British Library Electronic Table of Contents (United Kingdom)

Ochratoxin A (OTA) was analyzed from 44 liquorice confectionery samples using immunoaffinity cleanup and liquid chromatography coupled with fluorescence detection. The presence of OTA was confirmed by methyl-ester derivatization. Liquorice confectionery samples were purchased from different retail outlets and supermarkets in Spain during 2007-2008, 16 of hard candies and 28 of soft candies. The incidence of OTA varied between 75% and 39% and mean ranged from 2.96 to 0.34mg/kg for hard and soft candies, respectively. Assuming a total mean value of 1.29mgOTA/kg sweet and a consumption of about 1.2g liquorice sweets per day, an OTA weekly uptake of 11ng was obtained, or, based on a total body weight of 30kg for a child consuming these sweets regularly, a weekly intake of 0.37ng/kg body weight...

Energy Technology Data Exchange (ETDEWEB)

The development and evaluation of a post-column reaction detector sensitive to platinum(II) complexes is presented in which sodium bisulfite is used as the derivatizing agent with potassium dichromate as an activating agent. The influences of mobile phase changes (i.e., pH, organic modifiers, electrolytes), oxygen, metal ions, and order of reagent addition on reaction kinetics and product yield are defined and used in optimization of detector response. Detection at lambda/sub max/ 290 nm results in an on-line post-column sensitivity of 40-60 ng/mL for selected cis-dichloroplatinum complexes and a sensitivity of 300-1200 ng/mL for four (substituted)-malonato-platinum complexes. The reaction detector is used to monitor the kinetics of aquation of cisplatin (CDDP) and to quantitate CDDP degradation in plasma. As the sensitivity for CDDP in plasma is comparable to that achieved from high pressure liquid chromatography (HPLC) effluent ...

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The transfer function concept is well known as an additional method to evaluate the impulse test of power transformers in the test laboratory. Another application for the transfer function method is monitoring of transformers in service. Thereby, Off-line and On-line monitoring can be realized. Both kinds of monitoring are demonstrated with on-site measurements on a power transformer in service.

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This book deals with advanced computing applications in physics, and in particular in high energy physics environments. The main subjects covered are networking; vector and parallel processing; and embedded systems. Also examined are topics such as operating systems, future computer architectures and commercial computer products. The book presents solutions that are foreseen as coping, in the future, with computing problems in experimental and theoretical High Energy Physics. In the experimental environment the large amounts of data to be processed offer special problems on-line as well as off-line. For on-line data reduction, embedded special purpose computers, which are often used for trigger applications are applied. For off-line processing, parallel computers such as emulator farms and the cosmic cube may be employed. The analysis of these topics is therefore a main feature of this volume.

International Nuclear Information System (INIS)

This report discusses the work done on EPRI program S149-1. In this program the feasibility of cleaning steam generators off line with organic chelants as a means of arresting denting corrosion was investigated. The rationale behind this program is to make use of those periods during which nuclear steam generators are in cold shutdown or wet layup to carry out a low-temperature soak with a combined chelant-inhibitor solution in order to dissolve some of the magnetite which has built up in crevices and to concomitantly remove entrained corrodents such as chloride ion. It was hoped that these soaks would be effective in reducing carbon steel support plate corrosion which produces tube denting.

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A consortium has been formed to undertake the design and development work necessary to establish a comprehensive machine condition monitoring (MCM) and diagnostic system for hydroelectric generating units. By working closely with participating utilities and interested manufacturers, the consortium is initiating the integration of existing and developing technologies into a comprehensive, modular, on- and off-line hydroelectric MCM system.

UK PubMed Central (United Kingdom)

A technique for quantitative determination of cephalothin and desacetylcephalothin in serum using a method based on high-pressure liquid chromatography is described. Both compounds were quantitatively...Full Text Available

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This paper reported on a study in which partial discharge (PD) measurements were performed on 6 underground transmission cable circuits to determine the effectiveness of PD measurements on fluid fill cables. The cables were between 37 and 56 years old. PD activity was detected from the terminations of H11L and H3L Cable 2. However, for cables from H3L Basin TS to Mill Street junction, PD activity was detected originating from within the main cable insulation.

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Calibration system for spot welding robots has been developed. The purpose of this system is to reduce the misalignment of tool center point (TCP) generated when teaching data made by off-line system is input to an actual robot. After the factor of the misalignment was analyzed, the relation between a main factor and the misalignment was modeled. In addition, the model was verified on experiment. The achievement of the accuracy requirement and practical use in the site was confirmed by the result of the verification. (author)

British Library Electronic Table of Contents (United Kingdom)

Abstract Aims: The aim of this study was to examine whether metabolic syndrome (MS) is associated with periodontitis in a representative sample of Korean adults, who were involved in the Fourth Korea National Health and Nutrition Examination Survey (KNHANES). Materials and Methods: A total of 7178 subjects over the age of 19 years who participated in KNHANES were examined. MS was defined as the definition proposed by the National Cholesterol Education Program Adult Treatment Panel III and the abdominal obesity cut-off line based on Korean Society for the Study of Obesity. The periodontal status was assessed by the Community Periodontal Index. Multivariate logistic regression analysis was carried out adjusting for the sociodemographics, oral health behaviours and status, and health behaviou...

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A stable power system stabilizer (PSS) based on the inverse dynamics of the controlled system using an artificial neural network (ANN) is suggested to enhance the dynamic performances of a power system. First, an output feedback control law is driven with some conditions satisfied, which guarantees the internal stability and robustness against the asymptotically stable external disturbances. Then the control law is implemented using the inverse dynamics of the controlled plant. The inverse dynamics of the controlled plant is identified by an ANN, inverse dynamics neural network (IDNN), off-line. The pole-shifting technique and a scaling factor are introduced for the control system to meet the conditions for internal stability and robustness. The proposed controller is applied to a typical single-machine infinite-bus power system. Simulation results under various operation conditions are given which show that the proposed controller damps the low frequency ...

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A new recurrent neural network power system stabilizer (RNNPSS) based on genetic algorithm (GA) was presented. It shows faster convergence than the linear quadratic regulator (LQR) stabilizer in a multi-machine power system, because the proposed GA based neural network was first trained off-line to determine the optimal values of the learning rates. Otherwise, the RNNPSS consists of just two layers. As such, the time consumption of the damping oscillations is lower than with conventional methods. In addition, the operating range of the RNNPSS is greater than that of the LQR and conventional three layer neural networks, since the RNNPSS can greatly reduce system complexity and effectively damp system oscillations. 9 refs., 7 figs.

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Lithium isotope separation by displacement chromatography is studied using fundamental principles; the equations are derived assuming theoretical stages in lithium adsorption bands. The concentration profiles in the band are calculated numerically under unsteady state.

