection of trace REEs, precious and valuable metals beyond commercially available sorbents. This report details the organic and inorganic sorbent uptake, performance, and collection efficiency results for La, Eu, Ho, Ag, Cu and Zn, as well as the characterization of these select sorbent materials. The report also contains estimated costs from an in-depth techno-economic analysis of a scaled up separation process. The estimated financial payback period for installing this equipment varies between 3.3 to 5.7 years depending on the brine flow rate of the geothermal resource.

MOF-5(Zn)-Fe2O4 nanocomposite based magnetic solid-phase microextraction followed by HPLC-UV for efficient enrichment of colchicine in root of colchicium extracts and plasma samples.

PubMed

Bahrani, Sonia; Ghaedi, Mehrorang; Dashtian, Kheibar; Ostovan, Abbas; Mansoorkhani, Mohammad Javad Khoshnood; Salehi, Amin

2017-11-01

In present work, facile method is developed for determination of colchicine in human plasma sample, autumn and spring root of colchicium extracts by ultrasound assisted dispersive magnetic solid phase microextraction followed by HPLC-UV method (UAD-MSPME-HPLC-UV). Magnetic (Fe 2 O 4 -nanoparticles) metal organic framework-5, (MOF-5(Zn)-Fe 2 O 4 NPs) was synthesized by dispersing MOF-5 and Fe(NO 3 ) 3 .9H 2 O in ethylene glycol (as capping agent) and NaOH (pH adjustment agent) by hydrothermal method. The prepared sorbent was characterized via XRD and SEM analysis and applied as magnetic solid phase in UAD-MSPME-HPLC-UV method. In this method, colchicine molecules were sorbed on MOF-5(Zn)-Fe 2 O 4 NPs sorbent by various mechanisms like ion exchange, hydrogen bonding and electrostatic, ᴨ-ᴨ, hard-hard and dipole-ion interaction followed by exposing sonication waves as incremental mass transfer agent and then the sorbent was separated from the sample matrix by an external magnetic fields. Subsequently, accumulated colchicine were eluted by small volume of desorption organic solvent. Influence of operational variables such as MOF-5(Zn)-Fe 2 O 4 NPs mass, volume of extracting solvent and sonication time on response property (recovery) were studied and optimized by central composite design (CCD) combined with desirability function (DF) approach. Under optimum condition, the method has wide linear calibration rang (0.5-1700ngmL -1 ) with reasonable detection limit (0.13ngmL -1 ) and R 2 =0.9971. Finally, the UAD-MSPME-HPLC-UV method was successfully applied for determination of colchicine autumn and spring root of colchicium extracts and plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of heavy metal ions in vegetable samples using a magnetic metal-organic framework nanocomposite sorbent.

PubMed

Hassanpour, Akbar; Hosseinzadeh-Khanmiri, Rahim; Babazadeh, Mirzaagha; Abolhasani, Jafar; Ghorbani-Kalhor, Ebrahim

2015-01-01

This paper describes the synthesis and application of a novel magnetic metal-organic framework (MOF) [(Fe₃O₄-benzoyl isothiocyanate)/Cu₃(benzene-1,3,5-tricarboxylate)₂] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box-Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l(-1) EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml(-1) for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l(-1) of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe₃O₄-benzoyl isothiocyanate)/MOF] was 175 mg g(-1) for Cd(II), 168 mg g(-1) for Pb(II), 210 mg g(-1) for Zn(II) and 196 mg g(-1) for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe₃O₄-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.

A comparison study of nanofiber, microfiber, and new composite nano/microfiber polymers used as sorbents for on-line solid phase extraction in chromatography system.

PubMed

Háková, Martina; Havlíková, Lucie Chocholoušová; Chvojka, Jiří; Erben, Jakub; Solich, Petr; Švec, František; Šatínský, Dalibor

2018-09-06

Three different approaches has been used to obtain nano/micro fibers and their diversity and extraction properties were examined. The effect of their structure on stability in an ultra-high-performance liquid chromatography (UHPLC) system during on-line SPE procedure was monitored. Five types of various nano/micro fiber polymers were used as sorbents: polyamide 6 nanofibers, polyvinylidene difluoride nanofibers, polyethylene microfibers, and two new polycaprolactone microfiber/nanofiber and polycaprolactone microfibers/polyvinylidene difluoride nanofibers composite polymers. The fiber polymers were filled in a cartridge directly connected to the UHPLC system and tested. For each polymer, the optimal conditions of the on-line extraction were found and potential applicability on real samples was tested. The determination of ochratoxin A (OTA) in beer matrix was chosen as a case study. Relevant factors such as the mechanical and chemical stability of the nano/microfibers, filling the cartridges, fiber reusability and the possibility and the repeatability of all processes were involved in the proposed study. A new nano/micro composite sorbent consisting of polycaprolactone microfibers/polyvinylidene difluoride nanofibers was chosen as the most suitable sorbent for the on-line extraction of OTA from a beer matrix. The tested validation parameters had the value of intra-day precision lower than 1.48%, linearity in the range from 0.5 to 100 μg L -1 with r 2  ≥ 0.9999 for standard and matrix calibration curve, and recovery in the range 99.1-103.9% at five concentration levels. Long-term precision evaluated for 31 analyses over the period of three months did not exceed 2.9% RSD. It confirmed the column reusability and perfect stability of nano/micro composite sorbent in the presence of organic solvents and after repeated injection of a complex beer matrix. Copyright © 2018 Elsevier B.V. All rights reserved.

Carbon-Containing Waste of Coal Enterprises in Magnetic Sorbents Technology

NASA Astrophysics Data System (ADS)

Kvashevaya, Ekaterina; Ushakova, Elena; Ushakov, Andrey

2017-11-01

The article shows the issues state of coal-mining enterprises carbonaceous wastes utilization, including by obtaining oil-sorbent. The characteristics of the feedstock are presented; experiment methods of obtaining a binder based on the livestock enterprises waste, of forming binder with filler (sawdust, coal waste); of pyrogenetic processing to obtain a sorbent are described. Possible options for the introduction of magnetite (a magnetic component) in the composition of the oil sorbent are considered: on the surface, in the volume of the granule and the magnetite core. In the course of the work it was found that the optimum content of coal dust in the sorbent granules is 75% by weight, and the most effective way of obtaining the magnetic sorbent is to apply the carbon material directly to the "core" of magnetite. However, in this case, the problem of finding an effective binder for magnetite arises. The option of applying magnetite on the surface of a carbon sorbent is not effective. Thus, at present, we use a mixture of coal waste, which binds to the uniform distribution of magnetite in the volume. The developed magnetic sorbents can be used in various weather conditions, including strong winds and icing of water bodies, as well as for small and medium currents.

Simultaneous control of Hg0, SO2, and NOx by novel oxidized calcium-based sorbents.

PubMed

Ghorishi, S Behrooz; Singer, Carl F; Jozewicz, Wojciech S; Sedman, Charles B; Srivastava, Ravi K

2002-03-01

Efforts to develop multipollutant control strategies have demonstrated that adding certain oxidants to different classes of Ca-based sorbents leads to a significant improvement in elemental Hg vapor (Hg0), SO2, and NOx removal from simulated flue gases. In the study presented here, two classes of Ca-based sorbents (hydrated limes and silicate compounds) were investigated. A number of oxidizing additives at different concentrations were used in the Ca-based sorbent production process. The Hg0, SO2, and NOx capture capacities of these oxidant-enriched sorbents were evaluated and compared to those of a commercially available activated carbon in bench-scale, fixed-bed, and fluid-bed systems. Calcium-based sorbents prepared with two oxidants, designated C and M, exhibited Hg0 sorption capacities (approximately 100 microg/g) comparable to that of the activated carbon; they showed far superior SO2 and NOx sorption capacities. Preliminary cost estimates for the process utilizing these novel sorbents indicate potential for substantial lowering of control costs, as compared with other processes currently used or considered for control of Hg0, SO2, and NOx emissions from coal-fired boilers. The implications of these findings toward development of multipollutant control technologies and planned pilot and field evaluations of more promising multipollutant sorbents are summarily discussed.

Sorption of agrochemical model compounds by sorbent materials containing beta-cyclodextrin.

PubMed

Wilson, Lee D; Mohamed, Mohamed H; Guo, Rui; Pratt, Dawn Y; Kwon, Jae Hyuck; Mahmud, Sarker T

2010-04-01

Polymeric sorbent materials that incorporate beta-cyclodextrin (CD) have been prepared and their sorption behavior toward two model agrochemical contaminant compounds, p-nitrophenol (PNP) and methyl chloride examined. The sorption of PNP was studied in aqueous solution using ultraviolet-visible (UV-Vis) spectroscopy, whereas the sorption of methyl chloride from the gas phase was studied using a Langmuir adsorption method. The sorption results for PNP in solution were compared between granular activated carbon (GAC), modified GAC, CD copolymers, and CD-based mesoporous silica hybrid materials. Nitrogen porosimetry at 77 K was used to estimate the surface area and pore structure properties of the sorbent materials. The sorbents displayed variable surface areas as follows: copolymers (36.2-157 m(2)/g), CD-silica materials (307-906 m(2)/g), surface modified GAC (657 m(2)/g), and granular activated carbon (approximately 10(3) m(2)/g). The sorption capacities for PNP and methyl chloride with the different sorbents are listed in descending order as follows: GAC > copolymers > surface modified GAC > CD-silica hybrid materials. In general, the differences in the sorption properties of the sorbents were related to the following: (i) surface area of the sorbent, (ii) CD content and accessibility, (iii) and the chemical nature of the sorbent material.

Sorbent-based Oxygen Production for Energy Systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sethi, Vijay

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 CO 2 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 majormore » advancement in air separation technology. Newly developed perovskite ceramic sorbent materials with order-disorder transition have a higher O 2 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.« less

Building a better sticky trap: description of an easy-to-use trap and pole mount for quantifying the abundance of adult aquatic insects

USGS Publications Warehouse

Smith, Joshua T.; Kennedy, Theodore A.; Muehlbauer, Jeffrey D.

