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1.
Sensors (Basel) ; 18(12)2018 Dec 03.
Artículo en Inglés | MEDLINE | ID: mdl-30513956

RESUMEN

Buried explosive material, e.g., landmines, represent a severe issue for human safety all over the world. Most explosives consist of environmentally hazardous chemicals like 2,4,6-trinitrotoluene (TNT), carcinogenic 2,4-dinitrotoluene (2,4-DNT) and related compounds. Vapors leaking from buried landmines offer a detection marker for landmines, presenting an option to detect landmines without relying on metal detection. 2,4-Dinitrotoluene (DNT), an impurity and byproduct of common TNT synthesis, is a feasible detection marker since it is extremely volatile. We report on the construction of a wireless, handy and cost effective 2,4-dinitrotoluene biosensor combining recombinant bioluminescent bacterial cells and a compact, portable optical detection device. This biosensor could serve as a potential alternative to the current detection technique. The influence of temperature, oxygen and different immobilization procedures on bioluminescence were tested. Oxygen penetration depth in agarose gels was investigated, and showed that aeration with molecular oxygen is necessary to maintain bioluminescence activity at higher cell densities. Bioluminescence was low even at high cell densities and 2,4-DNT concentrations, hence optimization of different prototypes was carried out regarding radiation surface of the gels used for immobilization. These findings were applied to sensor construction, and 50 ppb gaseous 2,4-DNT was successfully detected.


Asunto(s)
Técnicas Biosensibles/instrumentación , Dinitrobencenos/aislamiento & purificación , Sustancias Explosivas/aislamiento & purificación , Tecnología Inalámbrica/instrumentación , Dinitrobencenos/toxicidad , Sustancias Explosivas/química , Gases/síntesis química , Gases/aislamiento & purificación , Humanos , Oxígeno/química
2.
J Chromatogr A ; 1497: 172-179, 2017 May 12.
Artículo en Inglés | MEDLINE | ID: mdl-28377164

RESUMEN

This work reports on the proof-of-principle of preparation of novel one step in-situ functionalized monolithic polysiloxane-polymethacrylate composite materials in capillary columns for enantioselective nano-HPLC using a thiol-ene click reaction. Quinine carbamate as functional monomer and ethylene dimethacrylate as crosslinker were both used as ene components in a thermally initiated double click-type polymerization reaction with poly(3-mercaptopropyl)methylsiloxane as thiol component in presence of 1-propanol as porogenic solvent. Elemental analysis and on-capillary fluorescence measurement proved the successful incorporation of the functional chiral monomer into the polymer. Scanning electron microscopy images revealed a macroporous polymer morphology which is typical for a nucleation and growth mechanism of pore formation. The individual microglobules appear relatively spherical and smooth indicating a non-porous nature. Nano-HPLC experiments of the chiral monolithic capillary column provided successful enantiomer separation of N-3,5-dinitrobenzoylleucine as test compound in polar organic elution mode clearly documenting the successful implementation of the proposed concept towards new functionalized monolithic composite materials.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Ácidos Polimetacrílicos/química , Siloxanos/química , Cromatografía Líquida de Alta Presión/instrumentación , Química Clic , Dinitrobencenos/análisis , Dinitrobencenos/aislamiento & purificación , Leucina/análogos & derivados , Leucina/análisis , Leucina/aislamiento & purificación , Metacrilatos/química , Microscopía Electrónica de Rastreo , Porosidad , Estereoisomerismo , Compuestos de Sulfhidrilo/química
3.
Bioresour Technol ; 218: 77-83, 2016 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-27347801

RESUMEN

Co-pyrolysis of polymer and biomass wastes was investigated as a novel method for waste treatment and synthesis of enhanced biochar. Co-pyrolysis of rice straw (RS) with polypropylene (PP), polyethylene (PE) or polystyrene (PS) increased the carbon content, cation exchange capacity (CEC), surface area and pH of the biochar. As a result, the sorption of 2,4-dinitrotoluene (DNT) and Pb to polymer/RS-derived biochar was markedly enhanced. The increased aromaticity and hydrophobicity may be responsible for enhancing the DNT sorption to the polymer/RS-derived biochar. In contrast, increasing CEC, higher pH, and the newly developed surface area may account for the enhancement in Pb sorption. The addition of polymer to RS did not significantly change the catalytic role of biochar during the reduction of DNT by dithiothreitol. Our results suggest that co-pyrolysis of RS and polymer can improve the biochar properties to enhance the sorption of DNT and Pb.


