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PubMed2005

Fe-based nanoparticulate metallic alloys as contrast agents for magnetic resonance imaging.

Pharmaceutical grade magnetic colloidal dispersions have been prepared from iron alloys synthesized by laser pyrolysis. The colloids were obtained by simultaneous dispersion and coating of the particles with dextran in a strong alkaline solution. Both powders and dispersions have been analyzed in terms of microstructural characteristics, chemical composition and magnetic properties. The powders consist of uniform spherical nanoparticles (12 nm of diameter) showing a metallic core encapsulated into an iron-oxide shell. On the other hand, the colloidal dispersions consist of magnetic particles-aggregates with hydrodynamic sizes of approximately 75 nm. Magnetic resonance images of rats were taken after the intravenously administration of the Fe colloidal dispersions, and compared with those obtained using a commercial iron oxide magnetic resonance imaging contrast agent. The results showed a contrast improvement of 60% in the liver with respect to the commercial sample, which suggests that this product could be a suitable contrast agent for NMR imaging of liver and spleen.

Alloys↗

PubMed2005

Chemical characterization of pitch deposits produced in the manufacturing of high-quality paper pulps from hemp fibers.

The composition of pitch deposits occurring in pulp sheets and mill circuits during soda/anthraquinone pulping and elemental chlorine-free pulp bleaching of bast fibers of industrial hemp (Cannabis sativa) was studied. Pitch deposits were extracted with acetone, and the extracts analyzed by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). Acetone extracts (15-25% of pitch deposits) were constituted by the defoamers used at the mill and by lipophilic extractives from hemp fibers. Acetone-insoluble residues (75-85% of pitch deposits) were analyzed by pyrolysis-GC/MS in the presence and absence of tetramethylammonium hydroxide. These residues were constituted by salts of fatty acids (arising from hemp fibers) with calcium, magnesium, aluminum and other cations that were identified in the deposits. It was concluded that inappropriate use of defoamer together with the presence of multivalent ions seemed to be among the causes of hemp extractives deposition in the pitch problems reported here.

Acetone↗

PubMed2005

Physical and thermochemical characterization of rice husk char as a potential biomass energy source.

The fixed bed pyrolysis of rice husk was studied under conventional conditions with the aim of determining the characteristics of the charcoal formed for its applicability as a solid fuel. Thermoanalytic methods were used to determine the kinetic parameters of its combustion. Palletisation using different binders and techniques to improve the time of sustained combustion of the char pallets were investigated. The optimum temperature for carbonization to obtain a char having moderately high heating value was found as 400 degrees C. For the active char combustion zone, the order of reaction was nearly 1, the activation energy 73.403 kJ/mol and the pre-exponential factor 4.97 x 10(4)min(-1). Addition of starch as a binder and 10% ferrous sulphate heptahydrate or sodium hypophosphite as an additive enhanced the ignitibility of the char pallets.

Bioelectric Energy Sources↗

PubMed2005

Select metal adsorption by activated carbon made from peanut shells.

Agricultural by-products, such as peanut shells, contribute large quantities of lignocellulosic waste to the environment each growing season; but few, if any, value-added uses exist for their disposal. The objective of this study was to convert peanut shells to activated carbons for use in adsorption of select metal ions, namely, cadmium (Cd2+), copper (Cu2+), lead (Pb2+), nickel (Ni2+) and zinc (Zn2+). Milled peanut shells were pyrolyzed in an inert atmosphere of nitrogen gas, and then activated with steam at different activation times. Following pyrolysis and activation, the carbons underwent air oxidation. The prepared carbons were evaluated either for adsorption efficiency or adsorption capacity; and these parameters were compared to the same parameters obtained from three commercial carbons, namely, DARCO 12x20, NORIT C GRAN and MINOTAUR. One of the peanut shell-based carbons had metal ion adsorption efficiencies greater than two of the three commercial carbons but somewhat less than but close to Minotaur. This study demonstrates that peanut shells can serve as a source for activated carbons with metal ion-removing potential and may serve as a replacement for coal-based commercial carbons in applications that warrant their use.

Adsorption↗

PubMed2006

Preparation of activated carbons from cattle-manure compost by zinc chloride activation.