2014-01-01

Insect emergence is a fundamental process in freshwaters. It is a critical life-history stage for aquatic insects and provides an important prey resource for terrestrial and aquatic consumers. Sticky traps are increasingly being used to sample these insects. The most common design consists of an acetate sheet coated with a nondrying adhesive that is attached to a wire frame or cylinder. These traps must be prepared at the deployment site, a process that can be time consuming and difficult given the vagaries of field conditions. Our goals were to develop a sturdy, low-cost sticky trap that could be prepared in advance, rapidly deployed and recovered in the field, and used to estimate the flight direction of insects. We used 150-mm Petri dishes with lids. The dishes can be coated cleanly and consistently with Tangle-Trap® adhesive. Deploying traps is simple and requires only a pole set near the body of water being sampled. Four dishes can be attached to the pole using Velcro and aligned in 4 different directions to enable quantification of insect flight direction. After sampling, Petri dishes can be taped closed, packed in boxes, and stored indefinitely. Petri traps are comparable in price to standard acetate sheet traps at ∼US$0.50/directional deployment, but they require more space for storage than acetate sheet traps. However, a major benefit of Petri traps is that field deployment times are ⅓ those of acetate traps. Our study demonstrated that large Petri dishes are an ideal platform for sampling postemergent adult aquatic insects, particularly when the study design involves estimating flight direction and when rapid deployment and recovery of traps is critical.

Comparison of Bottomless Lift Nets and Breder Traps for Sampling Salt-Marsh Nekton

EPA Pesticide Factsheets

Data set contains: the length of mummichogs (Fundulus heteroclitus) caught on lift nets and Breder traps from May to September 2002; the sizes of green crabs caught in the lift nets and Breder traps during same time frame; the mean density and sample size data for each sampling time and each site (3 sites total) for total nekton sampled and total nekton minus shrimp.This dataset is associated with the following publication:Raposa, K., and M. Chintala. Comparison of Bottomless Lift Nets and Breder Traps for Sampling Salt-Marsh Nekton. TRANSACTIONS OF THE AMERICAN FISHERIES SOCIETY. American Fisheries Society, Bethesda, MD, USA, 145(1): 163-172, (2016).

A transient performance method for CO2 removal with regenerable adsorbents

NASA Technical Reports Server (NTRS)

Hwang, K. C.

1972-01-01

A computer program is described which can be used to predict the transient performance of vacuum-desorbed sorbent beds for CO2 or water removal, and composite beds of two sorbents for simultaneous humidity control and CO2 removal. The program was written primarily for silica gel and molecular sieve inorganic sorbents, but can be used for a variety of adsorbent materials. Part 2 of this report describes a computer program which can be used to predict performance for multiple-bed CO2-removal sorbent systems. This program is an expanded version of the composite sorbent bed program described in Part 1.

Method and system for radioisotope generation

DOEpatents

Toth, James J.; Soderquist, Chuck Z.; Greenwood, Lawrence R.; Mattigod, Shas V.; Fryxell, Glen E.; O'Hara, Matthew J.

2014-07-15

A system and a process for producing selected isotopic daughter products from parent materials characterized by the steps of loading the parent material upon a sorbent having a functional group configured to selectively bind the parent material under designated conditions, generating the selected isotopic daughter products, and eluting said selected isotopic daughter products from the sorbent. In one embodiment, the process also includes the step of passing an eluent formed by the elution step through a second sorbent material that is configured to remove a preselected material from said eluent. In some applications a passage of the material through a third sorbent material after passage through the second sorbent material is also performed.

Sequential capture of CO2 and SO2 in a pressurized TGA simulating FBC conditions.

PubMed

Sun, Ping; Grace, John R; Lim, C Jim; Anthony, Edward J

2007-04-15

Four FBC-based processes were investigated as possible means of sequentially capturing SO2 and CO2. Sorbent performance is the key to their technical feasibility. Two sorbents (a limestone and a dolomite) were tested in a pressurized thermogravimetric analyzer (PTGA). The sorbent behaviors were explained based on complex interaction between carbonation, sulfation, and direct sulfation. The best option involved using limestone or dolomite as a SO2-sorbent in a FBC combustor following cyclic CO2 capture. Highly sintered limestone is a good sorbent for SO2 because of the generation of macropores during calcination/carbonation cycling.

A simple technique for trapping Siren lacertina, Amphiuma means, and other aquatic vertebrates

USGS Publications Warehouse

Johnson, S.A.; Barichivich, W.J.

2004-01-01

We describe a commercially-available funnel trap for sampling aquatic vertebrates. The traps can be used in heavily vegetated wetlands and can be set in water up to 60 cm deep without concern for drowning the animals. They were especially useful for capturing the aquatic salamanders Siren lacertina and Amphiuma means, which have been difficult to capture with traditional sampling methods. They also were effective for sampling small fishes, particularly centrarchids, and larval anurans. In total, 14 species of amphibians, nine species of aquatic reptiles, and at least 32 fish species were captured. The trap we describe differs significantly from traditional funnel traps (e.g., minnow traps) and holds great promise for studies of small, aquatic vertebrates, in particular Siren and Amphiuma species.

Evaluation of common methods for sampling invertebrate pollinator assemblages: net sampling out-perform pan traps.

PubMed

Popic, Tony J; Davila, Yvonne C; Wardle, Glenda M

2013-01-01

Methods for sampling ecological assemblages strive to be efficient, repeatable, and representative. Unknowingly, common methods may be limited in terms of revealing species function and so of less value for comparative studies. The global decline in pollination services has stimulated surveys of flower-visiting invertebrates, using pan traps and net sampling. We explore the relative merits of these two methods in terms of species discovery, quantifying abundance, function, and composition, and responses of species to changing floral resources. Using a spatially-nested design we sampled across a 5000 km(2) area of arid grasslands, including 432 hours of net sampling and 1296 pan trap-days, between June 2010 and July 2011. Net sampling yielded 22% more species and 30% higher abundance than pan traps, and better reflected the spatio-temporal variation of floral resources. Species composition differed significantly between methods; from 436 total species, 25% were sampled by both methods, 50% only by nets, and the remaining 25% only by pans. Apart from being less comprehensive, if pan traps do not sample flower-visitors, the link to pollination is questionable. By contrast, net sampling functionally linked species to pollination through behavioural observations of flower-visitation interaction frequency. Netted specimens are also necessary for evidence of pollen transport. Benefits of net-based sampling outweighed minor differences in overall sampling effort. As pan traps and net sampling methods are not equivalent for sampling invertebrate-flower interactions, we recommend net sampling of invertebrate pollinator assemblages, especially if datasets are intended to document declines in pollination and guide measures to retain this important ecosystem service.

Evaluation of Common Methods for Sampling Invertebrate Pollinator Assemblages: Net Sampling Out-Perform Pan Traps

PubMed Central

Popic, Tony J.; Davila, Yvonne C.; Wardle, Glenda M.

2013-01-01

Methods for sampling ecological assemblages strive to be efficient, repeatable, and representative. Unknowingly, common methods may be limited in terms of revealing species function and so of less value for comparative studies. The global decline in pollination services has stimulated surveys of flower-visiting invertebrates, using pan traps and net sampling. We explore the relative merits of these two methods in terms of species discovery, quantifying abundance, function, and composition, and responses of species to changing floral resources. Using a spatially-nested design we sampled across a 5000 km2 area of arid grasslands, including 432 hours of net sampling and 1296 pan trap-days, between June 2010 and July 2011. Net sampling yielded 22% more species and 30% higher abundance than pan traps, and better reflected the spatio-temporal variation of floral resources. Species composition differed significantly between methods; from 436 total species, 25% were sampled by both methods, 50% only by nets, and the remaining 25% only by pans. Apart from being less comprehensive, if pan traps do not sample flower-visitors, the link to pollination is questionable. By contrast, net sampling functionally linked species to pollination through behavioural observations of flower-visitation interaction frequency. Netted specimens are also necessary for evidence of pollen transport. Benefits of net-based sampling outweighed minor differences in overall sampling effort. As pan traps and net sampling methods are not equivalent for sampling invertebrate-flower interactions, we recommend net sampling of invertebrate pollinator assemblages, especially if datasets are intended to document declines in pollination and guide measures to retain this important ecosystem service. PMID:23799127

Experimentally validated mathematical model of analyte uptake by permeation passive samplers.

PubMed

Salim, F; Ioannidis, M; Górecki, T

2017-11-15

A mathematical model describing the sampling process in a permeation-based passive sampler was developed and evaluated numerically. The model was applied to the Waterloo Membrane Sampler (WMS), which employs a polydimethylsiloxane (PDMS) membrane as a permeation barrier, and an adsorbent as a receiving phase. Samplers of this kind are used for sampling volatile organic compounds (VOC) from air and soil gas. The model predicts the spatio-temporal variation of sorbed and free analyte concentrations within the sampler components (membrane, sorbent bed and dead volume), from which the uptake rate throughout the sampling process can be determined. A gradual decline in the uptake rate during the sampling process is predicted, which is more pronounced when sampling higher concentrations. Decline of the uptake rate can be attributed to diminishing analyte concentration gradient within the membrane, which results from resistance to mass transfer and the development of analyte concentration gradients within the sorbent bed. The effects of changing the sampler component dimensions on the rate of this decline in the uptake rate can be predicted from the model. Performance of the model was evaluated experimentally for sampling of toluene vapors under controlled conditions. The model predictions proved close to the experimental values. The model provides a valuable tool to predict changes in the uptake rate during sampling, to assign suitable exposure times at different analyte concentration levels, and to optimize the dimensions of the sampler in a manner that minimizes these changes during the sampling period.

Simulation of mercury capture by sorbent injection using a simplified model.

PubMed

Zhao, Bingtao; Zhang, Zhongxiao; Jin, Jing; Pan, Wei-Ping

2009-10-30

Mercury pollution by fossil fuel combustion or solid waste incineration is becoming the worldwide environmental concern. As an effective control technology, powdered sorbent injection (PSI) has been successfully used for mercury capture from flue gas with advantages of low cost and easy operation. In order to predict the mercury capture efficiency for PSI more conveniently, a simplified model, which is based on the theory of mass transfer, isothermal adsorption and mass balance, is developed in this paper. The comparisons between theoretical results of this model and experimental results by Meserole et al. [F.B. Meserole, R. Chang, T.R. Carrey, J. Machac, C.F.J. Richardson, Modeling mercury removal by sorbent injection, J. Air Waste Manage. Assoc. 49 (1999) 694-704] demonstrate that the simplified model is able to provide good predictive accuracy. Moreover, the effects of key parameters including the mass transfer coefficient, sorbent concentration, sorbent physical property and sorbent adsorption capacity on mercury adsorption efficiency are compared and evaluated. Finally, the sensitive analysis of impact factor indicates that the injected sorbent concentration plays most important role for mercury capture efficiency.

