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1.
Proc Natl Acad Sci U S A ; 120(37): e2305572120, 2023 Sep 12.
Artículo en Inglés | MEDLINE | ID: mdl-37669368

RESUMEN

One essential element of redox flow batteries (RFBs) is the flow field. Certain dead zones that cause local overpotentials and side effects are present in all conventional designs. To lessen the detrimental effects, a dead-zone-compensated design of flow field optimization is proposed. The proposed architecture allows for the detection of dead zones and their compensation on existing flow fields. Higher reactant concentrations and uniformity factors can be revealed in the 3D multiphysical simulation. The experiments also demonstrate that at an energy efficiency (EE) of 80%, the maximum current density of the novel flow field is 205 mA cm-2, which is much higher than the values for the previous ones (165 mA cm-2) and typical serpentine flow field (153 mA cm-2). Extensions of the design have successfully increased system EE (2.7 to 4.3%) for a variety of flow patterns. As a result, the proposed design is demonstrated to be a general method to support the functionality and application of RFBs.

2.
ACS Sens ; 8(7): 2702-2712, 2023 07 28.
Artículo en Inglés | MEDLINE | ID: mdl-37357408

RESUMEN

Total alkalinity (TA) is an essential variable for the study of physical and biogeochemical processes in coastal and oceanic systems, and TA data obtained at high spatiotemporal resolutions are highly desired. The performance of the current in situ TA analyzers/sensors, including precision, accuracy, and deployment duration, cannot fully meet most research requirements. Here, we report on a novel high-precision in situ analyzer for surface seawater TA (ISA-TA), based on an automated single-point titration with spectrophotometric pH detection, and capable of long-term field observations. The titration was carried out in a circulating loop, where the titrant (a mixture of HCl and bromocresol green) and seawater sample were mixed in a constant volume ratio. The effect of ambient temperature on the TA measurement was corrected with an empirical formula. The weight, height, diameter, and power consumption of ISA-TA were 8.6 kg (in air), 33 cm, 20 cm, and 7.3 W, respectively. A single measurement required ∼7 min of running time, ∼32 mL of seawater, and ∼0.6 mL of titrant. ISA-TA was able to operate continuously in the field for up to 30 days, and its accuracies in the laboratory and field were 0.5 ± 1.7 µmol kg-1 (n = 13) and 10.3 ± 2.8 µmol kg-1 (n = 29) with precisions of 0.6-0.8 µmol kg-1 (n = 51) and 0.2-0.7 µmol kg-1 (n = 8), respectively. This study provides the research community with a new tool to obtain seawater TA data of high temporal resolution.


Asunto(s)
Agua de Mar , Océanos y Mares , Espectrofotometría
3.
Sci Total Environ ; 800: 149517, 2021 Dec 15.
Artículo en Inglés | MEDLINE | ID: mdl-34391153

RESUMEN

High-resolution time-series concentrations (CTS) are very important for the investigation of the biogeochemical processes of trace metals in the aquatic environment. However, the acquisition of CTS of trace metals in water is still challenging because of the lack of suitable samplers. In this study, an osmotic sampler coupled with air segment injection and preservative addition was employed for time-series sampling of trace metals in surface waters. In the sampler, water sampling and preservative adding are both driven by osmotic pumps (OPs), while air segment injection is accomplished by a timer-controlled micro diaphragm pump. During deployment, the sampling OP continuously draws water through a filter and stores it in a narrow-bore coil. Simultaneously, a preservative OP slowly pushes 30% HNO3 (v/v) into the collected sample for in situ preservation. Periodically, the micro diaphragm pump injects air into the continuous water stream to divide it into water segments, enabling accurate time-stamping. After retrieval, the time-series samples were pumped out from the coil and re-collected to analyze the CTS of analytes. The sampler was deployed in river, reservoir, and marine waters for 26 h and one week to measure CTS of trace metals at time resolutions of 2 h and 12 h. Results showed that the recoveries of a preloaded standard mixture (1.0 µg/L) in all samplers ranged from 93.1% to 117.8%. The measured CTS of Cd, Co, Cr, Cu, Mn, and Ni in the waters only varied in small ranges. Accordingly, the measured CTS data from the sampler were consistent with the obtained concentrations from grab sampling. The relative percent differences between the measurements from two samplers were less than 37.4%. These results demonstrate the reliability and accuracy of the sampler for time-series sampling of the chosen trace metals in surface waters.