Asunto(s)
Biotecnología/métodos , Carbón Orgánico/química , Oryza/química , Polímeros/química , Adsorción , Biomasa , Carbono/química , Catálisis , Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Ditiotreitol/química , Electrones , Contaminantes Ambientales/química , Contaminantes Ambientales/aislamiento & purificación , Concentración de Iones de Hidrógeno , Plomo/química , Plomo/aislamiento & purificación , Brotes de la Planta/química
4.
Bioresour Technol ; 216: 1014-21, 2016 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-27343454

RESUMEN

In order to remediate organic contaminants in natural waters and soils, a novel zero-valent iron [Fe(0)]-included biochar was synthesized via slow pyrolysis. 2,4-Dinitrotoluene (DNT) and 2,4-dichlorophenol (DCP) were removed in water via sorption to the Fe(0)-included biochar. Compared to sorption control without Fe(0), the sorbed DNT and DCP were further transformed to reduction products by Fe(0)-included biochar. Compared to the reduction control with Fe(0), the presence of biochar promoted the reductive transformation of DNT and DCP. Increasing the pyrolysis temperature resulted in enhancing the removal of DNT and DCP, suggesting that the aromaticity of biochar may be responsible for the removal. The yields of the reduction products also indicated that unlike the direct reduction by Fe(0), different reduction pathways existed in the reduction of DNT and DCP with Fe(0)-included biochar. The results suggest that Fe(0)-included biochar is a viable option to immobilize and transform redox-sensitive organic contaminants in natural environments.


Asunto(s)
Carbón Orgánico/química , Clorofenoles , Dinitrobencenos , Hierro/química , Contaminantes Químicos del Agua , Purificación del Agua/métodos , Clorofenoles/análisis , Clorofenoles/química , Clorofenoles/aislamiento & purificación , Dinitrobencenos/análisis , Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación
5.
J Nanosci Nanotechnol ; 15(2): 1490-8, 2015 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-26353678

RESUMEN

This paper demonstrates the preparation and photocatalytic activity of sodium titanate nanorods and nanotubes prepared by hydrothermal method using P25-TiO2 as the precursor. XRD results confirmed the monoclinic structure of sodium titanate nanorods obtained after calcinations of orthorhombic sodium titanate nanotubes at 800 °C for 2 h. The BET surface area of sodium titanate nanotubes (176 m2 g-1) was significantly reduced for sodium titanate nanorods (21 m2 g-1) formation because of the collapsing of the hollow interior of the former during its high temperature sintering. The selective formation of m-diaminobenzene by the photoreduction of the m-dinitrobenzene was found to be comparable by sodium titanate nanorods (89.5 ± 0.5%) and P25-TiO2 (98.2 ± 0.8%), whereas Au-deposition (0.5 and 2 wt%) onto sodium titanate nanorods notably altered the products (m-nitroaniline and m-diaminobenzene) distribution after 8 h of UV-light irradiation and which was confirmed later by GC-MS analysis. This high photoactivity of as-prepared nanorods could be credited to better delocalization and longer relaxation lifetime (68 µs) of photoexcited e-/h+ pairs along the length of crystalline sodium titanate nanorods than P25-TiO2 (45 µs) as measured from Time-resolved spectroscopy. The photooxidation of sulfosulfuron herbicide (1000 ppm) and corresponding CO2 formation was found to be highest with sodium titanate nanotubes due to the presence of more hydroxyl groups over the largest surface area that dominates over its least relaxation lifetime (41 µs).


Asunto(s)
Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Nanoestructuras/química , Óxidos/química , Pirimidinas/química , Pirimidinas/aislamiento & purificación , Sulfonamidas/química , Sulfonamidas/aislamiento & purificación , Titanio/química , Catálisis , Dinitrobencenos/efectos de la radiación , Luz , Ensayo de Materiales , Nanoestructuras/efectos de la radiación , Nanoestructuras/ultraestructura , Oxidación-Reducción/efectos de la radiación , Óxidos/efectos de la radiación , Tamaño de la Partícula , Fotoquímica/métodos , Pirimidinas/efectos de la radiación , Sulfonamidas/efectos de la radiación , Propiedades de Superficie , Titanio/efectos de la radiación
6.
J Chromatogr A ; 1374: 224-230, 2014 Dec 29.
Artículo en Inglés | MEDLINE | ID: mdl-25488253