Highly attrition-resistant zinc oxide-based sorbents for H{sub 2}S removal by spray-drying technique

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, J.B.; Baek, J.I.; Ryu, C.K.

2008-07-15

A ZnO-based sorbent, ZAC 32N, applicable to transport reactors was successfully prepared by the spray-drying technique. Another sorbent, ZAC 32SU, was prepared by scale-up preparation of ZAC 32N sorbent. The physical properties of the sorbents such as attrition resistance, specific surface area, pore volume, and particle size were extensively characterized and exhibited a good potential for use in transport applications. The chemical reactivity tested in the thermogravimetric analyzer and microreactor exhibited desirable characteristics for effective desulfurization of syngas streams in the range of 450-550{sup o}C. Bench-scale tests for the sorbent ZAC 32SU were performed for a continuous 160 h withmore » a steady solid circulation of 54.6 kg/h. The results showed 99.5%+ desulfurization at 500-550{sup o}C and reasonable regenerability at 550-620{sup o}C. Test results on the physical properties and chemical reactivity indicated that the performance of developed sorbents proved to be outstanding.« less

Evaluation of polar organic chemical integrative and hollow fibre samplers for the determination of a wide variety of organic polar compounds in seawater.

PubMed

Mijangos, Leire; Ziarrusta, Haizea; Prieto, Ailette; Zugazua, Oihane; Zuloaga, Olatz; Olivares, Maitane; Usobiaga, Aresatz; Paschke, Albrecht; Etxebarria, Nestor

2018-08-01

The calibration of two passive samplers for the determination of 20 emerging organic compounds in seawater is described in this work: i) a new version of polar organic chemical integrative sampler (POCIS) containing 100 mg of mixed-mode anion exchanger (Strata X-AW) and 100 mg of polymeric HLB (Plexa) sorbent materials and using a highly porous Nylon membrane (30-μm pore size) and ii) polyethersulfone (PES) hollow fibre. Among the studied contaminants, herbicides, hormones, life style products (stimulants and artificial sweeteners), industrial chemicals (corrosion inhibitor and fluorinated compounds), personal care products and several pharmaceuticals were included. In the case of POCIS, both the sorbents and the Nylon membranes were extracted and analysed independently. The calibration set up consisted on a continuous-flow tank that was fed with a continuous flow of seawater (2 L/h) and a stock mixture of contaminants (20 mL/h), assuring a nominal concentration of ~ 600 ng/L (each analyte) in the tank. The uptake was linear in POCIS sorbent and Nylon membranes but exponential for PES hollow fibres. Furthermore, the highest sampling rates (Rs) values were obtained in POCIS sorbent (between 2.7 for acetaminophen and 491 mL/day for perfluoro-n-octanoic acid, PFOA) followed by Nylon membranes (between 3.6 for OBT and 50 mL/day for telmisartan) and the lowest were those from PES fibres (between 1.7 for bezafibrate and 157 mL/day for butylparaben). Additionally, five deuterated compounds ([ 2 H 5 ]-atrazine, [ 2 H 3 ]-amitriptyline, [ 2 H 7 ]-irbesartan, [ 2 H 3 ]-ketoprofen and [ 2 H 9 ]-progesterone) were studied as candidates for performance reference compounds (PRCs) in both POCIS and PES, and though [ 2 H 5 ]-atrazine, [ 2 H 9 ]-progesterone and [ 2 H 3 ]-amitriptyline showed acceptable results in the case of POCIS, only [ 2 H 5 ]-atrazine provided a good validation. In the case of PES fibres, the PRC corrections did not provide acceptable results due to a low dissipation of the PRCs. Finally, POCIS were deployed in two sites of the low part of the estuary of Bilbao (northern Spain) from where water samples were also taken and analysed. As a result, in addition to the overall good agreement between the passive and active samplings, passive samplers allowed the determination of several compounds that were below the detection limits in the active sampling. Copyright © 2018. Published by Elsevier B.V.

On-cartridge derivatisation using a calixarene solid-phase extraction sorbent for facile, sensitive and fast determination of formaldehyde in beer.

PubMed

Deng, Zhifen; Hu, Kai; Zhang, Yongming; Zhao, Wenjie; Wang, Fei; Guo, Ling; Zhang, Wenfen; He, Juan; Huang, Yanjie; Zhang, Shusheng

2016-11-15

This work demonstrates the successful application of an on-cartridge derivatisation procedure for facile, fast and sensitive determination of formaldehyde in beer by HPLC-UV. The derivatisation and solid-phase extraction (SPE) were integrated into a novel calixarene SPE sorbent: tetraazacalix[2]arene[2]triazine bonded silica gel. Specifically, 2,4-dinitrophenylhydrazine was adsorbed onto the sorbent in advance, based on the charge-transfer interaction between the macrocyclic molecule and nitrobenzenes. The method was optimised and validated: under the optimal conditions of derivatisation, SPE and HPLC separation, good linearity was obtained in the range of 0.080-3.2μgmL(-1) with a correlation coefficient of 0.9939, the limit of detection was 3.0ngmL(-1) (S/N=3), the limit of quantification was 10ngmL(-1) (S/N=10), and the recovery level using this method was desirable at 75-84%. The developed method was successfully applied to determine formaldehyde content in real beer samples; the results were in the range of 0.11-1.1μgmL(-1). Copyright © 2016. Published by Elsevier Ltd.

Fast-regenerable sulfur dioxide adsorbents for diesel engine emission control

DOEpatents

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

2011-03-15

Disclosed herein are sorbents and devices for controlling sulfur oxides emissions as well as systems including such sorbents and devices. Also disclosed are methods for making and using the disclosed sorbents, devices and systems. In one embodiment the disclosed sorbents can be conveniently regenerated, such as under normal exhaust stream from a combustion engine, particularly a diesel engine. Accordingly, also disclosed are combustion vehicles equipped with sulfur dioxide emission control devices.

Method And Apparatus For Production Of Bi-213 From The Activity Ac-225 Source

DOEpatents

Egorov, Oleg B.; O'Hara, Matthew J.

2005-12-06

A method and apparatus for isolating and purifying a .sup.213 Bi radioactive isotope from an .sup.225 Ac source using a primary column and a primary sorbent which preferentially retains .sup.225 Ac over .sup.213 Bi when exposed to a compatible solvent in combination with a secondary column having a secondary sorbent which retains .sup.213 Bi when exposed to a mixture of the compatible solvent and .sup.213 Bi. A "compatible solvent" is a solvent which will preferentially remove .sup.213 Bi radioactive isotopes from a primary sorbent without removing .sup.225 Ac radioactive isotopes, and then allow .sup.213 Bi radioactive isotopes removed from the primary sorbent to be retained on a secondary sorbent, without having to dilute or otherwise chemically or physically modify the compatible solvent in between exposure to the primary and secondary sorbents.

Desulfurization sorbent regeneration

DOEpatents

Jalan, V.M.; Frost, D.G.

1982-07-07

A spent solid sorbent resulting from the removal of hydrogen sulfide from a fuel gas flow is regenerated with a steam-air mixture. The mixture of steam and air may also include additional nitrogen or carbon dioxide. The gas mixture contacts the spent sorbent containing metal sulfide at a temperature above 500/sup 0/C to regenerate the sulfide to metal oxide or carbonate. Various metal species including the period four transition metals and the lanthanides are suitable sorbents that may be regenerated by this method. In addition, the introduction of carbon dioxide gas permits carbonates such as those of strontium, barium and calcium to be regenerated. The steam permits regeneration of spent sorbent without formation of metal sulfate. Moreover, the regeneration will proceed with low oxygen concentrations and will occur without the increase in temperature to minimize the risk of sintering and densification of the sorbent. This method may be used for high-temperature fuel cells.

Screening of zinc-based sorbents for hot-gas desulfurization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joong B. Lee; Chong K. Ryu; Chang K. Yi

2008-03-15

Highly reactive and attrition-resistant ZnO-based sorbents that are suitable for bubbling fluidized-bed reactors can be produced using the spray-drying method. Most of the ZnO-based sorbents prepared here (ZAC-X, X = 18N-25N) satisfy the physical and chemical criteria for bubbling fluidized-bed application (spherical shape, average particle size, 90-110 {mu}m; size distribution, 40-230 {mu}m; bulk density, 0.9-1.0 g/mL; attrition index (AI), 40-80%; sulfur sorption capacity, 14-17 wt %; sorbent use, 70-80%). The performance test of the ZAC-C sorbent at Korea Institute of Energy Research (KIER) with a bubbling fluidized-bed for 70 h also demonstrated that it had good sulfidation and regeneration performancemore » (11 wt % sorption capacity and 52% sorbent use) as well as reasonable attrition resistance (1.1% attrition loss for 70 h). 14 refs., 7 figs., 6 tabs.« less

Nanostructured Metal Oxide Sorbents for the Collection and Recovery of Uranium from Seawater

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chouyyok, Wilaiwan; Warner, Cynthia L.; Mackie, Katherine E.

2016-02-07

The ability to collect uranium from seawater offers the potential for a long-term green fuel supply for nuclear energy. However, extraction of uranium, and other trace minerals, is challenging due to the high ionic strength and low mineral concentrations in seawater. Herein we evaluate the use of nanostructured metal oxide sorbents for the collection and recovery of uranium from seawater. Chemical affinity, chemical adsorption capacity and kinetics of preferred sorbent materials were evaluated. High surface area manganese and iron oxide nanomaterials showed excellent performance for uranium collection from seawater. Inexpensive nontoxic carbonate solutions were demonstrated to be an effective andmore » environmental benign method of stripping the uranium from the metal oxide sorbents. Various formats for the utilization of the nanostructured metals oxide sorbent materials are discussed including traditional and nontraditional methods such as magnetic separation. Keywords: Uranium, nano, manganese, iron, sorbent, seawater, magnetic, separations, nuclear energy« less

Regenerative process for removal of mercury and other heavy metals from gases containing H.sub.2 and/or CO

DOEpatents

Jadhav, Raja A [Naperville, IL

2009-07-07

A method for removal of mercury from a gaseous stream containing the mercury, hydrogen and/or CO, and hydrogen sulfide and/or carbonyl sulfide in which a dispersed Cu-containing sorbent is contacted with the gaseous stream at a temperature in the range of about 25.degree. C. to about 300.degree. C. until the sorbent is spent. The spent sorbent is contacted with a desorbing gaseous stream at a temperature equal to or higher than the temperature at which the mercury adsorption is carried out, producing a regenerated sorbent and an exhaust gas comprising released mercury. The released mercury in the exhaust gas is captured using a high-capacity sorbent, such as sulfur-impregnated activated carbon, at a temperature less than about 100.degree. C. The regenerated sorbent may then be used to capture additional mercury from the mercury-containing gaseous stream.