Asunto(s)
Oligoelementos , Contaminantes Químicos del Agua , Monitoreo del Ambiente , Reproducibilidad de los Resultados , Ríos , Contaminantes Químicos del Agua/análisis
4.
Talanta ; 224: 121775, 2021 Mar 01.
Artículo en Inglés | MEDLINE | ID: mdl-33379010

RESUMEN

Automated instrument for long-term measurement of seawater pH is important for documenting the changes of the marine carbonate system and the impacts of ocean acidification. An automated pH analyzer based on loop flow analysis (LFA-pH) was developed to achieve precise and accurate measurements of seawater pH. The circulating loop allows complete mixing of an indicator and seawater, constant mixing volume of two solutions, and correcting indicator perturbation for each measurement. During laboratory testing, the LFA-pH precision achieved 0.0004, and the accuracy was 0.0017 ± 0.0038 compared with the certified standard buffer at different temperatures. During the 59 day underway measurement across the mid and high latitudes, more than 2500 pH measurements were carried out. LFA-pH showed good stability with high temperature and salinity changes, and measurement results were consistent with the discrete surface seawater pH measurement data. In situ testing of two LFA-pHs was completed near the Zhongyuan pier in Qingdao. The average pH offset between the two LFA-pHs was 0.0010 ± 0.0032 (n = 788), with the accuracies of the two LFA-pHs of 0.0012 ± 0.0033 and 0.0005 ± 0.0035 compared to discrete measurements. For continuous measurement, the average power consumption is 3.6 W at a 10 min measurement frequency. Given its low power consumption, high precision, and accuracy, FLA-pH could be adapted for underway and in situ measurements of ocean acidification observations.

5.
Sci Total Environ ; 759: 143538, 2021 Mar 10.
Artículo en Inglés | MEDLINE | ID: mdl-33229095

RESUMEN

The analysis of time-series concentrations (CTS) is of great importance when investigating the biogeochemical processes of nutrients in aquatic environments. However, obtaining CTS of nutrients remains a challenge using current sampling techniques. In this study, a novel in situ sampler was constructed using reverse osmosis membrane (ROM) osmotic pumps (OP) (ROM-OP sampler), and was used to obtain the CTS of nutrients in surface waters. The sampler consisted of a sampling OP, sample storing coil, filter, bubble injection module, and preservative adding module. When deployed, the sampling OP continuously draws ambient water through the filter into the sample storing coil, while simultaneously the preservative adding module continuously delivers preservative (H2SO4 solution) into the water flow. The bubble injection module periodically injects air bubbles into the sample storing coil, to segment the sample and create time stamp indicators that allow the sample age to be defined. Upon retrieval, the sample segments in the coil are sequentially pumped out of the sample storing coil and transferred into different vials for further analysis. The sampler was applied to measure the CTS of various nutrients, including dissolved total nitrogen, dissolved total phosphorus, dissolved reactive phosphorus, and nitrate in a river over a 20 day period and in municipal sewage treatment plant effluent for a 36 h period. Results showed that the ROM-OP sampler successfully obtained CTS of nutrients, capturing nutrient variations at a high temporal resolution. This sampler is relatively low-cost (~USD 300), small in size, lightweight, robust and does not require an external power source, showing high promise as an effective and efficient tool for monitoring nutrient CTS in aquatic environments.