RESUMEN

In this work, a reliable and robust vacuum-outlet gas chromatography-mass spectrometry (GC-MS) method is introduced for the identification and quantification of impurities in trinitrotoluene (TNT). Vacuum-outlet GC-MS allows for short analysis times; the analysis of impurities in TNT was performed in 4min. This study shows that impurity profiling of TNT can be used to investigate relations between TNT samples encountered in forensic casework. A wide variety of TNT samples were analyzed with the developed method. Dinitrobenzene, dinitrotoluene, trinitrotoluene and amino-dinitrotoluene isomers were detected at very low levels (<1wt.%) by applying the MS in selected-ion monitoring (SIM) mode. Limits of detection ranged from 6ng/mL for 2,6-dinitrotoluene to 43ng/mL for 4-amino-2,6-dinitrotoluene. Major impurities in TNT were 2,4-dinitrotoluene and 2,3,4-trinitrotoluene. Impurity profiles based on seven compounds showed to be useful to TNT samples from different sources. Statistical analysis of these impurity profiles using likelihood ratios demonstrated the potential to investigate whether two questioned TNT samples encountered in forensic casework are from the same source.


Asunto(s)
Cromatografía de Gases y Espectrometría de Masas/métodos , Trinitrotolueno/análisis , Compuestos de Anilina/aislamiento & purificación , Dinitrobencenos/aislamiento & purificación , Cromatografía de Gases y Espectrometría de Masas/instrumentación , Funciones de Verosimilitud , Vacio
7.
Anal Chim Acta ; 773: 68-75, 2013 Apr 22.
Artículo en Inglés | MEDLINE | ID: mdl-23561908

RESUMEN

In this work the development and validation of a new procedure for the simultaneous determination of 9 nitro and polycyclic musk compounds: musk ambrette (MA), musk ketone (MK), musk mosken (MM), celestolide (ADBI), phantolide (AHMI), tonalide (AHTN), traseolide (ATII), cashmeran (DPMI) and galaxolide (HHCB) in environmental water samples (estuarine and wastewater) using microextraction by packed sorbent (MEPS) followed by large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was carried out. Apart from the optimization of the different variables affecting MEPS (i.e., nature of the sorbent, nature of the solvent elution, sample load, and elution/injection volume) extraction recovery was also evaluated, not only for water samples but also for environmental water matrices such as estuarine and waste water. The use of two deuterated analogs ([(2)H3]-AHTN and [(2)H15]-MX) was successfully evaluated in order to correct matrix effect in complex environmental matrices such as influent samples from wastewater treatment plants. Method detection limits (MDLs) ranged from 5 to 25 ng L(-1), 7 to 39 ng L(-1) and 8 to 84 ng L(-1) for influent, effluent and estuarine samples, respectively. Apparent recoveries were higher than 75% for all target compounds in all the matrices studied (estuarine water and wastewater) and the precision of the method, calculated as relative standard deviation (RSD), was below 13.2% at 200 ng L(-1) concentration level and below 14.9% at low level (20 ng L(-1) for all the target analytes, except for AHTN which was set at 40 ng L(-1) and HHCB at 90 ng L(-1), due to the higher MDL values presented by those target compounds). Finally, this MEPS procedure was applied to the determination of the target analytes in water samples, including estuarine and wastewater, from two estuaries, Urdaibai (Spain) and Adour (France) and an established stir-bar sorptive extraction-liquid desorption/large volume injection-gas chromatography-mass spectrometry (SBSE-LD/LVI-GC-MS) method was performed in parallel for comparison. Results were in good agreement for all the analytes determined, except for DPMI.


Asunto(s)
Cromatografía de Gases y Espectrometría de Masas , Compuestos Policíclicos/análisis , Contaminantes Químicos del Agua/análisis , Adsorción , Benzopiranos/análisis , Benzopiranos/aislamiento & purificación , Dinitrobencenos/análisis , Dinitrobencenos/aislamiento & purificación , Indanos/análisis , Indanos/aislamiento & purificación , Compuestos Policíclicos/aislamiento & purificación , Microextracción en Fase Sólida , Temperatura , Tetrahidronaftalenos/análisis , Tetrahidronaftalenos/aislamiento & purificación , Eliminación de Residuos Líquidos , Aguas Residuales/química , Contaminantes Químicos del Agua/aislamiento & purificación , Xilenos/análisis , Xilenos/aislamiento & purificación
8.
J Chromatogr A ; 1218(52): 9314-20, 2011 Dec 30.
Artículo en Inglés | MEDLINE | ID: mdl-22129571