UK PubMed Central (United Kingdom)

A liquid chromatography/tandem mass spectrometric (LC/MS/MS) assay was developed for the quantitative determination of salirasib (S-trans, trans-farnesylthiosalicylic acid,...Full Text Available

UK PubMed Central (United Kingdom)

A pigment-dispersing hormone (PDH) from eyestalks of the fiddler crab Uca pugilator has been purified by gel filtration, ion-exchange chromatography, partition chromatography, and reversed-phase...Full Text Available

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Based on the IAPWS technical guidance on ''Instrumentation for Monitoring and Control of Cycle Chemistry for Steam-Water Circuits of Fossil-Fired and Combined Cycle Power Plants,'' the latest situation regarding instrumentation for nuclear power plants is discussed. As a result of the discussion, it is concluded that: (1) Reliable and safe operation of plants is established by the application of suitable chemical conditions in plant cooling systems, which should be supported by the selection of suitable control targets for monitoring and by the application of reliable instruments. (2) The minimum level of key instrumentation consists of on-line as well as off-line instruments for monitoring the key parameters: - on-line: pH, conductivity, cation conductivity, O{sub 2} and H{sub 2} concentrations, electrochemical corrosion potential; - off-line: radioactive nuclides ({sup 60}Co, {sup 58}Co, {sup 131}I, etc.), ...

Science.gov (United States)

We recently found that many RNA polymerase II transcription factors are modified with N-acetylglucosamine residues. These sugar moieties confer upon transcription factors an ability to bind the lectin wheat germ agglutinin. We have taken advantage of this interaction to devise a purification procedure for the "GC-box" binding transcription factor Sp1. Crude nuclear extracts are first subjected to wheat germ agglutinin affinity chromatography and then subjected to sequence-specific DNA affinity chromatography. The Sp1 protein purified by this procedure is at least 95% pure, and the overall recovery is greater than 80%. In addition to yielding larger quantities of Sp1 than conventional schemes, the new purification procedure is also simpler and more rapid. We show that wheat germ agglutinin affinity chromatography can also be used to purify the glycosylated forms of the CCAAT-binding transcription factor. Thus, wheat germ ...

International Nuclear Information System (INIS)

Combustion noise, knock and ignition limits data are measured and presented for a dual fuel engine running on dual fuels of Diesel and three gaseous fuels separately. The gaseous fuels used are liquefied petroleum gas, pure methane and compressed natural gas mixture. The maximum pressure rise rate during combustion is presented as a measure of combustion noise, and the knocking and ignition limits are presented as torque output at the onset of knocking and ignition failure. Experimental investigation on the dual fuel engine revealed the noise generated from combustion, knocking and ignition limits for all gases at different design and operating conditions. A Ricardo E6 Diesel version engine is converted to run on dual fuel of Diesel and the tested gaseous fuel and is used throughout the work. The engine is fully computerized, and the cylinder pressure data, crank angle data and engine operating variables are stored in a PC for off line ...

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This project evaluated the feasibility of using a low-concentration (approx. 0.5 wt %) chemical cleaning process to remove corrosion product deposits from steam generator surfaces and magnetite from tube-to-support plate crevices of PWR steam generators. The primary objective was to develop a dilute process that could be safely applied at scheduled intervals, such as during normal refueling outages, to maintain a clean operating condition in the steam generator. The dilute chemical cleaning process developed in this project was demonstrated successfully on two model generators which were operated on faulted chemistry by DOE/CRC at Commonwealth's State Line Facility. Unit 5 was cleaned after 48 days of operation with 1% seawater fouling, and Unit 6 was cleaned after 112 days of operations with Lake Michigan water. This report describes work leading to the model generator cleaning demonstrations and provides details of the cleaning operation for each model steam generator.

International Nuclear Information System (INIS)

In the present investigation the performance of digital data acquisition (DA) and analogue data acquisition (AA) systems are compared in neutron-induced fission experiments. The DA results are practically identical to the AA results in terms of angular-, energy- and mass-resolution, and both compare very well with literature data. However, major advantages were found with the digital techniques. DA allows for a very efficient #alpha#-particle pile-up correction. This is important when considering the accurate measurement of fission-fragment characteristics of highly #alpha#-active actinide isotopes relevant for the safe operation of Generation IV reactors and the successful reduction of long-lived radioactive nuclear waste. In case of a strong #alpha#-emitter, when applying the #alpha#-particle pile-up correction, the peak-to-valley ratio of the energy distribution was significantly improved. In addition, DA offers a very flexible expanded off-line analysis and ...

International Nuclear Information System (INIS)

This paper presents the analytical results of alcohols, esters and organic acids in sweet potato wine irradiated by #gamma#-rays. (author).

UK PubMed Central (United Kingdom)

The use of stable indole-3yl-acetic acid (IAA) labeled by 6 atoms of ¹³C allowed, after [¹³C]IAA treatment, simultaneous gas chromatography-mass spectrometry quantifications of...Full Text Available

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In this report, the quantitative relation between the height equivalent to a theoretical plate (HETP) and the size of ion exchange resin is studied by enriching lithium isotopes with high pressure ion exchange displacement chromatography. The dependence of HETP on the size of the resin can be expressed as H = C x (anti r)sup( ) in which = 2.4 and it is found that Snyder's equation is suitable for such a system of isotope separation as may be explained by the simple displacement mechanism.

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A simple method is presented for the separation of lead-203 from copper-backed thallium cyclotron targets. The procedure involves cation-exchange chromatography in hydrochloric acid and hydrochloric acid-acetone mixtures. Further purification involves anion-exchange chromatography in nitric acid-hydrobromic acid mixtures. A cation-exchange column containing 3.0 g of resin can handle as much as 15 g of thallium and 160 mg of copper. An anion-exchange column containing 3.0 g of resin can separate lead from up to 200 mg of thallium and 10 mg of copper. Separations are extremely sharp and less than 0.1 ..mu..g of thallium and less than 0.1 ..mu..g of copper remain in the lead-203 fraction.

British Library Electronic Table of Contents (United Kingdom)

18a(H)-, 18b(H)-oleanane and lupane are angiosperm-derived biomarkers that are used as age indicators for the Late Cretaceous onwards when the first proliferation of angiosperms occurred. In addition, the 18a(H)-/18b(H)-oleanane ratio is employed as a thermal maturity parameter of crude oil. However, evidence has shown that accurate quantification of these compounds has been impeded by inadequate chromatographic separation by traditional one-dimensional gas chromatography. In this study, we present the separation of 18a(H)-, 18b(H)-oleanane and lupane with comprehensive two-dimensional gas chromatography (GCxGC). Furthermore, it was observed that 18b(H)-oleanane elutes earlier than 18a(H)-oleanane in second dimension (polarity) which we attribute to steric hindrance effects. Two GC conditi...

British Library Electronic Table of Contents (United Kingdom)

Purpose To study the chemical modifications induced upon irradiation of solid human insulin at radiosterilization doses and investigate the influence of the absorbed dose on radiolysis. Materials and Methods Volatile radiolytic products were monitored by gas chromatography coupled with mass spectrometry (GC-MS) and non-volatile products by two different high performance liquid chromatography (HPLC) methods: the formation of higher molecular weight proteins was assessed by size exclusion liquid chromatography whereas assays for related compounds and chemical potency tests were carried out using reverse-phase HPLC-UV. Conformational changes were investigated by measurements of circular dichroism. Results After gamma irradiation at 10?kGy, the recovery of insulin was 96.8%; higher molecular w...