6.
Environ Sci Technol ; 53(5): 2579-2585, 2019 03 05.
Artículo en Inglés | MEDLINE | ID: mdl-30712344

RESUMEN

Active samplers for ambient monitoring of trace contaminants in surface water are highly desirable, but their use is often constrained by power supply. Here, we proposed a novel solution by coupling an improved osmotic pump (OP) with a solid-phase extraction (SPE) cartridge to construct a power-free active sampler for organic contaminants. The OP simply consisted of two cylindrical chambers separated by a reverse osmosis membrane. We, for the first time, added ion-exchange resins into the OP inlet chamber and successfully constructed OPs with a smooth and constant flow. In the OP-SPE sampler, water was continuously drawn through the SPE cartridge at a constant flow, and time-weighted average concentration over the sampling course may be easily calculated from the amount of target analytes retained on the SPE cartridge and water collected in the sampler. The OP-SPE samplers were deployed in a river to detect herbicides, and the measured concentrations were largely in agreement with the average of 11 daily spot samples. Given that a wide range of SPE cartridges are available for different classes of organic contaminants, this approach is versatile and may find widespread applications for in situ sampling of surface water under different conditions, including poorly accessible locations.


Asunto(s)
Contaminantes Ambientales , Contaminantes Químicos del Agua , Monitoreo del Ambiente , Ósmosis , Extracción en Fase Sólida , Agua
7.
Talanta ; 185: 419-426, 2018 Aug 01.
Artículo en Inglés | MEDLINE | ID: mdl-29759221

RESUMEN

A flow injection method combined with an on-line UV and thermal digestion for simultaneous determination of total dissolved nitrogen (TDN) and total dissolved phosphorus (TDP) in natural waters was established in this study. A novel flow manifold made the proposed system compact and automatic. The conversion rates of various nitrogen and phosphorus compounds to their nitrate and phosphate forms with different digestion models and different concentrations were well investigated using the flow injection technique. The reagent concentrations for colorimetric analysis were optimized based on a univariate experimental design. The detection limits were 0.8 µmol L-1 and 0.2 µmol L-1, and linear analytical ranges were up to 300 µmol L-1 and 25 µmol L-1 for TDN and TDP, respectively. The sample throughput was ~ 5 h-1. The recovery of spiked natural water samples varied from 86.8% to 102.6% for TDN and 88.0% to 102.0% for TDP. The present approach was successfully applied for the determination of TDN and TDP in natural water samples and was found to have good agreement with reference methods. The outcomes of present study indicated that the proposed method is suitable for routine analysis as well as for potential on-line monitoring.

8.
Environ Sci Technol ; 48(22): 13069-75, 2014 Nov 18.
Artículo en Inglés | MEDLINE | ID: mdl-25375182

RESUMEN

We identified a barely noticed contributor, submarine groundwater discharge (SGD), to acidification of a coastal fringing reef system in Sanya Bay in the South China Sea based on time-series observations of Ra isotopes and carbonate system parameters. This coastal system was characterized by strong diel changes throughout the spring to neap tidal cycle of dissolved inorganic carbon (DIC), total alkalinity, partial pressure of CO2 (pCO2) and pH, in the ranges of 1851-2131 µmol kg(-1), 2182-2271 µmol kg(-1), 290-888 µatm and 7.72-8.15, respectively. Interestingly, the diurnal amplitudes of these parameters decreased from spring to neap tides, governed by both tidal pumping and biological activities. In ebb stages during the spring tide, we observed the lowest salinities along with the highest DIC, pCO2 and Ra isotopes, and the lowest pH and aragonite saturation state. These observations were consistent with a concurrent SGD rate up to 25 and 44 cm d(-1), quantified using Darcy's law and (226)Ra, during the spring tide ebb, but negligible at flood tides. Such tidal-driven SGD of low pH waters is another significant contributor to coastal acidification, posing additional stress on coastal coral systems, which would be even more susceptible in future scenarios under higher atmospheric CO2.


Asunto(s)
Ácidos/química , Arrecifes de Coral , Ecosistema , Agua Subterránea/química , Navíos , Movimientos del Agua , Álcalis/análisis , Bahías , Carbono/análisis , Carbonatos/análisis , China , Geografía , Salinidad , Factores de Tiempo
9.
Talanta ; 123: 218-23, 2014 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-24725885