RESUMEN

In this paper, two phenothiazine bonded silica (PTZ-Si) sorbents were prepared and used as sorbents of solid-phase extraction (SPE) for the determination of nitrobenzene compounds in environmental water samples by gas chromatography-mass spectrometry (GC-MS). Different synthesis routes were proposed to obtain high bonded amount of PTZ on the surface of silica gel. PTZ molecule was derived to its amino or acyl chloride derivatives for reacting with isocyanate or amino silane coupling agent, which was further reacted with the surface silanol groups of silica gel to obtain the PTZ-Si sorbents. The resultant PTZ-Si sorbents were characterized by nitrogen sorption porosimetry (NSP), Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to assure the successful bonding of PTZ on the surface of silica gel. Then the PTZ-Si sorbents were served as SPE sorbents for the enrichment of nitrobenzene compounds. Several parameters affecting the extraction performance were investigated. Under the optimized conditions, the proposed method was applied to the analysis of six nitrobenzene compounds in environmental water samples. Good linearities were obtained for all nitrobenzene compounds with R(2) larger than 0.9958. The limits of detection were found to be in the range of 0.06-0.3 ng/mL. The method recoveries of nitrobenzene compounds spiked in water samples were from 71.4% to 124.3%, with relative standard deviations (RSDs) less than 10.1%.


Asunto(s)
Dinitrobencenos/análisis , Cromatografía de Gases y Espectrometría de Masas/métodos , Fenotiazinas/química , Extracción en Fase Sólida/métodos , Tolueno/análogos & derivados , Contaminantes Químicos del Agua/análisis , Dinitrobencenos/aislamiento & purificación , Agua Dulce/química , Límite de Detección , Modelos Lineales , Reproducibilidad de los Resultados , Gel de Sílice/química , Espectroscopía Infrarroja por Transformada de Fourier , Tolueno/análisis , Tolueno/aislamiento & purificación , Contaminantes Químicos del Agua/aislamiento & purificación
9.
J Appl Microbiol ; 110(6): 1476-84, 2011 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-21395949

RESUMEN

AIMS: To evaluate the biodegradability of 2,4-DNT using an anaerobic filter (AF) combined with a biological aerated filter (BAF), and elucidate the degradation mechanism of 2,4-DNT and analyze the bacterial community of the reactors over a long period of operation. METHODS AND RESULTS: The pilot test experienced wide fluctuations influent concentrations and there was lower than 0.50 mg l(-1) of 2,4-DNT in the effluent of the system. The removal efficiency was above 99%. GC-MS analysis demonstrated that 2,4-DNT was mainly reduced to 2-amino-4-nitrotoluene (2-A-4-NT), 4-amino-2-nitrotoluene (4-A-2-NT), and 2,4-diaminotoluene (2,4-DAT) during the anaerobic reaction. In addition, ethanol was added into the influent as the electron donor. Because of the use of part ethanol as an auxiliary carbon source, more than twice the theoretical requirement of ethanol was needed to achieve a high 2,4-DNT removal efficiency (>93%). ESEM observations showed that the carrier could immobilize micro-organisms, which flourished more in reactors operating over longer periods. Further research by PCR-DGGE revealed that new 2,4-DNT-resistant bacterial had been generated during the stress of 2,4-DNT for 150 days. The dominant species for 2,4-DNT degradation were identified by a comparison with gene sequences in GenBank. CONCLUSIONS: 2,4-DNT could be effectively degraded by the combined process and ethanol played an important role in the biotransformation. The proposed transformation pathway of 2,4-DNT was concluded. During the 150-day operation, some microbial taxa unaccustomed to 2,4-DNT died out and some new 2,4-DNT-resistant microbial taxa appeared. SIGNIFICANCE AND IMPACT OF THE STUDY: The study provides a novel method for the bioremediation of 2,4-DNT, which is difficult to degrade by traditional biological methods. The most 2,4-DNT-resistant microbial taxa have not been reported elsewhere and they may be helpful to the treatment of actual 2,4-DNT wastewater.