Dried cattle-manure compost was pyrolyzed by a one-step process to obtain activated carbon using chemical activation by zinc chloride. The influence of activation parameters such as ZnCl(2) to cattle-manure compost (ZnCl(2)/CMC) ratio, activation temperature and retention time on the final products was investigated. The resultant activated carbons were characterized by nitrogen adsorption-desorption isotherms at 77 K. The results showed that the surface area and pore volume of activated carbons, which were estimated by BET and t-plot methods, were achieved as high as 2170 m(2)/g and 1.70 cm(3)/g in their highest value, respectively. Thermogravimetric analysis (TGA) was carried out to monitor the pyrolysis process of cattle-manure compost (CMC) and ZnCl(2) impregnated one (ZnCl(2)/CMC). The capabilities of phenol adsorption were also examined for the CMC carbons prepared with various treatments.

Adsorption↗

PubMed2006

Low temperature conversion of rice husks, eucalyptus sawdust and peach stones for the production of carbon-like adsorbent.

In this study, the feasibility of preparing effective adsorbents from unmitigated agroforestry wastes was investigated. Three different kinds of carbon-like materials were produced by low temperature pyrolysis (LTC, <500 degrees C) of the raw materials rice husks, eucalyptus sawdust and peach stones. The carbon-like materials were characterized by instrumental methods (SEM,X-RDS,BET,MAS-RMN,FTIR), physico-chemical adsorption (iodine-, methylene blue- and phenazone-number; acetic acid adsorption isotherm; textile dyes- and carbohydrate adsorption), and heat value determination. The produced materials, which showed appreciable adsorption capacity, can be considered as precursors for the production of active coal or even be used directly as well.

Adsorption↗

PubMed2026

Metagenomic insights into the mechanisms of heteroatom-doped, iron-loaded biochar in enhancing anaerobic digestion of waste activated sludge.

Anaerobic digestion is a crucial technology for resource recovery from waste activated sludge. Enhancing its methane production efficiency using conductive materials is a key research objective. This study aimed to elucidate the mechanisms by which conductive materials promote this process. Three types of biochar(FeS@BC300, FeP@BC600, and FeP@BC900) were prepared by doping bamboo powder with N, P, S and iron salts under pyrolysis conditions at 300-900 °C, and their physical and chemical properties were characterized, including surface functional groups, specific surface area, capacitance, electrical resistance, electron-accepting capacity (EAC), and electron-donating capacity (EDC). These analyses assessed the influence of synthesis parameters. These materials were subsequently introduced into the anaerobic digestion of thermally hydrolyzed sludge to evaluate their impacts on methanogenic performance, microbial community structure, and metabolic pathways. The results show that the FeP@BC600 material, which exhibited the highest EDC, substantially increased microbial cytochrome c production (by 29.2 % compared to the control). This enhancement improved interspecies electron transfer, stimulated ATP synthesis (increased by 41.5 %), and reinforced both hydrogenotrophic and acetoclastic methanogenic pathways, ultimately elevating methane production by 55 %. Integrated analysis of metagenomic data, material properties, and performance metrics revealed that the key mechanism by which FeP@BC600 promotes methanogenesis is through the enrichment of cytochrome c-encoding genes, thereby facilitating direct interspecies electron transfer (DIET) and augmenting ATP synthesis. This study provides a foundation for the subsequent application of conductive materials to enhance anaerobic digestion and offers guidance for the optimized design of such materials.

Sewage↗

PubMed2005

From MEMS to NEMS with carbon.

Our work in carbon-microelectromechanical systems (C-MEMS) suggests that C-MEMS might provide a very interesting material and microfabrication approach to battery miniaturization, active DNA arrays and a wide variety of chemical and biological sensors. In C-MEMS, photoresist is patterned by photolithography and subsequently pyrolyzed at high-temperatures in an oxygen-free environment. We established that it is possible to use C-MEMS to create very high-aspect ratio carbon structures (e.g. posts with an aspect ratio >10), suspended carbon plates and suspended carbon nanowires (C-NEMS). By changing the lithography conditions, soft and hard baking times and temperatures, additives to the resist, pyrolysis time, temperature and environment, C-MEMS permits a wide variety of interesting new MEMS and NEMS applications that employ structures having a wide variety of shapes, resistivities and mechanical properties. We also demonstrate that arrays of high-aspect ratio carbon posts can be charged/discharged with Li and this enables the fabrication of a smart switchable array of batteries.

Biocompatible Materials↗

PubMed2006

Metallic oxide CdIn2O4 films for the label free electrochemical detection of DNA hybridization.