RESUMEN

The current flow based method for the determination of dissolved reactive phosphorus (DRP) suffers interference from salinity (e.g. index refractive difference) and the incidentally formed bubbles, which can be a problem for optical detection. Here we reported a simple and robust loop flow analysis (LFA) method for accurate measurement of DRP in different aqueous samples. The chemistry is based on the classic phosphomolybdenum blue (PMB) reaction and the PMB formed in a novel cross-shaped flow cell was detected at 700 nm using a miniature spectrophotometer. The effects of reagents on the kinetic formation of PMB were evaluated. The detection limit was 32 nM with an optical pathlength of 1cm and the relative standard deviations for repetitive determinations of 1, 2 and 8 µM phosphate solutions were 1.8% (n=113, without any stoppage during repeating analysis for >7h), 1.0% (n=49) and 0.39% (n=9), respectively. The analysis time was 4 min sample(-1). The effects of salinity and interfering ions (silicate and arsenate) were evaluated and showed no interference under the proposed protocol for DRP analysis. Using the LFA method, different aqueous samples with a salinity range of 0-34 were analyzed and the results showed excellent agreement with the reference method (slope 0.9982±0.0063, R(2)=0.9987, n=34). Recoveries for spiked samples varied from 95.4% to 103.7%. The proposed method showed insignificant interference from salinity, silicate and arsenate, higher reproducibility, easier operation and was free of the bubble problem.


Asunto(s)
Análisis de Inyección de Flujo/métodos , Fosfatos/análisis , Fósforo/análisis , Agua/química , Arseniatos/química , Concentración de Iones de Hidrógeno , Aguas Minerales/análisis , Molibdeno/análisis , Molibdeno/química , Fosfatos/química , Ácidos Fosfóricos/análisis , Ácidos Fosfóricos/química , Fósforo/química , Reproducibilidad de los Resultados , Ríos/química , Agua de Mar/química , Silicatos/química , Cloruro de Sodio/química , Solubilidad , Soluciones , Espectrofotometría , Aguas Residuales/química
10.
ACS Macro Lett ; 3(9): 916-921, 2014 Sep 16.
Artículo en Inglés | MEDLINE | ID: mdl-35596359

RESUMEN

A new and efficient strategy to synthesize multicompartment block copolymer nanoparticles (MCBNs) by two macro-RAFT agents comediated dispersion polymerization is proposed. By simultaneously employing two macro-RAFT agents in dispersion RAFT polymerization, one-pot synthesis of well-defined MCBNs constructed with two diblock copolymers of poly(tert-butyl methyl acrylate)-block-polystyrene (PtBMA-b-PS) and poly[N-(4-vinylbenzyl)-N,N-diethylamine]-block-polystyrene (PVEA-b-PS) is achieved. These MCBNs contain a PS core and discrete PVEA and/or PtBMA nodules on the PS core. By changing the ratio of the two macro-RAFT agents or the polymerization degree of the solvophobic block in the two diblock copolymer mixture, the structure of MCBNs can be tuned. Our strategy overcomes the inconvenience and difficulty in synthesis of MCBNs, and it introduces a valid way to prepare well-defined MCBNs constructed with two or more diblock copolymers.

11.
Environ Sci Technol ; 47(19): 11139-46, 2013 Oct 01.
Artículo en Inglés | MEDLINE | ID: mdl-23968512

RESUMEN

An automated analyzer was developed to achieve fast, precise, and accurate measurements of seawater total alkalinity (AT) based on single-point titration and spectrophotometric pH detection. The single-point titration was carried out in a circulating loop, which allowed the titrant (hydrochloric acid and bromocresol green solution) and a seawater sample to mix at a constant volume ratio. The dissolved CO2 in the sample-titrant mixture was efficiently removed by an inline CO2 remover, which consists of a gas-permeable tubing (Teflon AF2400) submerged in a sodium hydroxide (NaOH) solution. The pH of the mixture was then measured with a custom-made spectrophotometric detection system. The analyzer was calibrated against multiple certified reference materials (CRMs) with different AT values. The analyzer features a sample throughput time of 6.5 min with high precision (±0.33-0.36 µmol kg(-1); n = 48) and accuracy (-0.33 ± 0.99 µmol kg(-1); n = 10). Intercomparison to a traditional open-cell AT titrator showed overall good agreement of 0.88 ± 2.03 µmol kg(-1) (n = 22). The analyzer achieved excellent stability without recalibration over 11 days, during which time 320 measurements were made with a total running time of over 40 h. Because of its small size, low power consumption requirements, and its ability to be automated, the new analyzer can be adapted for underway and in situ measurements.