Asunto(s)
Bacterias/metabolismo , Biotransformación , Dinitrobencenos/aislamiento & purificación , Filtración , Bacterias/genética , Biodegradación Ambiental , Reactores Biológicos , Células Inmovilizadas , Electroforesis en Gel de Gradiente Desnaturalizante , Etanol/química , Cromatografía de Gases y Espectrometría de Masas , Fenilendiaminas/metabolismo , Reacción en Cadena de la Polimerasa , ARN Ribosómico 16S/genética , Toluidinas/metabolismo , Eliminación de Residuos Líquidos/métodos
10.
J Chromatogr A ; 1218(19): 2737-44, 2011 May 13.
Artículo en Inglés | MEDLINE | ID: mdl-21324467

RESUMEN

In this paper new cellulose tribenzoate/gypsum layers in the ratio up to 8/1 (w/w) were investigated for the chiral resolution of closely related aromatic ketones (e.g. tetralones and indanones), alcohols (e.g. benzhydrols) and racemates or enantiomers of other compound classes (e.g. dinitrophenyl amino acids). Among 22 investigated compounds, 16 racemates were baseline or partially resolved by eluting with methanol or 2-propanol/water mixtures on 4/1 (w/w) layers. The best results were compared with those achieved on microcrystalline cellulose triacetate plates and on cellulose tribenzoate columns. The study of structurally related solutes allowed us to increase the knowledge of the retention and resolution mechanisms on this chiral stationary phase and to highlight the role of π-π interactions between cellulose tribenzoate and solutes with different substituents on the aromatic ring. However, some results were unexpected and confirmed the complexity of enantioseparation mechanisms, thus evidencing the importance of experimental tests. Densitometric scan in the visible region of cellulose tribenzoate/gypsum plates after their exposure to iodine vapours allowed us to successfully perform the quantitative analysis of the investigated compounds, thus overcoming the detection problems normally encountered with this stationary phase.


Asunto(s)
Benzoatos/química , Celulosa/química , Cromatografía en Capa Delgada/métodos , Aminoácidos/aislamiento & purificación , Sulfato de Calcio/química , Celulosa/análogos & derivados , Cromatografía en Capa Delgada/instrumentación , Dinitrobencenos/aislamiento & purificación , Hidrocarburos Aromáticos/aislamiento & purificación , Análisis de los Mínimos Cuadrados , Estereoisomerismo
11.
Huan Jing Ke Xue ; 32(10): 2937-42, 2011 Oct.
Artículo en Chino | MEDLINE | ID: mdl-22279905

RESUMEN

ZPF(zeoliteartificial pillared by alpha-FeOOH) which prepared in the laboratory and characterized by FTIR and XRD was used as catalyst, and was tested for its activity in catalytic H2O2, of 2,4-DNT, which is persistent and difficult to be degraded in groundwater. The degradation of 2,4-DNT was examined at different pHs in the reduction, catalytic oxidation and combination technology of reduction-catalytic oxidation reaction systems. Moreover, the removal effect of 2,4-DNT was compared by these three approaches and the catalytic oxidation mechanism was analyzed. The results demonstrated that the removal effect of 2,4-DNT reduced to 2,4-DAT was up to 96.6% in 120 min at pH = 5, which was 1.2, 2.0 times of the rate at pH 7, pH 9 respectively. The catalytic effect was various at different pHs and more significant when the pH close to the zero point of charge of alpha-FeOOH. The order of removal effect of 2,4-DNT at different pHs was pH = 7 > pH = 9 > pH = 5. Compared to single reduction or catalytic oxidation, the removal effect of combination technology was 57.4%, which was evidently improved on the base of 2,4-DNT reduced to 2,4-DAT. The degradation of 2,4-DNT in the presence of ZPF/H2O2 follows a first-order kinetic model and the k(obs) was 0.002 7 min(-1). Due to the concentration of dissolved Fe ion was far less than 0.07 mmol/L, the mechanism was heterogeneous Fenton reaction acting on the surface of the catalyst. Therefore the combination technology was superior to the single treatment of reduction or catalytic oxidation.