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A method for product analysis that eliminates a problematic step in the radiometric sucrose-phosphate synthase assay is described. The method uses chromatography on a boronate-derivatized high-performance liquid chromatography column to separate the labeled product, (14C)sucrose phosphate, from unreacted uridine 5{prime}-diphosphate-(14C)glucose (UDP-Glc). Direct separation of these compounds eliminates the need for treatment of the reaction mixtures with alkaline phosphatase, thereby avoiding the problem of high background caused by contaminating phosphodiesterase activity in alkaline phosphatase preparations. The method presented in this paper can be applied to many UDP-Glc requiring enzymes; here the authors show its use for determining the activities of sucrose-phosphate synthase, sucrose synthase, and uridine diphosphate-glucose pyrophosphorylase in plant extracts.

UK PubMed Central (United Kingdom)

Fatty acid biomarker analysis coupled with gas chromatography-isotope ratio mass spectrometry was used to confirm the presence of methanotrophic and thiotrophic bacterial endosymbionts in the tissues...Full Text Available

UK PubMed Central (United Kingdom)

BackgroundLiquid chromatography-mass spectrometry (LC-MS) is one of the major techniques for the quantification of metabolites in complex biological samples. Peak modeling is one...Full Text Available

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The concentration of some organic acids in the atmosphere was determined using a wet effluent diffusion denuder-aerosol collector coupled with Ion Chromatography. Three organic acids and four inorganic anions were identified and quantified in the air sample, taken from the backyard of PSI. (author)

UK PubMed Central (United Kingdom)

Mycobacterium tuberculosis is the etiologic agent of tuberculosis and can be accurately detected by laboratories using commercial genetic tests. Nontuberculosis mycobacteria (NTM) causing other mycobacterioses...Full Text Available

UK PubMed Central (United Kingdom)

A Legionella-like organism (strain 1087-AZ-H) was isolated from a pleural-fluid specimen from a renal transplant patient undergoing immunosuppressive therapy. Growth characteristics and gas-liquid chromatography...Full Text Available

UK PubMed Central (United Kingdom)

Basal segments taken from Old Home and Bartlett pear hardwood cuttings collected at intervals during the rooting period in September were extracted with ethanol and fractionated by paper chromatography...Full Text Available

UK PubMed Central (United Kingdom)

In-vitro experiments using 203Pb were performed to identify lead-binding components in human haemoglobin. Sephadex A-50 ion-exchange chromatography of haemolysate showed that different types of haemoglobin...Full Text Available

UK PubMed Central (United Kingdom)

Human Factor VIII/von Willebrand factor, purified by calcium citrate-cellulose chromatography and 4% agarose gel filtration was subjected to sodium dodecyl sulfate gel electrophoresis on gels containing...Full Text Available

UK PubMed Central (United Kingdom)

Shoot meristem tissues of alfalfa, Medicago sativa L., were found by high performance liquid chromatography analyses to contain the uncommon polyamines, norspermidine and norspermine....Full Text Available

Energy Technology Data Exchange (ETDEWEB)

Polynuclear aromatic sulphur heterocycles (PASHs) were isolated from a coal extract by two-step separation method using silica gel column chromatography and ligand exchanges thin layer chromatography (PdCl{sub 2}/SiO{sub 2}). The subfraction was examined by capillary column gas chromatography with flame ionization detector and flame photometric detector and gas chromatography - mass spectrometry. Identification was accomplished by comparison of chromatographic retention indices and mass spectra of compounds with those reported in the literature. It was found that the principal structures of the sulphur-containing fraction of Guiding coal extract have 3-4 aromatic rings. Dibenzothiophene, C{sub 1} - C{sub 3} alkylated dibenzothiophenes, benzonaphthothiophene and its alkylated derivatives were the main compounds. Only a few other polynuclear sulfur heterocycles were detected. No benzothiophene and its ...

Science.gov (United States)

The report gives results of an examination, including mutagenic screening, of the chemical composition of residual fuel oils and their column chromatography pre-fractions. A degree of correlation between composition and mutagenicity has been achieved. Radionuclide data has been o...

UK PubMed Central (United Kingdom)

Amino acids labelled with dimethylaminoazobenzenesulphonyl chloride can be separated by reversed-phase high-pressure liquid chromatography and detected in the visible region (436 nm). All 19 naturally...Full Text Available

British Library Electronic Table of Contents (United Kingdom)

Purpose Study the radiolysis of solid-state metoclopramide hydrochloride at various absorbed doses. Elucidate the structure of the degradation products to gain information on the radiolysis mechanisms. Methods Solid-state metoclopramide samples were irradiated at several doses with gamma rays and high-energy electrons to evaluate the influence of the dose rate. High-performance liquid chromatography with a diode array detector was used to measure the chemical potency as a function of the absorbed dose and to quantify the degradation products. The characterization of degradation products was performed by liquid chromatography/atmospheric pressure chemical ionization/tandem mass spectrometry. Results The degradation of solid-state metoclopramide after irradiation was negligible. No qualitati...

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The high spin fraction (HSF) of {sup 131}Te as a function of fragment emission angle has been determined in the 40 MeV alpha-particle induced fission of {sup 238}U using off-line gamma ray spectrometric technique. From the HSF the fragment average spin (J{sub av}) of fission product has been deduced using statistical model analysis. The J{sub av} value of {sup 131}Te is seen to remain nearly constant (10{Dirac_h}) from 90 deg. to 20 deg. On the other hand, the J{sub av} value of {sup 132}I from earlier work shows a drastic decrease (33%) from 11.4{Dirac_h} at 90 deg. to 7.6{Dirac_h} at 20 deg. . However, the yield weighted J{sub av} value of both the products show a decrease of 13%, which in close agreement with the value of 5-10% change from 90 deg. to 0 deg. in the results obtained from gamma ray multiplicity measurements. Thus the drastic difference in the change of fragment average spin (J{sub av}) of individual product from 90 deg. to 20 deg. obtained from the ...

Science.gov (United States)

The precedence effect (PE) is thought to be beneficial for proper localization and perception of sounds. The majority of recent physiological studies focus on the neural discharges correlated with PE in the inferior colliculus (IC). Pentobarbital anesthesia is widely used in physiological studies. However, little is known of the effect of pentobarbital on the discharge of neurons in PE. Neuronal responses in the IC from 23 male SD rats were recorded by standard extracellular recording techniques following presentation of 4 ms white noise bursts, presented from either or both of two loud speakers, at different interstimulus delays (ISDs). The neural responses were recorded for off-line analysis before or after intraperitoneal administration of pentobarbital at a loading or maintenance dose. Data were assessed by one-way repeated measures analysis of variance and pairwise comparisons. When the ipsilateral stimuli were leading, pentobarbital at a loading dose ...

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In steel production lines such as pickling lines, cold rolling mills and coil processing lines, the needs for on-line continuous measurement of surface quality and property of products and on-line inspection of surface defects have become strong. This is because user requirements for the surface quality of various products have become severer than before and besides, expectations are running high on the side of manufacturers for higher speeds of production lines and higher quality by the adoption of automatic inspection. As for the measurement of surface quality, continuous measurements along the full length of a steel strip are required in order to overcome problems derived from off-line, batch measurements that cannot satisfy user's demands for quality assurance. As for surface defects detection, various kinds of methods have been practically applied to production lines. However, it is the matter of fact that performances of these methods are not ...