DNA functionalised semiconductor metallic oxide electrodes have been developed for the direct electrochemical detection of DNA hybridization, without labelling or the introduction of a redox couple. Conductive CdIn(2)O(4) thin films with controlled properties were deposited on glass substrates using an aerosol pyrolysis technique. The films exhibit a polycrystalline microstructure with a surface roughness of 1.5 nm (r.m.s.) and an electrical resistivity ranging between 1 and 3 x 10(-3) Omega cm. These electrodes were functionalised using hydroxylation and silanisation steps, to allow the binding of DNA probe sequences (20 bases). The electrical detection of DNA hybridization with complementary sequences has been performed using electrochemical impedance spectrometry (EIS) measuring the variation of impedance before and after hybridization. Two set-ups were used, a standard set-up including three electrodes and a set-up including two symmetrical electrodes. In both configurations, a significant increase of the impedance modulus, more particularly of the real part of the impedance (160-225% according to the electrochemical cell used) has been obtained over a frequency range of 10-10(5)Hz. DNA hybridization has also been systematically confirmed using the fluorescence spectrometry. This study emphasizes the high sensitivity of the CdIn(2)O(4) as a working electrode for the detection of biological events occurring at the electrode surface.

Biosensing Techniques↗

PubMed2006

Synthesis of 13-(substituted benzyl) berberine and berberrubine derivatives as antifungal agents.

By introducing various aromatic groups in 13-C of berberine and berberrubine, a series of 13-(substituted benzyl) berberine and berberrubine derivatives were synthesized and examined for antifungal activities against various human pathogenic fungi. The synthesized compounds exhibited more potent antifungal activities than berberine and berberrubine. Among them, 13-(4-isopropyl benzyl) berberine (6e) exerted the most potent antifungal activities against Candida species (MIC=1-8 microg/ml) and a 4-fold stronger activity than 13-(4-isopropyl benzyl) berberrubine (7e) synthesized by pyrolysis of compound 6e.

Antifungal Agents↗

PubMed2004

Preparation of activated carbon using low temperature carbonisation and physical activation of high ash raw bagasse for acid dye adsorption.

Activated carbons were prepared from bagasse through a low temperature (160 degrees C) chemical carbonisation treatment and gasification with carbon dioxide at 900 degrees C. The merit of low temperature chemical carbonisation in preparing chars for activation was assessed by comparing the physical and chemical properties of activated carbons developed by this technique to conventional methods involving the use of thermal and vacuum pyrolysis of bagasse. In addition, the adsorption properties (acid blue dye) of these bagasse activated carbons were also compared with a commercial activated carbon. The results suggest that despite the high ash content of the precursor, high surface areas (614-1433 m2 g(-1)) and microporous (median pore size from 0.45 to 1.2 nm) activated carbons can be generated through chemical carbonisation and gasification. The micropore area of the activated carbon developed from chars prepared by the low temperature chemical carbonisation provides favourable adsorption sites to acid blue dye (391 mg g(-1) of carbon). The alkalinity of the carbon surface and total surface area were shown to have complementary effects in promoting the adsorption of acid blue dye. Adsorption of the anionic coloured component of the acid dye was shown to be promoted in carbon exhibiting alkaline or positively charged surfaces. This study demonstrates that activated carbons with high acid dye adsorption capacities can be prepared from high ash bagasse based on low temperature chemical carbonisation and gasification.

Adsorption↗

PubMed2004

Organic matrix in produced water from the Osage-Skiatook petroleum environmental research site, Osage county, Oklahoma.

Produced water (water co-produced with oil and gas) constitutes the single largest waste stream for oil and gas industry. Reclaiming this water for beneficial use is thought to be one of the most practical solutions that can solve both environmental and water shortage problems. The feasibility of this practice depends on the ability to remove its chemical content to the levels that meets the appropriate standards. Organic compounds are probably the most difficult fraction to handle. In this paper, the discrete organic compounds and non-volatile, macromolecular organic compounds (i.e., natural organic matter--NOM) of three produced water samples from the Osage-Skiatook Environmental Research site were characterized. Two of the three produced waters had very little contribution from NOM, while one of the samples had about 23% NOM contribution to its organic matrix pool. Fluorescent spectrophotometric scans provided little differentiation among the organic quality of the produced water, while pyrolysis-GC/MS showed that the NOM characteristics of the three produced waters were distinct. Specifically, the overall halogenated content and aromaticity of the NOM were found to be possible qualifiers that distinguish produced water from the coalbed methane well from produced water from the oil well. And the specific chemical fragments that are linked to polysaccharide sources were found to be potential identifiers that distinguish produced water from the newer oil well from produced water from the older oil well. These identifiers were, however, only suggested for this preliminary study. More samples must be included to build a substantial database on produced water NOM to confirm and identify more markers.