Asunto(s)
Dinitrobencenos/aislamiento & purificación , Hierro/química , Contaminantes Químicos del Agua/aislamiento & purificación , Zeolitas/química , Carcinógenos/química , Carcinógenos/aislamiento & purificación , Catálisis , Dinitrobencenos/química , Agua Subterránea/análisis , Peróxido de Hidrógeno/química , Concentración de Iones de Hidrógeno , Oxidación-Reducción , Contaminantes Químicos del Agua/química
13.
J Chromatogr A ; 1217(43): 6674-80, 2010 Oct 22.
Artículo en Inglés | MEDLINE | ID: mdl-20570269

RESUMEN

Molecularly imprinted sorbents were synthesized and used as selective extraction sorbents for the analysis of nitroaromatic explosives. Their synthesis by radical polymerization using organic monomers and by sol-gel approach using organosilanes was considered to develop a selective sorbent. The sol-gel approach with phenyltrimethoxysilane (PTMS) as monomer and 2,4-dinitrotoluene (2,4-DNT) as template gave the most promising results. An optimized procedure adapted to the selective treatment of aqueous samples was then developed and applied to various target explosives. For the first time four nitroaromatic compounds were retained on the molecularly imprinted silica (MIS) with extraction recoveries between 29% and 81%, while only low recoveries were obtained on the non-imprinted sorbent, thus highlighting the high degree of selectivity. The MIS was then used for the clean-up of a sample containing motor oil spiked with 2,4-DNT and 2,4,6-trinitrotoluene (2,4,6-TNT). The results were compared with those obtained using a conventional sorbent (Oasis HLB). The cleanest chromatogram obtained using the MIS emphasized the high potential of the MIS as selective sorbent.


Asunto(s)
Sustancias Explosivas/aislamiento & purificación , Impresión Molecular , Nitrobencenos/aislamiento & purificación , Extracción en Fase Sólida/métodos , Tolueno/análogos & derivados , Acrilamida/química , Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Sustancias Explosivas/química , Metacrilatos/química , Nitrobencenos/química , Compuestos de Organosilicio/química , Petróleo , Picratos/química , Picratos/aislamiento & purificación , Sensibilidad y Especificidad , Tolueno/química , Tolueno/aislamiento & purificación
14.
Environ Sci Technol ; 43(20): 7870-6, 2009 Oct 15.
Artículo en Inglés | MEDLINE | ID: mdl-19921907

RESUMEN

A microporous carbon with very high specific surface area and narrow pore size distribution was synthesized using Y zeolite as a template. The structural, porosity, and surface characteristics of the material were investigated by elemental analysis, N2 adsorption, powder X-ray diffraction, and Raman spectroscopy. The batch adsorption technique was performed to assess adsorption of three monoaromatic compounds, phenol, 1,3-dichlorobenzene, and 1,3-dinitrobenzene, on the synthesized carbon. Nonporous graphite, single-walled carbon nanotubes, and two commercial microporous activated carbons were also included as comparative adsorbents. The synthesized microporous carbon showed extraordinarily high adsorption affinity (comparable or higher than activated carbons and carbon nanotubes) for the three adsorbates, and very fast adsorption/ desorption kinetics (equilibrium reached less than 3 h) and complete adsorption reversibility for phenol. These adsorption properties were attributed to the large hydrophobic surface area and the regular-shaped, open and interconnected three-dimensional pore structure of the synthesized microporous carbon. Additionally, with normalization of adsorbent surface area adsorption of a bulky solute, 1,2,4,5-tetrachlorobenzene, was prominently higher on the synthesized carbon than on the activated carbons, due to alleviated size exclusion effect. Findings of the present work highlight the potential of using zeolite-templated carbons as effective adsorbents for removal of hydrophobic organic contaminants in water treatment.


Asunto(s)
Carbono/química , Clorobencenos/aislamiento & purificación , Dinitrobencenos/aislamiento & purificación , Fenol/aislamiento & purificación , Purificación del Agua , Adsorción , Cinética , Termodinámica , Zeolitas
15.
J Chromatogr A ; 1216(35): 6310-8, 2009 Aug 28.
Artículo en Inglés | MEDLINE | ID: mdl-19640542

RESUMEN

Dual high-speed countercurrent chromatography (dual CCC) literally permits countercurrent flow of two immiscible solvent phases continuously through the coiled column for separation of solutes according to their partition coefficients. Application of this technique has been successfully demonstrated by separation of analytes by gas-liquid and liquid-liquid two-phase systems. However, the method cannot be directly applied to the system with a set of coiled columns connected in series, since the countercurrent process is interrupted at the junction between the columns. However, this problem can be solved by intermittent dual CCC by eluting each phase alternately through the opposite ends of the separation column. This mode of application has an advantage over the conventional dual CCC in that the method can be applied to all types of CCC systems including hydrostatic equilibrium systems such as toroidal coil CCC and centrifugal partition chromatography. Recently, the application of this method to high-speed CCC (hydrodynamic system) has been demonstrated for separation of natural products by Hewitson et al. using a set of conventional multilayer coil separation columns connected in series. Here, we have developed a mathematical model for this intermittent dual CCC system to predict retention time of the analytes, and using a simplified model system the validity of the model is justified by a series of basic studies on both hydrodynamic and hydrostatic CCC systems with a computer-programmed single sliding valve. The present method has been successfully applied to spiral tube assembly high-speed CCC (hydrodynamic system) and toroidal coil CCC (hydrostatic system) for separation of DNP-amino acid samples with two biphasic solvent systems composed of hexane-ethyl acetate-methanol-0.1M hydrochloric acid (1:1:1:1 and 4:5:4:5, v/v).