Asunto(s)
Agua de Mar/química , Dióxido de Carbono/química , Concentración de Iones de Hidrógeno , Espectrofotometría/instrumentación , Volumetría/instrumentación
12.
Talanta ; 85(4): 2212-7, 2011 Sep 30.
Artículo en Inglés | MEDLINE | ID: mdl-21872080

RESUMEN

The commercial solid phase microextraction (SPME) fibers are not stable enough in organic solvent and tend to swell and strip off from the silica fiber in the high performance liquid chromatography (HPLC) mobile phase, and therefore the application of SPME coupled online with HPLC is limited. In this study, an SPME fiber coated with single walled carbon nanotubes (SWCNTs), prepared by means of electrophoretic deposition, was coupled on line to HPLC for the determination of four endocrine-disrupting compounds, i.e. bisphenol A (BPA), estrone (E(1)), 17α-ethynylestradiol (EE(2)) and octylphenol (OP), in aqueous samples. The results showed that the SWCNTs coating on the prepared fiber did not swell and strip off from the platinum fiber throughout the experiment, thus indicating a high resistance to the HPLC mobile phase, the mixture of water and acetonitrile. The SWCNTs fiber had similar (for OP) or higher (for BPA, EE(2) and E(1)) extraction efficiencies than the commonly used polyacrylate fiber, and had a lifetime of more than 120 operation times. Under the optimized conditions, the linearity of the proposed method was 1.0-30.0 µg/L for BPA and OP and 3.0-90.0 µg/L for E(1) and EE(2). The limits of detection (LODs; S/N=3) and limits of quantification (LOQs; S/N=10) of the method were 0.32-0.52 µg/L and 1.06-1.72 µg/L, respectively. Repeatability for one fiber (n=3) was in the range of 1.3-7.1% and fiber-to-fiber reproducibility (n=3) was in the range of 1.6-8.4%. The proposed method was successfully applied for the analysis of spiked tap water and seawater samples with recoveries from 81.8 to 97.3%.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Disruptores Endocrinos/análisis , Disruptores Endocrinos/aislamiento & purificación , Nanotubos de Carbono/química , Microextracción en Fase Sólida/métodos , Integración de Sistemas , Agua/química , Resinas Acrílicas/química , Electroforesis , Disruptores Endocrinos/química , Hidrógeno/química , Sistemas en Línea
13.
Talanta ; 85(2): 1148-53, 2011 Aug 15.
Artículo en Inglés | MEDLINE | ID: mdl-21726751

RESUMEN

A platinum plate coated with single-walled carbon nanotubes (SWCNTs@Pt) was prepared by means of electrophoretic deposition. Using the SWCNTs@Pt plate, an electrosorption-enhanced solid-phase microextraction (EE-SPME) technique was proposed for the extraction of trace anions in water, described as follows: a positive potential was applied to the SWCNTs@Pt plate to extract F(-), Cl(-), Br(-), NO(3)(-) and SO(4)(2-) from water using electrosorption, and then a negative potential was applied to the plate placed in ultra-pure water for the desorption of the absorbed anions, and finally the desorbed anions were analyzed using ion chromatography (IC). The EE-SPME parameters, including extraction potential and time as well as desorption potential and time, were investigated. An analytical method based on the above procedures, i.e., EE-SPME-IC, was established and used for the analysis of trace anions in water. The results showed that the application of potential on the SWCNTs@Pt plate significantly enhanced the ion extraction efficiency, and an enrichment factor of 15-38 was achieved. The SWCNTs@Pt plate could be used more than 50 times without significant decay. The linear range, the limit of detection (S/N=3), the limit of quantification (S/N=10) and repeatability (n=7) of our EE-SPME-IC method were 1.0-150.0 µg/L, 0.06-0.26 µg/L, 0.19-0.85 µg/L and 2.1-8.0%, respectively. The proposed method was successfully applied for the analysis of trace anions in deionized water, and acceptable recoveries between 65.3 and 121.1% were obtained for the spiked deionized water samples.