Gas Chromatography-Mass Spectrometry↗

PubMed2005

Identification of chemical substances in industrial wastes and their pyrolytic decomposition products.

In order to quantify the sources of chemical pollutants in the leachate from reclaimed wastes, chemical substances in 11 different types of industrial wastes were identified. Their elution behaviors were also investigated. Alkanes (5.3-890 ng g(-1)), benzenes (8.1-110 ng g(-1)), polyaromatic hydrocarbons (PAHs) (3.2-560 ng g(-1)), alcohols, steroids, phenol (7.1 ng g(-1)), ketones, furans (190-210 ng g(-1)), phthalates (8.9-560 ng g(-1)), benzoquinones, dibenzothiophene (190 ng g(-1)), benthiocarb (4.2 ng g(-1)), sulfur, nitrile compounds, amino compounds, amido compounds, pyridines, quinolines (1.8-15 ng g(-1)), isoquinolines, carbazoles, acridines, chlordenes (1.5-1.6 ng g(-1)) and nonachlors (1.1-1.6 ng g(-1)) were detected in 9 types of industrial wastes. The chemical substances detected in waste at the highest concentrations were alkanes, PAHs and phthalates. Water supply sludge, dust and brick garbage contained many kinds of chemical substances. The elution behaviors of specific chemical substances, COD and nutrients varied by characteristic and production process of each waste. Over 100 different compounds were detected in pyrolysis products including carbohydrate, carotynoid, amino acids, proteins, humic acids, lignin and combustion products.

Dust↗

PubMed2005

Guidelines for routine mercury speciation analysis in seafood by gas chromatography coupled to a home-modified AFS detector. Application to the Andalusian coast (south Spain).

A home-modified atomic fluorescence detector (mAFS) has been employed for mercury and methylmercury determination in bivalves from the Andalusian coast (south Spain). This modification consists on the inclusion of a quartz flow cell into the detector, which increases the concentration of mercury atoms in the detector and therefore enhances sensitivity about two fold. Two analytical approaches for mercury speciation based on the coupling of gas chromatography on-line pyrolysis and mAFS (GC-Pyro-mAFS) have been tested. The first approach (Method 1) is based on aqueous ethylation followed by extraction into an organic solvent, and the second one (Method 2) in the extraction of monoalkylated mercury as chloride. Method 1 is a rapid procedure but not sensitive enough for the analysis of methylmercury in non-polluted sites (detection limit: 20 ng g(-1) as mercury, wet basis). The second one is quite more sensitive (detection limit: 0.2 ng g(-1), wet weight), but sample treatment is cumbersome and time-consuming. The optimum range for mercury determination for both methods are complementary and exhibit an overlapping measurable concentration range (OMCR) in which methylmercury can be indistinctly determined (75-100 ng g(-1) as mercury, wet basis). The suitability of both methods has been assayed with spiking experiences at levels within the OMCR with good recoveries. Both approaches have been validated with two certified reference materials (BCR-463, mercury and methylmercury in tuna fish; and NIST-2977, organic contaminants and trace metals in mussel tissue). Both procedures have been used for the analysis of three species of bivalve molluscs collected along the Andalusian coast (south Spain), all of them employed for human consumption (Chamelea gallina, Donax trunculus and Scrobicularia plana), and their potential use in routine analysis has been established.

Animals↗

PubMed2006

A study of polycyclic aromatic hydrocarbons concentrations and source identifications by methods of diagnostic ratio and principal component analysis at Taichung chemical Harbor near Taiwan Strait.

Fine (PM(2.5)) and Coarse (PM(2.5-10)) particulates concentrations of ambient air particle-bound polycyclic aromatic hydrocarbons (PAHs) were measured simultaneously from February 2004 to January 2005 at the Taichung Harbor (TH) sampling site near Taiwan of central Taiwan. Particle-bound polycyclic aromatic hydrocarbons (PAHs) were collected on quartz filters, the collected sample used soxhlet analytical method extracted with a dichloromethane (DCM)/n-hexane mixture (50/50, v/v) for 24h, and then the extracts were subjected to gas chromatography-mass spectrometric (GC-MS) analysis. The results indicated that vehicle emissions, coal combustion, incomplete combustion and pyrolysis of fuel and oil burning were the main source of PAHs near Taiwan Strait of central Taiwan. Diagnostic ratio and principal component analysis (PCA) were also used to characterize and identify PAHs emission source in this study.