Nonvolatile memories using deep traps formed in HfO2 by Nb ion implantation

NASA Astrophysics Data System (ADS)

Choul Kim, Min; Oh Kim, Chang; Taek Oh, Houng; Choi, Suk-Ho; Belay, K.; Elliman, R. G.; Russo, S. P.

2011-03-01

We report nonvolatile memories (NVMs) based on deep-energy trap levels formed in HfO2 by metal ion implantation. A comparison of Nb- and Ta-implanted samples shows that suitable charge-trapping centers are formed in Nb-implanted samples, but not in Ta-implanted samples. This is consistent with density-functional theory calculations which predict that only Nb will form deep-energy levels in the bandgap of HfO2. Photocurrent spectroscopy exhibits characteristics consistent with one of the trap levels predicted in these calculations. Nb-implanted samples showing memory windows in capacitance-voltage (V) curves always exhibit current (I) peaks in I-V curves, indicating that NVM effects result from deep traps in HfO2. In contrast, Ta-implanted samples show dielectric breakdowns during the I-V sweeps between 5 and 11 V, consistent with the fact that no trap levels are present. For a sample implanted with a fluence of 1013 Nb cm-2, the charge losses after 104 s are ˜9.8 and ˜25.5% at room temperature (RT) and 85°C, respectively, and the expected charge loss after 10 years is ˜34% at RT, very promising for commercial NVMs.

Nanohole optical tweezers in heterogeneous mixture analysis

NASA Astrophysics Data System (ADS)

Hacohen, Noa; Ip, Candice J. X.; Laxminarayana, Gurunatha K.; DeWolf, Timothy S.; Gordon, Reuven

2017-08-01

Nanohole optical trapping is a tool that has been shown to analyze proteins at the single molecule level using pure samples. The next step is to detect and study single molecules with dirty samples. We demonstrate that using our double nanohole optical tweezing configuration, single particles in an egg white solution can be classified when trapped. Different sized molecules provide different signal variations in their trapped state, allowing the proteins to be statistically characterized. Root mean squared variation and trap stiffness are methods used on trapped signals to distinguish between the different proteins. This method to isolate and determine single molecules in heterogeneous samples provides huge potential to become a reliable tool for use within biomedical and scientific communities.

Method of CO.sub.2 removal from a gasesous stream at reduced temperature

DOEpatents

Fisher, James C; Siriwardane, Ranjani V; Berry, David A; Richards, George A

2014-11-18

A method for the removal of H.sub.2O and CO.sub.2 from a gaseous stream comprising H.sub.2O and CO.sub.2, such as a flue gas. The method initially utilizes an H.sub.2O removal sorbent to remove some portion of the H.sub.2O, producing a dry gaseous stream and a wet H.sub.2O removal sorbent. The dry gaseous stream is subsequently contacted with a CO.sub.2 removal sorbent to remove some portion of the CO.sub.2, generating a dry CO.sub.2 reduced stream and a loaded CO.sub.2 removal sorbent. The loaded CO.sub.2 removal sorbent is subsequently heated to produce a heated CO.sub.2 stream. The wet H.sub.2O removal sorbent and the dry CO.sub.2 reduced stream are contacted in a first regeneration stage, generating a partially regenerated H.sub.2O removal sorbent, and the partially regenerated H.sub.2O removal sorbent and the heated CO.sub.2 stream are subsequently contacted in a second regeneration stage. The first and second stage regeneration typically act to retain an initial monolayer of moisture on the various removal sorbents and only remove moisture layers bound to the initial monolayer, allowing for relatively low temperature and pressure operation. Generally the applicable H.sub.2O sorption/desorption processes may be conducted at temperatures less than about 70.degree. C. and pressures less than 1.5 atmospheres, with certain operations conducted at temperatures less than about 50.degree. C.

Analysis of Ethane and Diethylbenzene Bridged Sorbents

DTIC Science & Technology

2017-12-13

Leska; P.T. Charles; B.J. Melde; J.R. Taft, "Electrochemical Detection with Preconcentration: Nitroenergetic Contaminants ," Chemosensors 2, 131...monitoring of contaminants in groundwater: Sorbent development; Naval Research Laboratory: 2013. Analysis of Ethane and Diethylbenzene Bridged Sorbents 7...

Electromembrane extraction of tartrazine from food samples: Effects of nano-sorbents on membrane performance.

PubMed

Yaripour, Saeid; Mohammadi, Ali; Nojavan, Saeed

2016-07-01

In the present study, for the first time electromembrane extraction followed by high-performance liquid chromatography coupled with ultraviolet detection was developed and validated for the determination of tartrazine in some food samples. The parameters influencing electromembrane extraction were evaluated and optimized. The membrane consists of 1-octanol immobilized in the pores of a hollow fiber. As a driving force, a 30 V electrical field was applied to make the analyte migrate from sample solution with pH 3, through the supported liquid membrane into an acceptor solution with pH 10. Best preconcentration (enrichment factor >21) was obtained in extraction duration of 15 min. Effects of some solid nano-sorbents like carbon nanotubes and molecularly imprinted polymers on membrane performance and electromembrane extraction efficiency were evaluated. The method provided the linearity in the range 25-1000 ng/mL for tartrazine (R(2) > 0.9996) with repeatability range (RSD) between 3.8 and 8.5% (n = 3). The limits of detection and quantitation were 7.5 and 25 ng/mL, respectively. Finally, the method was applied to the determination and quantification of tartrazine from some food samples with relative recoveries in the range between 90 and 98%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Application of a thiourea-containing task-specific ionic liquid for the solid-phase extraction cleanup of lead ions from red lipstick, pine leaves, and water samples.

PubMed

Saljooqi, Asma; Shamspur, Tayebeh; Mohamadi, Maryam; Mostafavi, Ali

2014-07-01

Here, task-specific ionic liquid solid-phase extraction is proposed for the first time. In this approach, a thiourea-functionalized ionic liquid is immobilized on the solid sorbent, multiwalled carbon nanotubes. These modified nanotubes packed into a solid-phase extraction column are used for the selective extraction and preconcentration of ultra-trace amounts of lead(II) from aqueous samples prior to electrothermal atomic absorption spectroscopy determination. The thiourea functional groups act as chelating agents for lead ions retaining them and so, give the selectivity to the sorbent. Elution of the retained ions can be performed using an acidic thiourea solution. The effects of experimental parameters including pH of the aqueous solution, type and amount of eluent, and the flow rates of sample and eluent solutions on the separation efficiency are investigated. The linear dependence of absorbance of lead on its concentration in the initial solution is in the range of 0.5-40.0 ng/mL with the detection limit of 0.13 ng/mL (3(Sb)/m, n = 10). The proposed method is applicable to the analysis of red lipstick, pine leaves, and water samples for their lead contents. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of Bio-VOC Sampler for Analysis of Volatile Organic Compounds in Exhaled Breath

PubMed Central

Kwak, Jae; Fan, Maomian; Harshman, Sean W.; Garrison, Catherine E.; Dershem, Victoria L.; Phillips, Jeffrey B.; Grigsby, Claude C.; Ott, Darrin K.

2014-01-01

Monitoring volatile organic compounds (VOCs) from exhaled breath has been used to determine exposures of humans to chemicals. Prior to analysis of VOCs, breath samples are often collected with canisters or bags and concentrated. The Bio-VOC breath sampler, a commercial sampling device, has been recently introduced to the market with growing use. The main advantage for this sampler is to collect the last portion of exhaled breath, which is more likely to represent the air deep in the lungs. However, information about the Bio-VOC sampler is somewhat limited. Therefore, we have thoroughly evaluated the sampler here. We determined the volume of the breath air collected in the sampler was approximately 88 mL. When sampling was repeated multiple times, with the succeeding exhalations applied to a single sorbent tube, we observed linear relationships between the normalized peak intensity and the number of repeated collections with the sampler in many of the breath VOCs detected. No moisture effect was observed on the Tenax sorbent tubes used. However, due to the limitation in the collection volume, the use of the Bio-VOC sampler is recommended only for detection of VOCs present at high concentrations unless repeated collections of breath samples on the sampler are conducted. PMID:25532709

Comparative study of glass tube and mist chamber sampling techniques for the analysis of gaseous carbonyl compounds

NASA Astrophysics Data System (ADS)

François, Stéphanie; Perraud, Véronique; Pflieger, Maryline; Monod, Anne; Wortham, Henri

In this work, glass tube and mist chamber sampling techniques using 2,4-dinitrophenylhydrazine as derivative agent for the analysis of gaseous carbonyl compounds are compared. Trapping efficiencies of formaldehyde, acetaldehyde, propionaldehyde, acetone, acrolein, glyoxal, crotonaldehyde, benzaldehyde, butyraldehyde and valeraldehyde are experimentally determined using a gas-phase generator. In addition to generalise our results to all atmospheric gaseous compounds and derivative agents, theoretical trapping efficiencies and enrichment factors are expressed taking into account mechanisms involved in the two kinds of traps. Theoretical and experimental results show that, as expected, the trapping efficiencies of the glass tube depend mainly on solubility of compounds. The results provide new information and better understanding of phenomena occurring in the mist chamber and the ability of this sampler to concentrate the samples. Hence, the mist chamber is the more convenient sampling method when the trapping is associated to a fast derivatisation of the compounds and the glass tube technique must be used to trap atmospheric compounds without simultaneous derivatisation.

Hydride vapor phase GaN films with reduced density of residual electrons and deep traps

DOE Office of Scientific and Technical Information (OSTI.GOV)

Polyakov, A. Y., E-mail: aypolyakov@gmail.com; Smirnov, N. B.; Govorkov, A. V.