International Nuclear Information System (INIS)

There is now an acute need to optimize maintenance to improve both reliability and competitiveness of nuclear power plant operation. There is an increasing tendency to move from the preventive (time based) maintenance concept to one dependent on plant and component conditions. In this context, various on-line and off-line condition monitoring and diagnostics, nondestructive inspection techniques and surveillance are used. Component selection for condition based maintenance, parameter selection for monitoring condition, evaluation of condition monitoring results are issues influencing the effectiveness of condition based maintenance. All these selections of components and parameters to be monitored, monitoring and diagnostics techniques to be used, acceptance criteria and trending for condition evaluation, and the economic aspect of predictive maintenance and condition monitoring should be incorporated into an integrated, effective condition based maintenance ...

Science.gov (United States)

This report describes the first phase of the AFS/DOE program on mathematical modeling of cupola behavior, covering the period May 19, 1989 to July 19, 1990. The objective of the program is to develop a comprehensive mathematical model of the cupola furnace for on-line and off-line process control and optimization. The work is being carried out by five organizations: Massachusetts Institute of Technology with responsibility for heat transfer and fluid flow modeling, and incorporation of the chemical models being developed by the University of Michigan team. Modern Equipment Company has the responsibility of compiling information on needed sensors for monitoring operation and providing materials data to be used for cupola input. General Motors, Central Foundry Division, is investigating the potential to augment the mathematical models with artificial intelligence programs. Lastly, General Motors Research laboratories are charged with providing accurate cupola ...

International Nuclear Information System (INIS)

Experimental excitation functions for deuteron-induced reactions up to 20 MeV on high purity natural hafnium were measured with the activation method using a stacked foil irradiation technique. Metallic hafnium foils with thickness of 10 #mu#m were stacked together with 50 #mu#m thick aluminium and 12 #mu#m thick titanium foils. The aluminium foils served as energy absorber while the titanium foils were used to monitor the energy and intensity of the bombarding deuteron beam. From a detailed remeasurement of the complete excitation function of the "n"a"tTi(d,x)"4"8V monitor reaction it was possible to adopt the proper incident energy and beam intensity by comparing the results with the recommended values. High resolution off-line gamma-ray spectrometry was applied to assess the activity of each foil. From the measured activity independent and/or cumulative elemental or isotopic cross section data for production of Ta, Hf and Lu radioisotopes by (d,x) reactions were ...

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The determination of the banned anabolic substance zeranol and the metabolites taleranol and zearalanone in bovine urine is complicated by the occurrence of the structurally-related mycotoxin zearalenone and the corresponding {alpha}- and {beta}-zearalenol metabolites which possess similar estrogenic properties. A liquid chromatography-negative ion electrospray tandem mass spectrometric method is presented for the confirmatory analysis of all six resorcylic acid lactones ('zeranols') in urine samples using deuterium-labelled internal standards. The method was validated as a confirmatory method for bovine urine samples according to new draft EU guidelines and showed good precision and linearity, and CC{alpha} and CC{beta} values of 0.02-0.30 and <1.0 ng ml{sup -1}, respectively. The applicability was demonstrated by comparing the results of an incurred sample with previous results on the same sample obtained by gas ...

Science.gov (United States)

Methods for the synthesis and quantitation of the novel choline analogues, telluronium choline and acetyltelluronium choline, are described. An assay procedure utilizing pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) with cold trapping was developed with [2H4]telluronium choline and [2H4]acetyltelluronium choline as internal standards. The telluronium compounds were ion-pair extracted from tissue with dipicrylamine, washed with 2-butanone, and pyrolyzed prior to GC-MS analysis. The compounds were monitored using selected ion monitoring at m/z 232 and m/z 190 for acetyltelluronium and telluronium choline, respectively, and at m/z 236 and m/z 194 for the analogous deuterated internal standards. The assay was linear over a range of 20 pmol-20 nmol of compound taken through the assay. PMID:8130881

British Library Electronic Table of Contents (United Kingdom)

A simple, sensitive and rapid method for analysis of granisetron in human plasma, utilizing liquid chromatography tandem mass spectrometry (LC-MS/MS), has been developed and validated to satisfy FDA guidelines for bioanalytical methods. The analyte and internal standard (IS) were isolated from 100ml plasma samples by liquid-liquid extraction (LLE). A Varian 1200l tandem mass spectrometer equipped with an electrospray ionization source was operated in selected reaction monitoring (SRM) mode with the precursor-to-product ion transitions m/z 313.4/138 for granisetron and m/z 270/201 for the IS used for quantitation. The assay exhibited a linear dynamic range of 0.02-20ng/ml for granisetron in human plasma. The lower limit of quantification (LLOQ) was 0.02ng/ml with a relative standard deviati...

British Library Electronic Table of Contents (United Kingdom)

The effect of sugar on plant metabolism, which is known to be similar to hormone-like signaling, was metabolomically studied using Melissa officinalis (lemon balm). The metabolite profiles of M. officinalis treated with sucrose were analyzed by gas chromatography-mass spectrometry (GC-MS) and principal component analysis (PCA). A total of 64 metabolites from various chemical classes including alcohols, amines, amino acids, fatty acids, inorganic acids, organic acids, phosphates, and sugars were identified by GC-MS. Three groups treated with different sucrose concentrations were clearly separated by PCA of their metabolite profiles, indicating changes in the levels of many metabolites depending on the sucrose concentration. Metabolite profiling revealed that treatment with a higher sucrose ...

Energy Technology Data Exchange (ETDEWEB)

Hybrid electric vehicles (HEV) need long-lived high-power batteries as energy storage devices. Batteries based on lithium-ion technology can meet the high-power goals but have been unable to meet HEV calendar-life requirements. As part of the US Department of Energy's Advanced Technology Development (ATD) Program, diagnostic studies are being conducted on 18650-type lithium-ion cells that were subjected to accelerated aging tests at temperatures ranging from 40 to 70 C. This article summarizes data obtained by gas chromatography, liquid chromatography, electron microscopy, X-ray spectroscopy and electrochemical techniques, and identifies cell components that are responsible for the observed impedance rise and power fade.

International Nuclear Information System (INIS)

Fractionation of isotopes of the alkali metals and the alkaline earth metals in ion exchange chromatography of their chlorides was studied. The heavier isotopes of potassium and rubidium were found to be preferentially fractionated into the ion exchanger phase while the lighter isotopes of lithium, magnesium, calcium and strontium were enriched in the exchanger phase. This can be interpreted as a resultant of the relative significance of isotope effect upon dehydration and isotope effect accompanying the phase change of the hydrated metal ion. Found was no evidence of anomalous isotope effect attributable to the odd-even difference in mass number of isotopes. Based on the spectroscopic and solution chemical data (experimental and theoretical), the isotopic reduced partition function ratios of the hydrated alkaline metal ions and stretching force constants of metal ion-hydrating water bonds were estimated. (author).