Asunto(s)
Aniones/aislamiento & purificación , Nanotubos de Carbono/química , Platino (Metal)/química , Microextracción en Fase Sólida/métodos , Aniones/análisis , Electroforesis , Factores de Tiempo , Agua/química
14.
J Hazard Mater ; 186(1): 473-80, 2011 Feb 15.
Artículo en Inglés | MEDLINE | ID: mdl-21122989

RESUMEN

An electrochemical technique was adopted to investigate the removal of Cr(VI) species and total chromium (TCr) from aqueous solution at a laboratory scale. The electrodes of stainless steel nets (SSNE) coated with single wall carbon nanotubes (SWCNTs@SSNE) were used as both anode and cathode. Three parameters, including solution pH, voltage and electrolyte concentration, were studied to explore the optimal condition of chromium removal. The optimal parameters were found to be pH 4, voltage 2.5 V and electrolyte concentration 10 mg/L. Under these conditions, the Cr(VI) and TCr removal had a high correlation with the amount of SWCNTs coated on the electrodes, with coefficients of the regression equations 0.953 and 0.928, respectively. The mechanism of Cr(VI) removal was also investigated. X-ray photoelectron spectroscopy (XPS) study and scanning electron microscope (SEM) picture showed that the process of chromium removal involved the reduction of Cr(VI) to Cr(III) on the cathode, and then the adsorption of Cr(III) by SWCNTs on the cathode. The study results indicated that the proposed method provided an interesting means to remove chromium species from aqueous solution, especially Cr(VI) in acidic condition.


Asunto(s)
Cromo/aislamiento & purificación , Electroquímica/métodos , Nanotubos de Carbono , Acero Inoxidable , Contaminantes Químicos del Agua/aislamiento & purificación , Electrólitos , Concentración de Iones de Hidrógeno , Microscopía Electrónica de Rastreo , Soluciones , Análisis Espectral/métodos , Rayos X
15.
J Chromatogr A ; 1217(15): 2191-6, 2010 Apr 09.
Artículo en Inglés | MEDLINE | ID: mdl-20207361

RESUMEN

A solid-phase microextraction (SPME) fiber coated with single walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition and treated at 500 degrees C in H(2) stream. In order to evaluate the characteristics of the obtained fiber, it was applied in the headspace solid-phase microextraction (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) from water sample and quantification by gas chromatography with flame ionization detection (GC-FID). The results indicated that the thermal treatment with H(2) enhanced the extraction of the SWCNTs fiber for BTEX significantly. Thermal stability and durability of the fiber were also investigated, showing excellent stability up to 350 degrees C and life time over 120 times. In the comparison with the commercial CAR-PDMS fiber, the SWCNTs fiber showed similar and higher extraction efficiencies for BTEX. Under the optimized conditions, the linearity, LODs (S/N=3) and LOQs (S/N=10) of the method based on the SWCNTs fiber were 0.5-50.0, 0.005-0.026 and 0.017-0.088 microg/L, respectively. Repeatability for one fiber (n=3) was in the range of 1.5-5.6% and fiber-to-fiber reproducibility (n=3) was in the range of 4.2-8.3%. The proposed method was successfully applied in the analysis of BTEX compounds in seawater, tap water and wastewater from a paint plant.


Asunto(s)
Derivados del Benceno/análisis , Benceno/análisis , Nanotubos de Carbono/química , Microextracción en Fase Sólida/instrumentación , Tolueno/análisis , Agua/química , Xilenos/análisis , Dimetilpolisiloxanos/química , Hidrógeno/química , Límite de Detección , Cloruro de Sodio/química , Espectrofotometría Infrarroja , Temperatura , Factores de Tiempo
16.
J Environ Monit ; 11(2): 439-44, 2009 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-19212604