2014-05-14

Electrical properties and deep electron and hole traps spectra are compared for undoped n-GaN films grown by hydride vapor phase epitaxy (HVPE) in the regular process (standard HVPE samples) and in HVPE process optimized for decreasing the concentration of residual donor impurities (improved HVPE samples). It is shown that the residual donor density can be reduced by optimization from ∼10{sup 17} cm{sup −3} to (2–5) × 10{sup 14} cm{sup −3}. The density of deep hole traps and deep electron traps decreases with decreased donor density, so that the concentration of deep hole traps in the improved samples is reduced to ∼5 × 10{sup 13} cm{sup −3} versusmore » 2.9 × 10{sup 16} cm{sup −3} in the standard samples, with a similar decrease in the electron traps concentration.« less

Solid sorbent air sampler

NASA Technical Reports Server (NTRS)

Galen, T. J. (Inventor)

1986-01-01

A fluid sampler for collecting a plurality of discrete samples over separate time intervals is described. The sampler comprises a sample assembly having an inlet and a plurality of discreet sample tubes each of which has inlet and outlet sides. A multiport dual acting valve is provided in the sampler in order to sequentially pass air from the sample inlet into the selected sample tubes. The sample tubes extend longitudinally of the housing and are located about the outer periphery thereof so that upon removal of an enclosure cover, they are readily accessible for operation of the sampler in an analysis mode.

High specific surface area aerogel cryoadsorber for vacuum pumping applications

DOEpatents

Hill, Randal M.; Fought, Eric R.; Biltoft, Peter J.

2000-01-01

A cryogenic pumping system is provided, comprising a vacuum environment, an aerogel sorbent formed from a carbon aerogel disposed within the vacuum environment, and cooling means for cooling the aerogel sorbent sufficiently to adsorb molecules from the vacuum environment onto the aerogel sorbent. Embodiments of the invention include a liquid refrigerant cryosorption pump, a compressed helium cryogenic pump, a cryopanel and a Meissner coil, each of which uses carbon aerogel as a sorbent material.

Surface Functionalized Nanostructured Ceramic Sorbents for the Effective Collection and Recovery of Uranium from Seawater

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chouyyok, Wilaiwan; Pittman, Jonathan W.; Warner, Marvin G.

2016-05-02

The ability to collect uranium from seawater offers the potential for a nearly limitless fuel supply for nuclear energy. We evaluated the use of functionalized nanostructured sorbents for the collection and recovery of uranium from seawater. Extraction of trace minerals from seawater and brines is challenging due to the high ionic strength of seawater, low mineral concentrations, and fouling of surfaces over time. We demonstrate that rationally assembled sorbent materials that integrate high affinity surface chemistry and high surface area nanostructures into an application relevant micro/macro structure enables collection performance that far exceeds typical sorbent materials. High surface area nanostructuredmore » silica with surface chemistries composed of phosphonic acid, phosphonates, 3,4 hydroxypyridinone, and EDTA showed superior performance for uranium collection. A few phosphorous-based commercial resins, specifically Diphonix and Ln Resin, also performed well. We demonstrate an effective and environmentally benign method of stripping the uranium from the high affinity sorbents using inexpensive nontoxic carbonate solutions. The cyclic use of preferred sorbents and acidic reconditioning of materials was shown to improve performance. Composite thin films composed of the nanostructured sorbents and a porous polymer binder are shown to have excellent kinetics and good capacity while providing an effective processing configuration for trace mineral recovery from solutions. Initial work using the composite thin films shows significant improvements in processing capacity over the previously reported sorbent materials.« less

Quantitative organic vapor-particle sampler

DOEpatents

Gundel, Lara; Daisey, Joan M.; Stevens, Robert K.

1998-01-01

A quantitative organic vapor-particle sampler for sampling semi-volatile organic gases and particulate components. A semi-volatile organic reversible gas sorbent macroreticular resin agglomerates of randomly packed microspheres with the continuous porous structure of particles ranging in size between 0.05-10 .mu.m for use in an integrated diffusion vapor-particle sampler.

METHODOLOGY OF AMBIENT AIR MONITORING FOR POLYCYCLIC AROMATIC HYDROCARBONS

EPA Science Inventory

In the last decade, several studies of polycyclic aromatic hydrocarbons (PAH) in ambient air in the U.S. specifically investigated (1) the sampling efficiency of two sorbents for PAH in air: XAD-2 and polyurethane foam (PUP); (2) the storage stability of PAH on quartz fiber fil...

COMPARISON OF SODIUM AND POTASSIUM CARBONATES AS LITHIUM ZIRCONATE MODIFIERS FOR HIGH-TEMPERATURE CARBON DIOXIDE CAPTURE FROM BIOMASS-DERIVED SYNTHESIS GAS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Olstad, J.L.; Phillips, S.D.

2009-01-01

The process of gasifi cation converts biomass into synthesis gas (syngas), which can be used to produce biofuels. Solid-phase sorbents were investigated for the removal of CO2 from a N2/CO2 gas stream using a CO2 concentration similar to that found in a biomass gasifi cation process. During the gasifying process, large amounts of carbon dioxide (CO2) are created along with the syngas. The produced CO2 must be removed before the syngas can be used for fuel synthesis and to avoid the possible formation of unwanted byproducts. A thermogravimetric analyzer was used to test the CO2 absorption rates of sorbents composedmore » of lithium zirconate (Li2ZrO3), as well as mixtures of Li2ZrO3 with potassium carbonate (K2CO3) and sodium carbonate (Na2CO3). The experimental results show that Li2ZrO3 has a low absorption rate, but sorbents containing combinations of Li2ZrO3 and the K2CO3 and Na2CO3 additives have high uptake rates. Using different proportions of K2CO3 and Na2CO3 produces varying uptake rates, so an optimization experiment was performed to obtain an improved sorbent. The CO2 absorption and regeneration stability of the solid-phase sorbents were also examined. A sorbent composed of Li2ZrO3 and 12.1 weight % Na2CO3 was shown to be stable, based on the consistent CO2 uptake rates. Sorbents prepared with Li2ZrO3, 17.6 weight % K2CO3 and 18.1 weight % Na2CO3 showed instability during regeneration cycles in air at 800 °C. Sorbent stability improved during regeneration cycles at 700 °C. Further testing of the Li2ZrO3 sorbent under actual syngas conditions, including higher pressure and composition, should be done. Once the optimum sorbent has been found, a suitable support will be needed to use the sorbent in an actual reactor.« less

Multiresidue determination of carbamate, organochlorine, organophosphorus, and dicarboximide pesticides in lettuce by GC/MS.

PubMed

Da Silva, Rogério Luiz; Da Silva, Claudia Pereira; Navickiene, Sandro

2010-08-01

An extraction method based on matrix solid-phase dispersion was developed to determine pirimicarb, methyl parathion, malathion, procymidone, alpha-endosulfan and beta-endosulfan in lettuce using gas chromatography-mass spectrometry. The best results were obtained using 4.0 g of lettuce, 2.0 g of silica as dispersant sorbent, 0.1 g of activated carbon as clean up sorbent and acetonitrile as eluting solvent. The method was validated using lettuce samples fortified with pesticides at six different concentration levels (0.1 to 2.0 mg/kg). Average recoveries (7 replicates) ranged from 50 to 120%, with relative standard deviations between 0.6 and 8.0%. Detection and quantification limits for lettuce ranged from 0.01 to 0.02 mg/kg and 0.04 to 0.10 mg/kg, respectively.

Selective extraction based on poly(MAA-VB-EGMDA) monolith followed by HPLC for determination of hordenine in plasma and urine samples.

PubMed

Chen, Yonggang; Meng, Junhua; Zou, Jili; An, Jing

2015-06-01

Hordenine is an active compound found in several foods, herbs and beer. In this work, a novel sorbent was fabricated for selective solid-phase extraction (SPE) of hordenine in biological samples. The organic polymer sorbent was synthesized in one step in the plastic barrel of a syringe by a pre-polymerization solution consisting of methacrylic acid (MAA), 4-vinylphenylboronic acid (VB) and ethylene glycol dimethacrylate (EGDMA). The conditions for preparation were optimized to generate a poly(MAA-VB-EGMDA) monolith with good permeability. The monolith exhibited good enrichment efficiency towards hordenine. By using tyramine as the internal standard, a poly(MAA-VB-EGMDA)-based SPE-HPLC method was established for analysis of hordenine. Conditions for SPE, including volume of eluting solvent, pH of sample solution, sampling rate and sample volume, were optimized. The proposed SPE-HPLC method presented good linearity (R(2)  = 0.9992) within 10-2000 ng/mL and the detection limits was 3 ng/mL, which is significantly more sensitive than reported methods. The method was also applied in plasma and urine samples; good capability of removing matrices was observed, while hordenine in low content was well extracted and enriched. The recoveries were from 90.6 to 94.7% and from 89.3 to 91.5% for the spiked plasma and urine samples, respectively, with the relative standard deviations <4.7%. Copyright © 2014 John Wiley & Sons, Ltd.

Active Search on Carcasses versus Pitfall Traps: a Comparison of Sampling Methods.

PubMed

Zanetti, N I; Camina, R; Visciarelli, E C; Centeno, N D

2016-04-01

The study of insect succession in cadavers and the classification of arthropods have mostly been done by placing a carcass in a cage, protected from vertebrate scavengers, which is then visited periodically. An alternative is to use specific traps. Few studies on carrion ecology and forensic entomology involving the carcasses of large vertebrates have employed pitfall traps. The aims of this study were to compare both sampling methods (active search on a carcass and pitfall trapping) for each coleopteran family, and to establish whether there is a discrepancy (underestimation and/or overestimation) in the presence of each family by either method. A great discrepancy was found for almost all families with some of them being more abundant in samples obtained through active search on carcasses and others in samples from traps, whereas two families did not show any bias towards a given sampling method. The fact that families may be underestimated or overestimated by the type of sampling technique highlights the importance of combining both methods, active search on carcasses and pitfall traps, in order to obtain more complete information on decomposition, carrion habitat and cadaveric families or species. Furthermore, a hypothesis advanced on the reasons for the underestimation by either sampling method showing biases towards certain families. Information about the sampling techniques indicating which would be more appropriate to detect or find a particular family is provided.

Comparative evaluation of four mosquitoes sampling methods in rice irrigation schemes of lower Moshi, northern Tanzania.