Energy Technology Data Exchange (ETDEWEB)

Conditions of the separation and detection of organic and inorganic anions by gradient ion chromatography and suppressed conductivity detection were studied, and the procedure of gradient elution was optimized. A detection limit of 1 x 10{sup -3} {mu}g x L{sup -1} was obtained using the pre-concentrated column and most relative standard deviations obtained in the determination of seven organic and inorganic anions were below 5%. This method was proved to be simple, rapid and accurate for the separation and determination of low-molecular-weight organic acids and inorganic anions and could be applied in the analysis of the samples from water and steam systems of thermal power plants with satisfactory results. (orig.)

British Library Electronic Table of Contents (United Kingdom)

Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines (TCs), sulfanilamides (SAs), and quinolones (QLs). The method consists of solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, using electrospray ionization (ESI) in positive mode. The SPE was performed with Oasis HLB and Oasi...

International Nuclear Information System (INIS)

The study reports the identification of different organic acids that are formed during the pyrohydrolysis of mixed carbide of uranium and plutonium using ion chromatography (IC). The identification of organic acids present in the pyrohydrolysis distillate is required to carry out interference free analysis of Cl and F. The study describes three stage isocratic separations with NaOH eluents having concentrations 2 mM, 10 mM and 50 mM respectively in order to separate and identify both aliphatic and aromatic acids. The present investigation identified formic, acetic, propionic, butyric, tartaric and oxalic acids in the distillate, however, aromatic acids could not be identified. (author)

British Library Electronic Table of Contents (United Kingdom)

This is a report of extraction and identification of 1-O-alkyl glycerol present in the dried leaves of Bauhinia scandens. Fifty percent aqueous ethanolic extract of the plant at room temperature was fractionated over petroleum ether and diethyl ether. The diethyl ether soluble fraction showed positive bioactivity in Brine Shrimp bioassay. Isolation and purification of the active principle was subsequently done from diethyl ether fraction. The diethyl ether fraction was separated into acidic and neutral part. The acid free fraction was screened to be positive in Brine Shrimp bioassay. The NMR spectra (in CDCl3) indicated the probability of its lipoidal nature. The total lipid fraction was resolved into neutral, glyco, and phospho-lipids by column chromatography. Only the neutral fraction sh...

Science.gov (United States)

The analysis of complex fluids such as crude oils, fuels, vegetable oils and mixed waste streams poses significant challenges arising primarily from the multiplicity of components, the different properties of the components (polarity, polarizability, etc.) and matrix properties. We have recently introduced an analytical strategy that simplifies many of these analyses, and provides the added potential of linking compositional information with physical property information. This aspect can be used to facilitate equation of state development for the complex fluids. In addition to chemical characterization, the approach provides the ability to calculate thermodynamic properties for such complex heterogeneous streams. The technique is based on the advanced distillation curve (ADC) metrology, which separates a complex fluid by distillation into fractions that are sampled, and for which thermodynamically consistent temperatures are measured at atmospheric pressure. The collected sample ...

UK PubMed Central (United Kingdom)

The polysaccharide components from cultured cells of Rhizobium fredii USDA205 and Rhizobium meliloti AK631 were extracted with hot phenol-water and separated by repetitive gel filtration chromatography....Full Text Available

UK PubMed Central (United Kingdom)

Gas chromatography-selected ion monitoring-mass spectral analysis using [¹³C₆]indole-3-acetic acid (IAA) as an internal standard provides an effective means for quantitation of...Full Text Available

Energy Technology Data Exchange (ETDEWEB)

A method is provided for detecting pathological macromolecules in a patient. The method is comprised of the following: obtaining body fluid from the patient; pretreating the body fluid; subjecting the pretreated body fluid to size-exclusion chromatography to create an excluded fluid; and analyzing the excluded fluid to detect macromolecules having a predetermined molecular weight. The method also allows for comparing elution spectra with reference spectra of suspect pathologic proteins.

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Dianionic tridentate, O, N, S, Schiff bases derived from salicylaldehyde and 2-mercapto-amines react with Tc(V) gluconate to form radiochemically pure neutral Tc chelates. The existence of lipophilic Tc complexes could be proved by high voltage electrophoresis, thin layer chromatography and octanol/water partition coefficients. 11 refs.

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From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} ...

International Nuclear Information System (INIS)

Carbaryl is one of the insecticides used in large quantities in Indonesia. It is effective against soybean and peanut plant insects. The residues in the plants are determined by Colorimetry at the residues level up to 5 ppm and by thin layer chromatography at level up to 0,1 ppm. Both methods use coupling reaction between hydrolysis product of Carbaryl and diazo reagent to produce colour. (author).

International Nuclear Information System (INIS)

The complex formation of astatine(I) cation with diethylene triamine pentaacetic acid (DTPA) and characterization of the complexes were investigated by electromigration in free electrolytes and by gel-chromatography on Sephadex G 25. The conjugation procedure for the production of At-DTPA conjugated polyclonal antibodies is described. (author) 15 refs.; 2 figs.

Science.gov (United States)

Plerocercoids of the tapeworm Spirometra mansonoides produce a substance that stimulates growth of experimental hosts. We report purification of plerocercoid growth factor (PGF) to homogeneity by a process involving isolation and solubilization of plerocercoid membranes, isoelectric point selection by chromatofocusing chromatography or preparative isoelectric focusing, and anion-exchange chromatography. A radioreceptor assay (RRA) for human growth hormone (hGH) was used to detect PGF and purity of the 27.5-kDa protein was judged by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). Proteolytic activity was detected in the 27.5-kDa protein by gelatin substrate PAGE. Characterization of PGF as a neutral cysteine proteinase was based on substrate and inhibitor specificities and dependence on pH and thiol-containing reagents. The association of hGH agonist and proteinase activities was shown by comparing RRA and hydrolytic ...

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The retention indices of cycloalkenes and cycloalkadienes with C/sub 6/-C/sub 13/ rings are determined by gas-liquid chromatography (GLC) on glass capillary columns coated with OV-1 and Ucon LB 550X and by gas-solid chromatrography (GSC) on a microcolumn packed with uncoated graphitized thermal carbon black (GTCB). Structure-retention correlations are derived on using index differences such as H/sup OV/, H/sup GTCB/ and ..delta..I values, considering the differences in the stereochemistry of these compounds. It is shown that the combined application of index increments obtained in GLC and GSC provides more detaled structure informations. The value of the retention index units agree with the most stable conformations of the alicyclic compounds. The high value for the energy equivalent to an index unit (..delta..G/sub I.U./ = 4.18 kJ/mol) confirms that graphitized thermal carbon black causes much stronger dispersive interactions than any nonpolar liquid phase.

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Headspace solid-phase microextraction (HS-SPME) coupled to comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GCxGC-TOFMS) was applied for equilibrium headspace analysis of Malaysian soursop (Annona muricata) volatile flavor compounds. A two-level fractional factorial design (25-1) was used to determine the effect of SPME variables, namely, SPME fibers, adsorption temperature, extraction time, amount of salt, sample amount and sample concentration on the extraction efficiency of volatile flavor compounds. A total of 37 volatile compounds were identified, comprising 21 esters, 6 alcohols, 3 terpenes, 2 acids, 2 ketones, 2 aldehydes and an aromatic with different hydrophobicities (log P) ranging between -0.14 and 4.83. Extraction using 10g of diluted (5% w/w) ...