Asunto(s)
Distribución en Contracorriente/instrumentación , Modelos Teóricos , Aminoácidos/aislamiento & purificación , Dinitrobencenos/aislamiento & purificación , Programas Informáticos
16.
J Forensic Sci ; 54(4): 846-50, 2009 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-19457149

RESUMEN

The application of attenuated total reflection (ATR)-Fourier transform infrared (FTIR) spectromicroscopy for detection of explosive particles in fingerprints is described. The combined functions of ATR-FTIR spectromicroscopy are visual searching of particles in fingerprints and measuring the FTIR spectra of the particles. These functions make it possible to directly identify whether a suspect has handled explosives from the fingerprints alone. Particles in explosive contaminated fingerprints are either ingredients of the explosives, finger residues, or other foreign materials. These cannot normally be discriminated by their morphology alone. ATR-FTIR spectra can provide both particle morphology and composition. Fingerprints analyzed by ATR-FTIR can be used for further analysis and identification because of its non-destructive character. Fingerprints contaminated with three different types of explosives, or potential explosives, have been analyzed herein. An infrared spectral library was searched in order to identify the explosive residues. The acquired spectra are compared to those of finger residue alone, in order to differentiate such residue from explosive residue.


Asunto(s)
Dermatoglifia , Sustancias Explosivas/aislamiento & purificación , Espectroscopía Infrarroja por Transformada de Fourier , Trinitrotolueno/aislamiento & purificación , Dinitrobencenos/aislamiento & purificación , Humanos , Nitratos/aislamiento & purificación , Polvos , Trinitrobencenos/aislamiento & purificación
17.
Chemosphere ; 72(4): 601-7, 2008 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-18433833

RESUMEN

Oxidative degradation of dinitrotoluene (DNT) isomers and 2,4,6-trinitrotoluene (TNT) in spent acid was conducted by Electro-Fenton's reagents. The electrolytic experiments were carried out to elucidate the influence of various operating parameters on the performance of mineralization of total organic compounds (TOC) in spent acid, including reaction temperature, dosage of oxygen, sulfuric acid concentration and dosage of ferrous ions. It deserves to note that organic compounds could be completely destructed by Electro-Fenton's reagent with in situ electrogenerated hydrogen peroxide obtained from cathodic reduction of oxygen, which was mainly supplied by anodic oxidation of water. Based on the spectra analyzed by gas chromatograph/mass spectrometer, it is proposed that initial denitration of 2,4,6-TNT gives rise to formation of 2,4-DNT and/or 2,6-DNT, which undergo the cleavage of nitro group into o-mononitrotoluene, followed by denitration to toluene and subsequent oxidation of the methyl group. Owing to the removal of both TOC and partial amounts of water simultaneously, the electrolytic method established is potentially applied to regenerate spent acid from toluene nitration processes in practice.


Asunto(s)
Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Peróxido de Hidrógeno/química , Hierro/química , Trinitrotolueno/química , Trinitrotolueno/aislamiento & purificación , Electroquímica , Electrólisis , Compuestos Ferrosos/química , Gases/química , Ácido Clorhídrico/química , Isomerismo , Minerales/química , Oxidación-Reducción , Oxígeno/química , Aguas del Alcantarillado/química , Ácidos Sulfúricos/química , Temperatura
18.
J Sep Sci ; 30(6): 804-12, 2007 Apr.
Artículo en Inglés | MEDLINE | ID: mdl-17536724

RESUMEN

A novel bovine serum albumin (BSA)-modified magnesia-zirconia stationary phase was prepared using the sodium salt of cis-(3-methyloxiranyl)phosphonic acid (fosfomycin) as spacer and glutaraldehyde as coupler. Baseline separation of six derivatized amino acids (DNB-Leu, Dansyl-Val, etc.) was achieved on this column using ammonium acetate buffer-isopropanol mobile phase at a flow rate of 1.0 mL/min. The effects of mobile phase composition, eluent pH value, column temperature, and flow rate on the retention and separation of chiral compounds were also investigated. The BSA chiral stationary phase (BSA-CSP) was relatively stable under experimental conditions. The coupling reaction in this method was mild, reliable, and reproducible; thus it was also suitable for the immobilization of various biopolymers with amino groups in the preparation of chromatography stationary phases.