PubMed

Kweka, Eliningaya J; Mahande, Aneth M

2009-07-06

Adult malaria vector sampling is the most important parameter for setting up an intervention and understanding disease dynamics in malaria endemic areas. The intervention will ideally be species-specific according to sampling output. It was the objective of this study to evaluate four sampling techniques, namely human landing catch, pit shelter, indoor resting collection and odour-baited entry trap. These four sampling methods were evaluated simultaneously for thirty days during October 2008, a season of low mosquitoes density and malaria transmission. These trapping methods were performed in one village for maximizing homogeneity in mosquito density. The cattle and man used in odour-baited entry trap were rotated between the chambers to avoid bias. A total of 3,074 mosquitoes were collected. Among these 1,780 (57.9%) were Anopheles arabiensis and 1,294 (42.1%) were Culex quinquefasciatus. Each trap sampled different number of mosquitoes, Indoor resting collection collected 335 (10.9%), Odour-baited entry trap-cow 1,404 (45.7%), Odour-baited entry trap-human 378 (12.3%), Pit shelter 562 (18.3%) and HLC 395 (12.8%). General linear model univariate analysis method was used, position of the trapping method had no effect on mosquito density catch (DF = 4, F = 35.596, P = 0.78). Days variation had no effect on the collected density too (DF = 29, F = 4.789, P = 0.09). The sampling techniques had significant impact on the caught mosquito densities (DF = 4, F = 34.636, P < 0.0001). The Wilcoxon pair-wise comparison between mosquitoes collected in human landing catch and pit shelter was significant (Z = -3.849, P < 0.0001), human landing catch versus Indoor resting collection was not significant (Z = -0.502, P = 0.615), human landing catch versus odour-baited entry trap-man was significant (Z = -2.687, P = 0.007), human landing catch versus odour-baited entry trap-cow was significant (Z = -3.127, P = 0.002). Odour-baited traps with different baits and pit shelter have shown high productivity in collecting higher densities of mosquitoes than human landing catch. These abilities are the possibilities of replacing the human landing catch practices for sampling malaria vectors in areas with An. arabiensis as malaria vectors. Further evaluations of these sampling methods need to be investigated is other areas with different species.

The modeling of reactive solute transport with sorption to mobile and immobile sorbents 1. Experimental evidence and model development

NASA Astrophysics Data System (ADS)

Knabner, P.; Totsche, K. U.; Kögel-Knabner, I.

Modeling carrier-influenced transport needs to take into account the reactivity of the carrier itself. This paper presents a mathematical model of reactive solute transport with sorption to mobile and immobile sorbents. The mobile sorbent is also considered to be reactive. To justify the assumptions and generality of our modeling approach, experimental findings are reviewed and analyzed. A transformation of the model in terms of total concentrations of solute and mobile sorbents is presented which simplifies the mathematical formulations. Breakthrough data on dissolved organic carbon are presented to exemplify the need to take into account the reactivity of the mobile sorbent. Data on hexachlorobiphenyl and cadmium are presented to demonstrate carrier-introduced increased mobility, whereas data on anthracene and pyrene are presented to demonstrate carrier-introduced reduced mobility. The experimental conditions leading to the different findings are pointed out. The sorption processes considered in the model are both equilibrium and nonequilibrium processes, allowing for different sorption sites and nonlinear isotherms and rate functions. Effective isotherms, which describe the sorption to the immobile sorbent in the presence of a mobile sorbent and rate functions, are introduced and their properties are discussed.

Concentration and immobilization of 137Cs from liquid radioactive waste using sorbents based on hydrated titanium and zirconium oxides

NASA Astrophysics Data System (ADS)

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.

Mercury removal sorbents

DOEpatents

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.

Effect of cerium oxide doping on the performance of CaO-based sorbents during calcium looping cycles.

PubMed

Wang, Shengping; Fan, Shasha; Fan, Lijing; Zhao, Yujun; Ma, Xinbin

2015-04-21

A series of CaO-based sorbents were synthesized through a sol-gel method and doped with different amounts of CeO2. The sorbent with a Ca/Ce molar ratio of 15:1 showed an excellent absorption capacity (0.59 gCO2/g sorbent) and a remarkable cycle durability (up to 18 cycles). The admirable capture performance of CaCe-15 was ascribed to its special morphology formed by the doping of CeO2 and the well-distributed CeO2 particles. The sorbents doped with CeO2 possessed a loose shell-connected cross-linking structure, which was beneficial for the contact between CaO and CO2. CaO and CeO2 were dispersed homogeneously, and the existence of CeO2 also decreased the grain size of CaO. The well-dispersed CeO2, which could act as a barrier, effectively prevented the CaO crystallite from growing and sintering, thus the sorbent exhibited outstanding stability. The doping of CeO2 also improved the carbonation rate of the sorbent, resulting in a high capacity in a short period of time.

Iron oxide functionalized graphene nano-composite for dispersive solid phase extraction of chemical warfare agents from aqueous samples.

PubMed

Chinthakindi, Sridhar; Purohit, Ajay; Singh, Varoon; Tak, Vijay; Goud, D Raghavender; Dubey, D K; Pardasani, Deepak

2015-05-15

Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. Copyright © 2015 Elsevier B.V. All rights reserved.

Suitability of polydimethylsiloxane rods for the headspace sorptive extraction of polybrominated diphenyl ethers from water samples.

PubMed

Montes, R; Rodríguez, I; Rubí, E; Cela, R

2007-03-02

The suitability of an inexpensive polydimethysiloxane (PDMS) sorbent, produced on an industrial scale, for the extraction of polybrominated diphenyl ethers (PBDEs), from tetra- to hexabrominated congeners, from water samples was assessed. Experiments were carried out using samples spiked with a pentabromo diphenyl ether (pentaBDE) mixture, PDMS rods with a diameter of 2 mm and gas chromatography with micro-electron-capture detection (GC-micro-ECD). Influence of several variables on the efficiency of the enrichment step and the further desorption of the analytes was investigated in detail. The best performance was achieved in the headspace sorptive extraction (HSSE) mode, at 95 degrees C, using 80 mL water samples containing a 30% of sodium chloride. Extractions were performed overnight using disposable PDMS rods with a length of 10 mm (31 microL volume). Analytes were further recovered from the PDMS sorbent using just 1 mL of diethyl ether. This solvent was evaporated and extracts reconstituted with 25 microL of isooctane. Under final working conditions absolute extraction efficiencies from 69 to 93% and enrichment factors higher than 2200 folds were achieved for all species. The proposed method provided acceptable precisions (relative standard deviations values under 12%), correlation coefficients higher than 0.998 and the yield of the HSSE process remained constant for different water samples.

Halloysite nanotubes as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction for the determination of bismuth in water samples using high-resolution continuum source graphite-furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Krawczyk-Coda, Magdalena

2017-03-01

In this research, a simple, accurate, and inexpensive preconcentration procedure was developed for the determination of bismuth in water samples, using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS). During the preconcentration step, halloysite nanotubes (HNTs) were used as a solid sorbent in ultrasound-assisted dispersive micro solid-phase extraction (USA DMSPE). The influence of the pH of the sample solution, amount of HNTs, and extraction time, as well as of the main parameters of HR CS GFAAS, on absorbance was investigated. The limit of detection was 0.005 μg L- 1. The preconcentration factor achieved for bismuth was 32. The relative standard deviation (RSD) was 4%. The accuracy of this method was validated by analyses of NIST SRM 1643e (Trace elements in water) and TMDA-54.5 (A high level fortified sample for trace elements) certified reference materials. The measured bismuth contents in these certified reference materials were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. The proposed method has been successfully applied to the determination of bismuth in five different real water samples (seawater, lake water, river water, stream water and rain water).

Dynamical traps in Wang-Landau sampling of continuous systems: Mechanism and solution

NASA Astrophysics Data System (ADS)

Koh, Yang Wei; Sim, Adelene Y. L.; Lee, Hwee Kuan

2015-08-01

We study the mechanism behind dynamical trappings experienced during Wang-Landau sampling of continuous systems reported by several authors. Trapping is caused by the random walker coming close to a local energy extremum, although the mechanism is different from that of the critical slowing-down encountered in conventional molecular dynamics or Monte Carlo simulations. When trapped, the random walker misses the entire or even several stages of Wang-Landau modification factor reduction, leading to inadequate sampling of the configuration space and a rough density of states, even though the modification factor has been reduced to very small values. Trapping is dependent on specific systems, the choice of energy bins, and the Monte Carlo step size, making it highly unpredictable. A general, simple, and effective solution is proposed where the configurations of multiple parallel Wang-Landau trajectories are interswapped to prevent trapping. We also explain why swapping frees the random walker from such traps. The efficacy of the proposed algorithm is demonstrated.

A FLUID SORBENT RECYCLING DEVICE FOR INDUSTRIAL FLUID USERS

EPA Science Inventory

A roller compression Extractor® that extracts fluids from reusable sorbent pads was evaluated as a method of waste reduction. The extraction device, evaluated for industrial fluid users in New Jersey, was found to be effective in recycling unpleated sorbent pads, especially ...

MERCURIC CHLORIDE CAPTURE BY ALKALINE SORBENTS

EPA Science Inventory

The paper gives results of bench-scale mechanistic studies of mercury/sorbent reactions that showed that mercuric chloride (HgC12) is readily adsorbed by alkaline sorbents, which may offers a less expensive alternative to the use of activated carbons. A laboratory-scale, fixed-b...

Kinetics of the sorption of triterpene saponin by hypercrosslinked polystyrene

NASA Astrophysics Data System (ADS)

Mironenko, N. V.; Brezhneva, T. A.; Selemenev, V. F.

2013-03-01

The kinetics of sorption of triterpene saponin by the polymer sorbent NM-200 is considered. The influence of the surface activity of glycoside on the rate of formation and structure of the adsorption layer on the sorbent's surface is established. The rate-determining step of sorption is found to be diffusion into the sorbent grain. The value of the activation energy demonstrates the determining role of dispersion forces in the interaction between triterpene saponin and the polymer sorbent MN-200.

High temperature regenerable hydrogen sulfide removal agents

DOEpatents

Copeland, Robert J.

1993-01-01

A system for high temperature desulfurization of coal-derived gases using regenerable sorbents. One sorbent is stannic oxide (tin oxide, SnO.sub.2), the other sorbent is a metal oxide or mixed metal oxide such as zinc ferrite (ZnFe.sub.2 O.sub.4). Certain otherwise undesirable by-products, including hydrogen sulfide (H.sub.2 S) and sulfur dioxide (SO.sub.2) are reused by the system, and elemental sulfur is produced in the regeneration reaction. A system for refabricating the sorbent pellets is also described.

Determination of heat purgeable and ambient purgeable volatile organic compounds in water by gas chromatography/mass spectrometry

USGS Publications Warehouse

Rose, Donna L.; Sandstrom, Mark W.; Murtagh, Lucinda K.