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The radiochemical purity of the cobalt-57 complex of bleomycin could be enhanced by adjusting the pH of the final product to a value between 5 and 6. This radiopharmaceutical appeared to have better tumor visualizing properties compared to the not neutralized preparation. The clinical use of the cobalt-57 bleomycin complex is however limited by the long physical half-life of the label, causing a risk of radioactive contamination. It appeared to be possible to label bleomycin with radioactive cations ("1"1"1In"3"+, sup(99m)Tc"4"+, "1"9"7Hg"2"+ and "6"7Cu"2"+) having suitable gamma ray energies and short half-lifes. These bleomycin complexes showed a high radiochemical purity judged by their behaviour on thin layer chromatography, paper chromatography, and electrophoresis, but their application as tumor visualizing radiopharmaceutical turned out to be disappointing compared with cobalt-57 bleomycin. (orig.).

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The further development of a Guideline (formerly Protocol) for sampling and analysis of 'tars' from biomass producer gases is reported. This Guideline is being developed as a project within the European Fifth Framework Programme with additional partners from Switzerland and North-America. In this paper an outline and the principle of the Guideline are given. The Guideline is based on isokinetic sampling of particles and 'tar' from the main producer gas duct, particle filtration at high temperature, gas cooling in a liquid quench, 'tar' absorption in a solvent at low temperatures, an optional backup adsorber, and flow measurement and control. The Guideline gives a definition for 'Gravimetric tar' which is the 'tar' number to be determined by the Guideline. Also, the Guideline gives procedures for compound analysis by gas chromatography - mass spectrometry (GC-MS) or gas ...

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Forty synthetic food colors were determined in drinks and candies by reversed-phase high-performance liquid chromatography with photodiode array detection. The following food colors were analyzed within 19min using a short analytical column (50mmx4.6mm i.d., 1.8mm) at 50degreeC with gradient elution: Ponceau 6R, Tartrazine, Fast yellow AB, Amaranth, Indigotine, Naphthol yellow S, Chrysoine, Ponceau 4R, Sunset yellow FCF, Red 10B, Orange G, Acid violet 7, Brilliant black PN, Allura red AC, Yellow 2G, Red 2G, Uranine, Fast red E, Green S, Ponceau 2R, Azorubine, Orange I, Quinoline yellow, Martius yellow, Ponceau SX, Ponceau 3R, Fast green FCF, Eosine, Brilliant blue FCF, Orange II, Orange RN, Acid blue 1, Erythrosine, Amido black 10B, Acid red 52, Patent blue V, Acid green 9, Phloxine B, Ben...

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A comprehensive and highly selective method for detecting in bacterial supernatants a modified sulfur nucleoside, S-adenosyl-L-methionine (SAM), and its metabolites, i.e., S-adenosylhomocysteine (SAH), adenosine (Ado), 5prime-deoxy-5prime-methylthioadenosine (MTA), adenine (Ade), S-adenosyl-methioninamine (dcSAM), homocysteine (Hcy) and methionine (Met), was developed. The method is based on reversed-phase liquid chromatography with positive electrospray ionization (ESI+) coupled to a hybrid linear quadrupole ion trap (LTQ) and 7-T Fourier transform ion cyclotron resonance mass spectrometry (FTICRMS). A gradient elution was employed with a binary solvent of 0.05 M ammonium formate at pH 4 and acetonitrile. The assay involves a simultaneous cleanup of cell-free bacterial broths by solid-pha...

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The authors discuss radioimmunoassays (RIAs) for eicosanoids widely used in the field of experimental, clinical and pharmacological research. The main drawback of RIAs is the possibility of low specificity. This was clearly demonstrated during the controversy on plasma levels of 6-keto-PGF_1 #alpha#, the stable hydrolysis product of PGI_2. When extensive purification including reverse phase high pressure liquid chromatography (rp-HPLC) was performed prior to the RIA for 6-keto-PGF_1 #alpha# the levels were at least one order of magnitude less than previously claimed, and did not support the so-called circulating hormone hypothesis.

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Separation of lithium isotope by NTOE compound was carried out with 0.01M HCl solution. The ion exchange capacity of NTOE was 0.8 meq/g. The separation factor, #alpha#=("7Li/"6Li)_s_o_l_i_d/("7Li/"6Li)_l_i_q_u_i_d was 1.0242 by the elution chromatography. The lighter isotope, "6Li was concentrated in the liquid phase, while the heavior isotope, "7Li was enriched in the solid phase. (author).

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A simple highly efficient procedure has been developed for recovery of thallium radioisotopes from lead and bismuth targets irradiated by 1-GeV protons. The procedure is based on the use of extraction chromatography. The cross-sections have been determined for formation of "2"0"0Pb, "2"0"1Pb, "2"0"2"mPb, and "2"0"3Pb radioisotopes in targets from lead with natural isotopic composition, irradiated by 1-GeV protons.

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The variations of measurements were estimated for microamounts SO_4"2"-, Br"-, I"- ions in samples of carnallite by ionchromatography method. The composition of carbonate eluent was verified. The investigated minima were about 0,004 %, 0,001 %, 0,01 % for SO_4"2"-, Br"-, I"- completively correspondingly. It was shown that the limit of ion-chromatography measurement would be decreased when Br"- and I"- ions were concentrated by extraction before. Besides the determination of I"- ion in carnallite was preformed by potentiometry with I"--ionselective electrode. 6 refs.; 3 tabs.

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The aim of this study was to investigate the photodegradation of the antiemetic drug metoclopramide. Metoclopramide aqueous solutions were photoirradiated at 254nm under argon atmosphere. Irradiated metoclopramide solutions were analyzed by high performance liquid chromatography-ion trap mass spectrometry in order to characterize photolysis products. Rapid decrease in metoclopramide purity, following first-order kinetic, was observed following irradiation. The structures of 18 photolysis products were tentatively identified based on their mass spectra and fragmentation. The main degradation mechanism was scission of the chlorine which could be followed by polymerization of the resulting products since dimeric and trimeric products were observed.

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Dimethyl methylphosphonate (DMMP), a chemical simulant of the nerve gas GB, was decontaminated with a nonthermal atmospheric pressure plasma. The decontamination efficiency was measured qualitatively by means of Fourier transform spectroscopy and quantitatively by means of gas chromatography. With helium gas only, 10g/m2 of DMMP on an aluminum surface was 99.9% decontaminated in 2min, furthermore, with the addition of 5% of oxygen gas, it was 99.99% decontaminated in 10min. Given the low input power (<100W) and temperature (<75degreeC), this plasma is eligible for nondestructive decontamination of almost all material surfaces.

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Separation of lithium isotopes was investigated by chemical ion exchange with a hydrous manganese(IV) oxide ion exchanger using an elution chromatography. The capacity of manganese(IV) oxide ion exchanger was 0.5 meq/g. The heavier lithium isotope was enriched in the solution phase, while the lighter isotope was enriched in the ion exchanger phase. The separation factor was determined according to the method of Glueckauf from the elution curve and isotopic assays. The separation factor of {sup 6}Li{sup +} -{sup 7}Li{sup +} isotope pair fractionation was 1.018.