Air Pollutants↗

PubMed2004

Application of high-performance liquid chromatography with ultraviolet diode array detection and refractive index detection to the determination of class composition and to the analysis of gasoline.

A method of effective application of normal-phase high-performance liquid chromatography (NP-HPLC) with ultraviolet diode array detection (DAD) and refractive index detection (RID) for the determination of class composition of gasoline and its components, i.e. for the determination of content of alkenes, aromatic and saturated hydrocarbons in gasoline meeting modern quality standards, has been developed. An aminopropyl-bonded silica stationary phase was used along with n-hexane or n-heptane as the mobile phase. A DAD signal integrated over the 207-240 nm range was used to determine alkenes. This eliminates the necessity of separating alkenes from saturates, because the latter do not absorb UV radiation above 200 nm. The content of aromatic hydrocarbons is determined by means of a refractive index detector. Calibration was based on hydrocarbon type composition determined by the fluorescent indicator adsorption method, ASTM D1319. The results obtained by the developed method were found to be consistent with those obtained by fluorescent indicator adsorption or by a multidimensional GC method (PIONA) (ASTM D5443). The method can be applied to gasoline meeting recent quality standards, irrespective of refining technology used in the production of gasoline components, including gasoline with various contents of oxygenates. The developed method cannot be used to determine the hydrocarbon type composition of gasoline that contains as a component the so-called pyrocondensate, i.e. the fraction with a boiling point up to 220 degrees C, obtained through thermal pyrolysis of distillation residues of crude oil or coal and, consequently, does not meet the quality standards. The paper includes the procedure for identification of this type of gasoline.

Chromatography, High Pressure Liquid↗

PubMed2004

Development of a novel solid-phase extraction element for thermal desorption gas chromatography analysis.

A novel solid-phase extraction element is developed for sorptive enrichment of dilute analytes from liquid samples with high extraction efficiencies due to its larger amounts of polydimethylsiloxane (PDMS) absorbent than the conventional syringe type of solid-phase microextraction (SPME). The extraction element is made of titanium (Ti) open tubular tube (30 mm x 1.2 mm i.d. x 1.6 mm o.d.) coated with a chemically bonded layer of PDMS (500 microm in thickness). The extraction element combined with thermal desorption-gas chromatography-mass spectrometry using a pyrolysis-gas chromatography-mass spectrometry system was used to extract and analyze a typical herbicide, bethrodine in water samples over a concentration range from 2.5 to 2.5 x 10(4) ng/l. Thus obtained calibration curve showed good linearity for the tested whole concentration range with regression coefficient of 0.992. Detection limit of 0.5 ng/l level was achieved and the reproducibility of the measurements for bethrodine at 10 ng/l level was found to be fairly good with relative standard deviation below 7.5%.

Calibration↗

PubMed2005

Determination of mercury species in fish reference materials by gas chromatography-atomic fluorescence detection after closed-vessel microwave-assisted extraction.

A simple and rapid method has been developed for speciation analysis of inorganic mercury and monomethylmercury (MMHg) in biological tissues. The procedure is based on the quantitative closed-vessel microwave-assisted leaching of mercury from biological samples with an alkaline extractant. The extracted mercury species are ethylated and analysed by capillary gas chromatography coupled to an atomic fluorescence detector via pyrolysis (CGC-pyro-AFS). The coupling between capillary gas chromatography and atomic fluorescence detector was optimized with the aim of minimizing the detection limits and time necessary for the species-selective determination of mercury compounds. The use of closed-vessel microwave-assisted extraction along with no clean-up steps before the ethylation leads to a significant total analysis time decrease with respect to similar procedures. The detection limit was 2 pg for MMHg (as Hg) and 1 pg for inorganic mercury. The method was validated by the analysis of DORM-2 (dogfish muscle) and DOLT-3 (dogfish liver) certified reference materials. The inorganic mercury and methylmercury concentrations found were in good agreement with the certified values. Recovery studies of fish muscle tissue spiked with inorganic mercury and MMHg were done to check the reliability of the method. In all cases satisfactory recoveries (92-105%) were obtained.

Animals↗