2016-09-08

Two new analytical methods have been developed by the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL) that allow the determination of 37 heat purgeable volatile organic compounds (VOCs) (USGS Method O-4437-16 [NWQL Laboratory Schedule (LS) 4437]) and 49 ambient purgeable VOCs (USGS Method O-4436-16 [NWQL LS 4436]) in unfiltered water. This report documents the procedures and initial performance of both methods. The compounds chosen for inclusion in the methods were determined as having high priority by the USGS National Water-Quality Assessment (NAWQA) Program. Both methods use a purge-and-trap technique with gas chromatography/mass spectrometry. The compounds are extracted from the sample by bubbling helium through a 25-milliliter sample. For the polar and less volatile compounds, the sample is heated at 60 degrees Celsius, whereas the less polar and more volatile compounds are purged using a separate analytical procedure at ambient temperature. The compounds are trapped on a sorbent trap, desorbed into a gas chromatograph/mass spectrometer for separation, and then identified and quantified. Sample preservation is recommended for both methods by adding a 1:1 solution of hydrochloric acid (HCl [1:1]) to water samples to adjust the pH to 2. Analysis within 14 days from sampling is recommended.The heat purgeable method (USGS Method O-4437-16) operates with the mass spectrometer in the simultaneous full scan/selected ion monitoring mode. This method supersedes USGS Method O-4024-03 (NWQL LS 4024). Method detection limits (MDLs) for fumigant compounds 1,2-dibromoethane, 1,2-dichloropropane, 1,2,3-trichloropropane, chloropicrin, and 1,2-dibromo-3-chloropropane range from 0.002 to 0.010 microgram per liter (µg/L). The MDLs for all remaining heat purgeable VOCs range from 0.006 µg/L for tert-butyl methyl ether to 3 µg/L for alpha-terpineol. Calculated holding times indicate that 36 of the 37 heat purgeable VOCs are stable for a minimum of 14 days preserved with HCl (1:1) to pH 2, and many are stable longer. Acrolein was retained in the method validation and initial method implementation and subsequently deleted because of instability and inconsistent performance. 2-Chloromethyl oxirane, methyl oxirane, and oxirane were tested using this method, but the compounds degraded quickly with the HCl (1:1) used for microbial preservation.The ambient purgeable method, USGS Method O-4436-16, operates with the mass spectrometer in the full scan mode. This method is a modification of USGS Method O-4127-96 (NWQL LS 2020). Several compounds were retained from Method O-4127-96 and will continue to be determined in Method O-4436-16. Eleven high priority compounds were added. MDLs for the high priority compounds range from 0.007 µg/L for 2,2-dichloro-1,1,1-trifluoroethane to 0.04 µg/L for 1,2,3,4-tetrahydronaphthalene and 1,3-butadiene. Historical MDLs for the compounds retained from Method O-4127-96 range from 0.009 µg/L for trans-1,2-dichloroethene to 0.1 µg/L for bromomethane. The calculated holding times for the compounds indicate the majority of the compounds are stable for a minimum of 14 days, or longer, at pH 2 with HCl (1:1) preservation. Four semivolatile compounds, 1,2-dimethylnaphthalene, 1,6-dimethylnaphthalene, 2,6-di-tert-butyl phenol, and 2-chloronapthalene, were tested and deleted from the method due to poor performance. Benzyl chloride was tested and deleted due to instability.

Radiation detector using a bulk high T.sub.c superconductor

DOEpatents

Artuso, Joseph F.; Franks, Larry A.; Hull, Kenneth L.; Symko, Orest G.

1993-01-01

A radiation detector (10) is provided, wherein a bulk high T.sub.c superconducting sample (11) is placed in a magnetic field and maintained at a superconducting temperature. Photons of incident radiation will cause localized heating in superconducting loops of the sample destroying trapped flux and redistributing the fluxons, and reducing the critical current of the loops. Subsequent cooling of the sample in the magnetic field will cause trapped flux redistributed Abrikosov fluxons and trapped Josephson fluxons. The destruction and trapping of the fluxons causes changes in the magnetization of the sample inducing currents in opposite directions in a pickup coil (12) which is coupled by an input coil (15) to an rf SQUID (16).

Radiation detector using a bulk high T[sub c] superconductor

DOEpatents

Artuso, J.F.; Franks, L.A.; Hull, K.L.; Symko, O.G.

1993-12-07

A radiation detector is provided, wherein a bulk high T[sub c] superconducting sample is placed in a magnetic field and maintained at a superconducting temperature. Photons of incident radiation will cause localized heating in superconducting loops of the sample destroying trapped flux and redistributing the fluxons, and reducing the critical current of the loops. Subsequent cooling of the sample in the magnetic field will cause trapped flux redistributed Abrikosov fluxons and trapped Josephson fluxons. The destruction and trapping of the fluxons causes changes in the magnetization of the sample inducing currents in opposite directions in a pickup coil which is coupled by an input coil to an rf SQUID. 4 figures.

Preparation of a hollow porous molecularly imprinted polymer using tetrabromobisphenol A as a dummy template and its application as SPE sorbent for determination of bisphenol A in tap water.

PubMed

Li, Jin; Zhang, Xuebin; Liu, Yuxin; Tong, Hongwu; Xu, Yeping; Liu, Shaomin

2013-12-15

In this paper, a highly selective sample cleanup procedure combing dummy molecular imprinting and solid-phase extraction (DMIP-SPE) was developed for the isolation and determination of bisphenol A (BPA) in tap water. The novel hollow porous dummy molecularly imprinted polymer (HPDMIP) was prepared adopting a sacrificial support approach, using tetrabromobisphenol A (TBBPA), whose structure was similar to that of BPA, as the dummy template and mesoporous MCM-48 nanospheres as the support. Owing to a very short distance between the binding sites and the surface, a large surface area and a good steric structure to match its imprint molecules, the maximum adsorption capacities (Qmax) of the dummy-imprinted and non-imprinted sorbents for BPA were as high as 445 and 340 μmol g(-1), respectively, and the adsorption reached about 73% of Qmax in 10 min. Meanwhile, a method was developed for the determination of BPA using HPDMIP as a solid-phase extraction enrichment sorbent coupled with HPLC. Under the optimum experimental conditions, HPDMIP exhibited satisfactory results in the enrichment and determination of BPA in tap water with a recovery rate of 95-105%, and relative standard deviations of below 6%, and it can achieve a limit of detection as low as 3 ng mL(-1). The developed extraction protocol eliminated the effect of template leakage on quantitative analysis and could be applied for the determination of BPA in complicated functional samples. © 2013 Elsevier B.V. All rights reserved.

Use of a novel cation-exchange restricted-access material for automated sample clean-up prior to the determination of basic drugs in plasma by liquid chromatography.

PubMed

Chiap, P; Rbeida, O; Christiaens, B; Hubert, Ph; Lubda, D; Boos, K S; Crommen, J

2002-10-25

A new kind of silica-based restricted-access material (RAM) has been tested in pre-columns for the on-line solid-phase extraction (SPE) of basic drugs from directly injected plasma samples before their quantitative analysis by reversed-phase liquid chromatography (LC), using the column switching technique. The outer surface of the porous RAM particlescontains hydrophilic diol groups while sulphonic acid groups are bound to the internal surface, which gives the sorbent the properties of a strong cation exchanger towards low molecular mass compounds. Macromolecules such as proteins have no access to the internal surface of the pre-column due to their exclusion from the pores and are then flushed directly out. The retention capability of this novel packing material has been tested for some hydrophilic basic drugs, such as atropine, fenoterol, ipratropium, procaine, sotalol and terbutaline, used as model compounds. The influence of the composition of the washing liquid on the retention of the analytes in the pre-column has been investigated. The elution profiles of the different compounds and the plasma matrix as well as the time needed for the transfer of the analytes from the pre-column to the analytical column were determined in order to deduce the most suitable conditions for the clean-up step and develop on-line methods for the LC determination of these compounds in plasma. The cationic exchange sorbent was also compared to another RAM, namely RP-18 ADS (alkyl diol silica) sorbent with respect to retention capability towards basic analytes.

High-Temperature Desulfurization of Heavy Fuel-Derived Reformate Gas Streams for SOFC Applications

NASA Technical Reports Server (NTRS)

Flytzani-Stephanopoulos, Maria; Surgenor, Angela D.

2007-01-01

Desulfurization of the hot reformate gas produced by catalytic partial oxidation or autothermal reforming of heavy fuels, such as JP-8 and jet fuels, is required prior to using the gas in a solid oxide fuel cell (SOFC). Development of suitable sorbent materials involves the identification of sorbents with favorable sulfidation equilibria, good kinetics, and high structural stability and regenerability at the SOFC operating temperatures (650 to 800 C). Over the last two decades, a major barrier to the development of regenerable desulfurization sorbents has been the gradual loss of sorbent performance in cyclic sulfidation and regeneration at such high temperatures. Mixed oxide compositions based on ceria were examined in this work as regenerable sorbents in simulated reformate gas mixtures and temperatures greater than 650 C. Regeneration was carried out with dilute oxygen streams. We have shown that under oxidative regeneration conditions, high regeneration space velocities (greater than 80,000 h(sup -1)) can be used to suppress sulfate formation and shorten the total time required for sorbent regeneration. A major finding of this work is that the surface of ceria and lanthanan sorbents can be sulfided and regenerated completely, independent of the underlying bulk sorbent. This is due to reversible adsorption of H2S on the surface of these sorbents even at temperatures as high as 800 C. La-rich cerium oxide formulations are excellent for application to regenerative H2S removal from reformate gas streams at 650 to 800 C. These results create new opportunities for compact sorber/regenerator reactor designs to meet the requirements of solid oxide fuel cell systems at any scale.

Adsorption and desorption of sulfur dioxide on novel adsorbents for flue gas desulfurization. Final report, September 1, 1993--August 31, 1994

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lin, Y.S.