Science.gov (United States)

The adsorption properties of four samples of ..cap alpha..-BN were studied by means of gas chromatography. The particles of ..cap alpha..-BN particles, according to data obtained by electron microscopy, have the shape of thin platelets. A sample of ..cap alpha..-BN prepared from magnesium polyboride was found to be the most nearly homogeneous adsorbent. For a number of n-alkanes, benzene, and alkylbenzenes, data have been obtained on the retention volumes (Henry constants) and the differential heats of adsorption for surface coverages approaching zero. These thermodynamic data on the adsorption showed that ..cap alpha..-BN, like graphitized thermal carbon black, is a nonspecific adsorbent.

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A useful method for preparing radioiodinated photoaffinity labels from alkyl anilines which offer significant advantages over present methods is described. The one-pot synthesis gives good radiochemical yields (40-64%) of pure, high specific activity (350-1500 mCi/{mu}mol) {sup 124}I labelled iodaryl azides while minimising manipulation of radioactive materials. Purification of the ({sup 125}I)iodoazido photoaffinity labels is achieved by high performance liquid chromatography. (author).

Science.gov (United States)

The thermostable Thermus aquaticus DNA polymerase (Taq Pol) has been the key factor in transforming the initial PCR method into one with huge impact in molecular biology and biotechnology. Therefore, the development of effective affinity adsorbents for the purification of Taq Pol, as well as other DNA polymerases, attracts the attention of the enzyme manufacturers and the research laboratories. In this report we describe a simple protocol for the purification of Taq Pol from E. coli lysates, leading to enzymes of high specific activity and purity. The protocol is based on a single affinity chromatography step, featuring an immobilized ligand selected from a structure-biased combinatorial library of dNTP-mimetic synthetic ligands. The ligand library was screened for its ability to bind and purify Taq Pol from E. coli lysates. One immobilized ligand (mABSGu) of the general formula X-Trz-Y, bearing 9-aminoethylguanine (AEGu) and aniline-2-sulfonic acid (mABS) linked ...

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Solid-phase extraction and gas chromatography with electron-capture detection has been used for sensitive, simple, and reliable analysis of carfentrazone-ethyl residues in water. Carfentrazone-ethyl was enriched by use of multiwalled carbon nanotubes (MWCNT), a new adsorptive material. Several conditions affecting recovery of the analyte, for example polarity and volume of eluents, pH of water samples, and sample volume, were studied. Recovery from fortified samples, linear range, and limit of detection were evaluated. The results showed that MWCNT are an efficient SPE adsorbent for preconcentration of carfentrazone-ethyl in water. Under the optimized SPE conditions, recovery of carfentrazone-ethyl from fortified water was 81.49?91.08%, with RSD from 1.66 to 8.21%. The limits of detection ...

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A water trap system based on a thermoelectric cooling device is employed to remove a major fraction of the water from air samples, prior to analysis of these samples for chemical composition, by a variety of analytical techniques where water vapor interferes with the measurement process. These analytical techniques include infrared spectroscopy, mass spectrometry, ion mobility spectrometry and gas chromatography. The thermoelectric system for trapping water present in air samples can substantially improve detection sensitivity in these analytical techniques when it is necessary to measure trace analytes with concentrations in the ppm (parts per million) or ppb (parts per billion) partial pressure range. The thermoelectric trap design is compact and amenable to use in a portable gas monitoring instrumentation.

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We have developed a method for the synthesis of C-11 iodoantipyrine. Carbon-11-labeled methyl iodide, prepared from /sup 11/CO2, was used to methylate 3-methyl-1-phenyl-2-pyrazolin-5-one to form C-11 antipyrine. Following silica-gel column chromatography and iodination, radiochemical purity of the C-11 iodoantipyrine was more than 99.5%, with a 10% yield and a specific activity of 30 mCi/mumol. Preliminary animal studies showed complete cerebral extraction and local cerebral blood-flow values that were within 4.6% of those obtained using C-14 iodoantipyrine. The C-11 analog, with positron emission tomography, will facilitate local cerebral blood-flow studies in human subjects.

International Nuclear Information System (INIS)

Homidium bromide and isometamidium chloride are used extensively in the treatment of bovine trypanosomiasis in Africa, but no specific and sensitive method to detect the drug in plasma has been published yet. Comparing the methods of other investigators it was found that they could not overcome the protein binding of these drugs which reduced the available and determined drug to 10% of the real concentrations. These techniques overcome the protein binding by enzyme digestion and an alteration of the pH before adding the sample directly on clean-up columns. Drug recover rates above 80% were obtained. For the detection, the HPLC was employed using a C18 reversed phase analytical column and UV detection, determining both drugs as intact molecules. (author).

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To address lithium-ion cell safety issues in demanding power applications, electrical and thermal abuse tests were performed on 18650 sized cells. Video and electrically monitored abuse tests in air included short circuit, forced overcharge, forced reversal, and controlled overheating (thermal) modes. Controlled overheating tests to 200 C were performed in a sealed chamber under a helium atmosphere and the gases released from the cell during thermal runaway were analyzed at regular intervals using gas chromatography and mass spectrometry. In addition to alkane and alkene solvent breakdown fragments, significant H{sub 2} was detected and evidence that HF was evolved was also found.

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Summary Isomalto-oligosaccharides (IMO) belong to a group of prebiotics that can significantly increase the number of protective gut microflora. A one-step method using neopullulanase (NPN) in conjunction with saccharifying -amylase (SAA) for the bioconversion of rice starch into IMO was investigated. Purified rice starch slurry (30% w/w) was mixed with NPN (3.5 U g-1 starch substrate) and SAA (6.5 U g-1 starch substrate) and the slurry was incubated at 57 C for 92-h under constant stirring. The carbohydrate composition of the resulting syrup was analysed by high performance liquid chromatography (HPLC) and the dextrose equivalent (DE) determined by titration. The amount of IMO in the syrup reached maximum (59.2%, dry basis) after 72-h of bioconversion. The concentration of glucose and mal...

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Polyethylene pipes and connections are being widely used in treated water distribution services. Migration of low molecular weight compounds from the polyethylene into the water can change its final quality. This paper is about the concentrations and identification of the migration compounds found in treated water after staying in contact with low and high-density polyethylene. Identification and quantification were carried out using CLSA (Closed Loop Stripping Analysis) extraction technique and gas chromatography coupled to mass spectrometry (HRGC/HRMS). (Author) 12 refs.

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After irradiation at 254nm of aqueous solutions of the antipsychotic drug flupentixol, the structures of the photodegradation products were determined by ultra high performance liquid-chromatography linked to mass spectrometry. Fragmentation patterns of the parent ions were established on a hybrid linear ion trap-orbitrap mass spectrometer allowing accurate mass measurements of both parent and daughter ions. This allowed to propose plausible structures for the main photolysis products of flupentixol. A total of nine photoproducts were detected after irradiation of the drug. The main photoproduct is generated following the addition of a hydroxyl group on the double bond adjacent to the thioxanthene ring. Secondary photoproducts were also observed.