RESUMEN

The development of new sorbents, which are able to trap polar compounds, is a growing research field in solid-phase extraction (SPE). In this study, multi-walled carbon nanotubes (MWCNTs) and single-walled carbon nanotubes (SWCNTs) were oxidized in air at 600 degrees C and 500 degrees C, respectively, for 2 h. MWCNTs, SWCNTs, air oxidized MWCNTs (OMWCNTs) and SWCNTs (OSWCNTs) (200 mg of each) were packed in SPE cartridges. The four cartridges obtained, together with a commercial Oasis HLB cartridge, were used to extract six polar organophosphorous pesticides (OPPs), i.e., dichlorvos, methamidophos, acephate, omethoate, monocrotophos and dimethoate, from an aqueous sample. The results showed that the oxidation process significantly enhanced the adsorption abilities of both SWCNTs and MWCNTs for polar OPPs. A comparative study indicated that OSWCNTs were more effective than Oasis HLB for the extraction of methamidophos and acephate and as effective as Oasis HLB for the other four OPPs from aqueous samples. When 100 mL of a natural sample was spiked with OPPs and extracted with OSWCNTs, the recoveries of five of the six polar OPPs (methamidophos excepted) ranged from 79.1 to 101.9%. The detection limits of the method based on OSWCNTs was found to be 0.07-0.12 microg L(-1).


Asunto(s)
Nanotubos de Carbono/química , Compuestos Organotiofosforados/aislamiento & purificación , Plaguicidas/aislamiento & purificación , Extracción en Fase Sólida/instrumentación , Extracción en Fase Sólida/métodos , Adsorción , Oxidación-Reducción , Agua de Mar/análisis , Sensibilidad y Especificidad , Agua/análisis , Contaminantes Químicos del Agua/aislamiento & purificación
17.
J Chromatogr A ; 1216(9): 1305-11, 2009 Feb 27.
Artículo en Inglés | MEDLINE | ID: mdl-19162268

RESUMEN

A novel solid-phase microextraction (SPME) Pt fiber coated with single-walled carbon nanotubes (SWCNTs) was prepared by electrophoretic deposition (EPD) and applied to the determination of phenols in aqueous samples by direct immersion (DI)-SPME-HPLC-UV. The results revealed that EPD was a simple and reproducible technique for the preparation of SPME fibers coated with SWCNTs without the use of adhesive. The obtained SWCNT coating did not swell in organic solvents nor strip off from substrate, and possessed high mechanical strength due to the strong Van der Waals attractions between the surfaces of the SWCNTs. The prepared SPME fiber was conductive since both SWCNT coating and Pt wire were conductive. Using Pt wire as substrate, the fiber was unbreakable. Owing to the presence of oxygenated groups on SWCNTs and the high surface area of SWCNTs, the SWCNT fiber was similar to or superior to commercial PA fiber in extracting the studied phenols from aqueous sample. A durability of more than 80 analyses was achieved for one unique fiber. Under optimized conditions, the detection limits for the phenols varied between 0.9 and 3.8 ng/mL, the precisions were in the range of 0.7-3.2% (n=3), and linear ranges were within 10 and 300 ng/mL. The method was successfully applied to the analysis of spiked seawater and tap water samples with the recoveries from 87.5 to 102.0%.


Asunto(s)
Nanotubos de Carbono/química , Fenoles/aislamiento & purificación , Microextracción en Fase Sólida/métodos , Agua/química , Cromatografía Líquida de Alta Presión , Interpretación Estadística de Datos , Electroforesis/métodos , Equipo Reutilizado , Concentración de Iones de Hidrógeno , Nanotubos de Carbono/ultraestructura , Concentración Osmolar , Fenoles/química , Platino (Metal)/química , Reproducibilidad de los Resultados , Agua de Mar/química , Sensibilidad y Especificidad , Solventes/química , Espectroscopía Infrarroja por Transformada de Fourier
18.
J Nanosci Nanotechnol ; 8(11): 5807-12, 2008 Nov.
Artículo en Inglés | MEDLINE | ID: mdl-19198309

RESUMEN

Multi-walled carbon nanotubes (MWCNTs) prepared by the decomposition of CH4 on a Ni-MgO catalyst were treated with air and hydrogen annealing, and the combination of air and hydrogen annealing, respectively, followed by acid reflux. The treated MWCNTs were characterized by the techniques of transmission electron microscopy, thermogravimetric analysis and flame atomic absorption spectrometry. The results showed that hydrogen annealed MWCNTs were more air stable than air annealed ones. Followed by acid treatment, the combination of air and hydrogen annealing was more efficient than either air annealing or hydrogen annealing for the removal of catalyst in MWCNTs. For the treatment with 2 h of hydrogen annealing followed by 2 h of air annealing, the catalyst Ni remained in the purified sample was 10.8 microg/g, and the yield rate was 82.3%. With 2 h of air annealing followed by 2 h of hydrogen annealing, the data were 5.8 microg/g and 61.9%, respectively. The different functions of air and hydrogen during annealing were discussed.