Dry regenerative sorption processes have recently attracted increasing attention in flue gas desulfurization (FGD) because of their several advantages over the conventional wet-scrubbing processes. Dry sorbents are usually made by coating a transition or alkaline earth metal precursor on the surface of a porous support. Major disadvantages of these sorbents prepared by the conventional methods include relatively poor attrition resistance and low SO{sub 2} sorption capacity. The physical and especially chemical attrition (associated with the sulphation-oxidation-reduction cycles in the process) deteriorates the performance of the sorbents. The low SO{sub 2} sorption capacity is primarily due to the small surface areamore » of the support. Materials with a high surface area are not used as the supports for FGD sorbents because these materials usually are not thermally stable at high temperatures. In the past year, the research supported by Ohio Coal Development Office was focused on synthesis and properties of sol-gel derived alumina and zeolite sorbents with improved properties for FGD. The sol-gel derived alumina has large surface area, mesopore size and excellent mechanical strength. Some alumina-free zeolites not only posses the basic properties required as a sorbent for FGD (hydrophobicity, thermal and chemical stability, mechanical strength) but also have extremely large surface area and selective surface chemistry. The major objectives of this research program were to synthesize the sol-gel derived sorbents and to explore the use of the zeolites either directly as adsorbents or as sorbent support for FGD. The research was aimed at developing novel FGD sorbents possessing better sorption equilibrium and kinetic properties and improved physical and chemical attrition resistance.« less

Oil sorbents from plastic wastes and polymers: A review.

PubMed

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.

Hybrid biosorbents for removal of pollutants and remediation

NASA Astrophysics Data System (ADS)

Burlakovs, Juris; Klavins, Maris; Robalds, Artis; Ansone, Linda

2014-05-01

For remediation of soils and purification of polluted waters, wastewaters, biosorbents might be considered as prospective groups of materials. Amongst them peat have a special role due to low cost, biodegradability, high number of functional groups, well developed surface area and combination of hydrophilic/hydrophobic structural elements. Peat as sorbent have good application potential for removal of trace metals, and we have demonstrated peat sorption capacities, sorption kinetics, thermodynamics in respect to metals with different valencies - Tl(I), Cu(II), Cr(III). However, peat sorption capacity in respect to nonmetallic (anionic species) elements is low. Also peat mechanical properties do not support application in large scale column processes thereby, to expand peat application sphere, the approach of biomass based hybrid sorbents has been elaborated. The concept "hybrid sorbent" in understanding of biosorbent means natural, biomass based modified material, covered with another sorbent material, thus combining properties of both such as sorbent functionalities, surface properties etc. As the "covering layer" both inorganic substances, mineral phases (iron oxohydroxides, oxyappatite) and organic polymers (using graft polymerization) were used. The obtained sorbents were characterised by their spectral properties, surface area and elemental composition. The obtained hybrid sorbents were tested for sorption of compounds in anionic speciation forms, for example of arsenic, antimony, tellurium and phosphorous compounds in comparison with weakly basic anionites. The highest sorption capacity was observed when peat sorbents modified with iron compounds were used. Sorption of different arsenic speciation forms onto iron-modified peat sorbents was investigated as a function of pH and temperature. It was established that sorption capacity increases with a rise in temperature as the calculation of sorption process thermodynamic parameters indicates the spontaneity of sorption process and its endothermic nature. The recycling options of obtained compounds after their saturation with metal or non-metallic species are suggested.

Method for increasing the dynamic range of mass spectrometers

DOEpatents

Belov, Mikhail; Smith, Richard D.; Udseth, Harold R.

2004-09-07

A method for enhancing the dynamic range of a mass spectrometer by first passing a sample of ions through the mass spectrometer having a quadrupole ion filter, whereupon the intensities of the mass spectrum of the sample are measured. From the mass spectrum, ions within this sample are then identified for subsequent ejection. As further sampling introduces more ions into the mass spectrometer, the appropriate rf voltages are applied to a quadrupole ion filter, thereby selectively ejecting the undesired ions previously identified. In this manner, the desired ions may be collected for longer periods of time in an ion trap, thus allowing better collection and subsequent analysis of the desired ions. The ion trap used for accumulation may be the same ion trap used for mass analysis, in which case the mass analysis is performed directly, or it may be an intermediate trap. In the case where collection is an intermediate trap, the desired ions are accumulated in the intermediate trap, and then transferred to a separate mass analyzer. The present invention finds particular utility where the mass analysis is performed in an ion trap mass spectrometer or a Fourier transform ion cyclotron resonance mass spectrometer.

Bench-scale Development of an Advanced Solid Sorbent-based CO 2 Capture Process for Coal-fired Power Plants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nelson, Thomas; Kataria, Atish; Soukri, Mustapha

It is increasingly clear that CO 2 capture and sequestration (CCS) must play a critical role in curbing worldwide CO 2 emissions to the atmosphere. Development of these technologies to cost-effectively remove CO 2 from coal-fired power plants is very important to mitigating the impact these power plants have within the world’s power generation portfolio. Currently, conventional CO 2 capture technologies, such as aqueous-monoethanolamine based solvent systems, are prohibitively expensive and if implemented could result in a 75 to 100% increase in the cost of electricity for consumers worldwide. Solid sorbent CO 2 capture processes – such as RTI’s Advancedmore » Solid Sorbent CO 2, Capture Process – are promising alternatives to conventional, liquid solvents. Supported amine sorbents – of the nature RTI has developed – are particularly attractive due to their high CO 2 loadings, low heat capacities, reduced corrosivity/volatility and the potential to reduce the regeneration energy needed to carry out CO 2 capture. Previous work in this area has failed to adequately address various technology challenges such as sorbent stability and regenerability, sorbent scale-up, improved physical strength and attrition-resistance, proper heat management and temperature control, proper solids handling and circulation control, as well as the proper coupling of process engineering advancements that are tailored for a promising sorbent technology. The remaining challenges for these sorbent processes have provided the framework for the project team’s research and development and target for advancing the technology beyond lab- and bench-scale testing. Under a cooperative agreement with the US Department of Energy, and part of NETL’s CO 2 Capture Program, RTI has led an effort to address and mitigate the challenges associated with solid sorbent CO 2 capture. The overall objective of this project was to mitigate the technical and economic risks associated with the scale-up of solid sorbent-based CO 2 capture processes, enabling subsequent larger pilot demonstrations and ultimately commercial deployment. An integrated development approach has been a key focus of this project in which process development, sorbent development, and economic analyses have informed each of the other development processes. Development efforts have focused on improving the performance stability of sorbent candidates, refining process engineering and design, and evaluating the viability of the technology through detailed economic analyses. Sorbent advancements have led to a next generation, commercially-viable CO 2 capture sorbent exhibiting performance stability in various gas environments and a physically strong fluidizable form. The team has reduced sorbent production costs and optimized the production process and scale-up of PEI-impregnated, fluidizable sorbents. Refinement of the process engineering and design, as well as the construction and operation of a bench-scale research unit has demonstrated promising CO 2 capture performance under simulated coal-fired flue gas conditions. Parametric testing has shown how CO 2 capture performance is impacted by changing process variables, such as Adsorber temperature, Regenerator temperature, superficial flue gas velocity, solids circulation rate, CO 2 partial pressure in the Regenerator, and many others. Long-term testing has generated data for the project team to set the process conditions needed to operate a solids-based system for optimal performance, with continuous 90% CO 2 capture, and no operational interruptions. Data collected from all phases of testing has been used to develop a detailed techno-economic assessment of RTI’s technology. These detailed analyses show that RTI’s technology has significant economic advantages over current amine scrubbing and potential to achieve the DOE’s Carbon Capture Program’s goal of >90% CO 2 capture rate at a cost of < $40/T-CO 2 captured by 2025. Through this integrated technology development approach, the project team has advanced RTI’s CO 2 capture technology to TRL-4 (nearly TRL-5, with the missing variable being testing on actual, coal-fired flue gas), according to the DOE/FE definitions for Technology Readiness Levels. At a broader level, this project has advanced the whole of the solid sorbent CO 2 capture field, with advancements in process engineering and design, technical risk mitigation, sorbent scale-up optimization, and an understanding of the commercial viability and applicability of solid sorbent CO 2 capture technologies for the U.S. existing fleet of coal-fired power plants.« less

Regenerable sorbent technique for capturing CO.sub.2 using immobilized amine sorbents

DOEpatents

Pennline, Henry W; Hoffman, James S; Gray, McMahan L; Fauth, Daniel J; Resnik, Kevin P

2013-08-06

The disclosure provides a CO.sub.2 absorption method using an amine-based solid sorbent for the removal of carbon dioxide from a gas stream. The method disclosed mitigates the impact of water loading on regeneration by utilizing a conditioner following the steam regeneration process, providing for a water loading on the amine-based solid sorbent following CO.sub.2 absorption substantially equivalent to the moisture loading of the regeneration process. This assists in optimizing the CO.sub.2 removal capacity of the amine-based solid sorbent for a given absorption and regeneration reactor size. Management of the water loading in this manner allows regeneration reactor operation with significant mitigation of energy losses incurred by the necessary desorption of adsorbed water.

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

NASA Astrophysics Data System (ADS)

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.

Rotary moving bed for CO.sub.2 separation and use of same

DOEpatents

Elliott, Jeannine Elizabeth; Copeland, Robert James; McCall, Patrick P.

2017-01-10

A rotary moving bed and process for separating a carbon dioxide from a gas stream is disclosed. The rotary moving bed can have a rotational assembly rotating on a vertical axis, and a plurality of sorbent cells positioned horizontally to the axis of rotation that fills a vertical space in the moving bed, where the sorbent cells adsorb the carbon dioxide by concentration swing adsorption and adsorptive displacement. The sorbent can be regenerated and the carbon dioxide recaptured by desorbing the carbon dioxide from the sorbent using concentration swing adsorption and desorptive displacement with steam. The gas flows in the system flow in a direction horizontal to the axis of rotation and in a direction opposite the rotational movement of the sorbent cells.

Validated Test Method 5030C: Purge-and-Trap for Aqueous Samples

EPA Pesticide Factsheets

This method describes a purge-and-trap procedure for the analysis of volatile organic compoundsin aqueous samples & water miscible liquid samples. It also describes the analysis of high concentration soil and waste sample extracts prepared in Method 5035.

Dual-stage trapped-flux magnet cryostat for measurements at high magnetic fields

DOEpatents

Islam, Zahirul; Das, Ritesh K.; Weinstein, Roy

2015-04-14

A method and a dual-stage trapped-flux magnet cryostat apparatus are provided for implementing enhanced measurements at high magnetic fields. The dual-stage trapped-flux magnet cryostat system includes a trapped-flux magnet (TFM). A sample, for example, a single crystal, is adjustably positioned proximate to the surface of the TFM, using a translation stage such that the distance between the sample and the surface is selectively adjusted. A cryostat is provided with a first separate thermal stage provided for cooling the TFM and with a second separate thermal stage provided for cooling sample.