Asunto(s)
Fosfomicina/química , Óxido de Magnesio/química , Compuestos Orgánicos/aislamiento & purificación , Albúmina Sérica Bovina/química , Circonio/química , Animales , Bovinos , Cromatografía Liquida/métodos , Compuestos de Dansilo/aislamiento & purificación , Dinitrobencenos/aislamiento & purificación , Leucina/análogos & derivados , Leucina/aislamiento & purificación , Estructura Molecular , Organofosfonatos/química , Preparaciones Farmacéuticas/aislamiento & purificación , Fenilalanina/aislamiento & purificación , Espectroscopía Infrarroja por Transformada de Fourier , Estereoisomerismo , Temperatura , Triptófano/análogos & derivados , Triptófano/aislamiento & purificación , Valina/análogos & derivados , Valina/aislamiento & purificación
19.
Ultrason Sonochem ; 13(4): 303-7, 2006 May.
Artículo en Inglés | MEDLINE | ID: mdl-15990352

RESUMEN

The removal of nitroaromatics from polluted water is difficult due to their high stability to conventional treatment methods. This paper presents a method for the destruction of 1,3-dinitrobenzene and 2,4-dinitrotoluene in aqueous solutions. The compounds are shown to be stable to reaction with ozone, even under ultrasonic activation. The use of ultrasound enhances the rate of electrochemical reduction but the overall rate of reaction is still slow. However, the simultaneous application of ultrasound and ozonation to the electrochemical reaction allows virtually complete destruction of the compounds in short times. The effect is attributed to the ultrasonic enhancement of the electrochemical process giving intermediates that are susceptible to ozone oxidation. While further analytical work is needed to deduce the exact contributions of the various possible degradation mechanisms, the work demonstrates the synergies that can be gained by using combined techniques for the destruction of these difficult compounds.


Asunto(s)
Dinitrobencenos/aislamiento & purificación , Ozono/química , Ultrasonido , Eliminación de Residuos Líquidos/métodos , Purificación del Agua/métodos , Electroquímica/métodos , Factores de Tiempo
20.
J Hazard Mater ; 136(1): 61-7, 2006 Aug 10.
Artículo en Inglés | MEDLINE | ID: mdl-16359784

RESUMEN

Electrokinetic soil remediation has been proven to remove heavy metals and polar organics from low hydraulic conductivity subsurface environment. In this study, carboxymethyl-beta-cyclodextrin (CMCD) was used as a carrier to assist electrokinetic treatment for removal of low polarity organic contaminants from soils (2.2% organic carbon content). Naphthalene and 2,4-dinitrotoluene (2,4-DNT) were selected as the test compounds. The results from columns experiments showed that 46 and 43% of naphthalene and 2,4-DNT, respectively, were removed using 0.01 N NaNO(3) flushing solution with 40 V electrical potential while 70 and 72% of naphthalene and 2,4-DNT were removed using 2 g/L CMCD solution. Naphthalene and 2,4-DNT removal was enhanced to 83 and 89%, respectively, by using 2 g/L CMCD with 40 V electrical potential. Findings from this study also demonstrated that cyclodextrin assisted electrokinetics can enhance the removal rate of naphthalene and 2,4-DNT. Electric potential applied has more influence on the contaminant removal than the amount of CMCD used. Higher voltage application caused increase in the removal rate of naphthalene and 2,4-DNT, and appeared to be one of the critical factors in obtaining higher contaminant removal while increasing CMCD solution concentration above 2 g/L appeared to have little effect on the contaminant removal.


Asunto(s)
Dinitrobencenos/química , Dinitrobencenos/aislamiento & purificación , Naftalenos/química , Naftalenos/aislamiento & purificación , Contaminantes del Suelo/aislamiento & purificación , Electroquímica , Cinética , Soluciones , beta-Ciclodextrinas/química
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