Asunto(s)
Cristalización/métodos , Hidrógeno/química , Metales/aislamiento & purificación , Nanotecnología/métodos , Nanotubos de Carbono/química , Nanotubos de Carbono/ultraestructura , Titanio/química , Aire , Catálisis , Calor , Sustancias Macromoleculares/química , Ensayo de Materiales , Metales/química , Conformación Molecular , Tamaño de la Partícula , Propiedades de Superficie
19.
Anal Chim Acta ; 571(2): 184-90, 2006 Jul 07.
Artículo en Inglés | MEDLINE | ID: mdl-17723437

RESUMEN

Solid-phase extraction technique had been applied to extract molybdophosphoric heteropoly acid (MoP) paired with cetyltrimethylammonium bromide (CTAB) from seawater matrix using C18 sorbent. Chemiluminescence emission could be generated via MoP reaction with alkaline luminol. Based on these, a novel on-line solid-phase extraction method coupled with flow injection (FI) analysis and luminol chemiluminescence detection had been established to determine ultratrace orthophosphate in seawater. The MoP-CTAB compound could be efficiently extracted on an in-line Sep-Pak C18 cartridge, and rapidly eluted by 0.3 mol l(-1) sulphuric acid-ethanol solution. Then the compound was reduced by luminol to produce chemiluminescence light, which could be detected using a luminescence analyzer. Experimental parameters were optimized using a univariate experimental design. Using artificial seawater with salinity of 35 as a matrix, the standard curve with a linear range between 0.005 and 0.194 micromol l(-1) had been obtained, and the recovery and the detection limit of the proposed method were found to be 92.5% and 0.002 micromol l(-1), respectively. The relative standard deviation (R.S.D.), which was determined over eight hour, was 4.66% (n=7) for the artificial seawater at a concentration of 0.097 micromol l(-1) orthophosphate. Si of 200 micromol l(-1) would not interfere with the detection of 0.012 micromol l(-1) orthophosphate compound. Three typical seawater samples were analyzed using both the proposed method and the magnesium hydroxide-induced coprecipitation (MAGIC) method, and the results of the two methods showed no significant difference using the t test. Compared to the MAGIC method, the proposed method was more sensitive, time saving and easy for on-line analysis.

20.
J Chromatogr A ; 1026(1-2): 283-8, 2004 Feb 13.
Artículo en Inglés | MEDLINE | ID: mdl-14763755

RESUMEN

A type of purified multi-walled carbon nanotubes (PMWCNTs) prepared by catalytic decomposition of methane, with a surface area of 98 m2/g, was evaluated as an adsorbent used for tapping volatile organic compounds (VOCs). The performance in evaluation was based on breakthrough volumes (BTVs) and recoveries of selected VOCs. PMWCNTs were also used as a trap packing material to adsorb VOCs purged from spiked water sample. Due to their porous structure, PMWCNTs were found to have much higher BTVs than that of Carbopack B, a graphitized carbon black with the same surface area as PMWCNTs. The recoveries of the tested VOCs trapped on PMWCNTs ranged from 80 to 110%, and not affected by the humidity of purge gas. The results indicate that PMWCNTs are a potential useful adsorbent for direct trapping VOCs from air samples and may be a supplement to VOCARB 3000, a commercially available trap, in purge-and-trap system to preconcentrate VOCs from water samples.


Asunto(s)
Cromatografía de Gases/instrumentación , Nanotubos de Carbono/química , Compuestos Orgánicos/análisis , Compuestos Orgánicos/química , Agua/química , Adsorción , Humedad , Compuestos Orgánicos/aislamiento & purificación , Reproducibilidad de los Resultados , Volatilización
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