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The exceptional ability of marine sponges to adapt to often drastic changes of their environments could be due to special structural features in cell membranes, including firstly phospholipids (PL). Thus, PL class composition was investigated in marine sponges (22 species from 19 genera to 15 families) originating from various locations (East Atlantic, North Atlantic, South-West Pacific, Mediterranean Sea, Red Sea, Arabian?Persian Gulf). The quantitative determination of PL class composition was obtained by high-performance thin-layer chromatography (HPTLC) with scanning densitometry of the different spots. Previous reports have shown phosphatidylethanolamine (PE) as the major PL class in marine sponges, followed by phosphatidylcholine (PC), while other papers described PC as a minor class...

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The thermodynamic characteristics of adsorption (TCA) on the basal face of graphite have been calculated in terms of the semiempirical molecular statistical theory of adsorption for molecules of O-, S-, and Se-containing heteroadamantanes of different structure and isostructural cyclohexane derivatives. The influence of the nature, number, and position of heteroatoms in the adamantane framework on the TCA values was studied in detail, which made it possible to predict the retention of the compounds considered on the surface of graphitized thermal carbon black under the conditions of equilibrium gas adsorption chromatography. The introduction of each subsequent heteroatom into a polyheteroadamantane molecule makes a non-additive contribution to the TCA values. The contributions of various f...

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Samples of vitamin D fortified orange juice obtained from retail food stores were analyzed for vitamin D3 content using a method developed by combining the best features of two AOAC methods. Detection by ultraviolet absorption at 265nm was compared to detection by selected ion monitoring (SIM) using atmospheric pressure chemical ionization (APCI) mass spectrometry (MS). Furthermore, an ion trap (IT) mass spectrometer was employed in a 'dual parallel MS' arrangement to simultaneously obtain qualitative APCI-ITMS data. The method was applied to 33 samples of 3 national American orange juice brands and 7 samples of 5 other American brands collected using a statistically designed sampling plan as part of the National Food and Nutrient Analysis Program to provide values for the USDA National Nu...

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Antibodies to hemoglobin have been studied with a radioimmunoassay which employs ["1"4C]carbamylated (= carbamoylated) hemoglobin S. An antiserum raised against hemoglobin S, which initially discriminated poorly between hemoglobins S and A, was fractionated by absorption to a column of Sepharose to which a synthetic peptide corresponding to the first 13 amino-acid residues of the #beta# chain of sickle hemoglobin had been covalently bound. A subpopulation of the antiserum was eluted from this column with 4 M guanidine . HCl. These antibodies showed binding to hemoglobin S but not to hemoglobin A and this interaction could be inhibited by the synthetic peptide. These antibodies, of demonstrated fine structural specificity, may be useful in the detection of sickle hemoglobin and in the study of its structure in solution.

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Summary The aroma impact volatiles of twenty-four pine honey samples produced in Marmaris, Data and Fethiye regions of Turkey were evaluated by solid phase micro extraction/gas chromatography/mass spectrometry (MS) technique and the results were evaluated by using the analysis of variance and Duncan tests. A total of eight common volatiles nonanal, nonanol, decanal, octanal, 16-oxosalutaridine, dodecanal, nonadecane and pentadecane were detected in three regions. The total area of the common volatiles were 73.01%, 78.10% and 73.91% in Marmaris, Data, and Fethiye regions, respectively. There were not significant differences (P-<-0.05) between the common volatiles detected in pine honey samples from three different regions. The major contributers to the pine honey aroma seems to be nonanal (...

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A qualitative method, involving supported liquid?liquid extraction (SLE) and ultra high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS?MS), was developed for the rapid tentative identification of various drugs of abuse in urine. In this study, 28 drugs and metabolites were covered by the screening procedure. Before analysis, urine samples were extracted by SLE and good extraction recoveries were obtained for most investigated compounds. The UHPLC strategy was then selected for the rapid separation of amphetamines, cocaine, opiates and related compounds in urine. Using columns packed with sub-2??m particles, analysis time was reduced down to 2?min, while maintaining acceptable performance. Finally, the detection was by tandem MS operating in the single reaction...

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Fragranced consumer products are pervasive in society. Relatively little is known about the composition of these products, due to lack of prior study, complexity of formulations, and limitations and protections on ingredient disclosure in the U.S. We investigated volatile organic compounds (VOCs) emitted from 25 common fragranced consumer products-laundry products, personal care products, cleaning supplies, and air fresheners-using headspace analysis with gas chromatography/mass spectrometry (GC/MS). Our analysis found 133 different VOCs emitted from the 25 products, with an average of 17 VOCs per product. Of these 133 VOCs, 24 are classified as toxic or hazardous under U.S. federal laws, and each product emitted at least one of these compounds. For ''green'' products, emissions of these c...

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The thermodynamic characteristics of adsorption (the Henry constant, the heat and entropy of adsorption) of amino acids associates with acetic, trifluoroacetic, nonafluoropentanoic acids and formamide with different values of hydrogen bond lengths and various conformations on a graphitized thermal carbon black (GTCB) were calculated. The experimental results, as the Henry constant, lnK1, and the differences in the molar Gibbs energies, d(DG), obtained by a high performance liquid chromatography (HPLC) on a carbon sorbent Hypercarb, were compared with the values of thermodynamic characteristics of adsorption of the amino acids on the GTCB surface calculated by a molecular-statistical method. A satisfactory correlation was observed between the experimental and calculated values with a coeffi...

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IntroductionThe elimination of microorganisms from the root canal system necessitates the use of combination of irrigating solutions to enhance their antimicrobial property. The combination of irrigants and their interaction sometimes could be detrimental to the outcome of the root canal therapy. The purposes of this study were (1) to evaluate the interaction between 7% maleic acid (MA) and 2% chlorhexidine gluconate solution (CHX) and to find out the availability of individual irrigant and (2) to determine the free available chlorine content when 7% MA was mixed with 2.5% sodium hypochlorite (NaOCl) solution. MethodsInteraction between MA and CHX was assessed by high-performance liquid chromatography. Available chlorine content in NaOCl was evaluated by the standard iodine/thiosulfate tit...

International Nuclear Information System (INIS)

Poly(lactic acid) (PLA) is attractive as a substitute for classical polymer packaging material due to its biodegradability and sufficient mechanical and barrier properties. Presented research was focused on the changes of basic mechanical parameters after ionizing irradiation performed with doses in the range of 2.5-25 kGy, commonly used in radiation sterilization and preservation of foods. Two commercial available PLA packaging films were tested. The influence of radiation dose on the mechanical properties - tensile strength and elongation were determined using standardized methods. Radiation resistance of PLA is sufficient for packaging applications. The investigations of gas products of radiolysis of PLA have been made by gas chromatography after electron beam (EB) irradiations. (authors)

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Breath analysis could offer a non-invasive means of intravenous drug monitoring if robust correlations between drug concentrations in breath and blood can be established. In this study, propofol blood and breath concentrations were determined in an animal model under varying physiological conditions. Propofol concentrations in breath were determined by means of two independently calibrated analytical methods: continuous, real-time proton transfer reaction mass spectrometry (PTR-MS) and discontinuous solid-phase micro-extraction coupled with gas chromatography mass spectrometry (SPME-GC-MS). Blood concentrations were determined by means of SPME-GC-MS. Effects of changes in pulmonary blood flow resulting in a decreased cardiac output (CO) and effects of dobutamine administration resulting in...

International Nuclear Information System (INIS)

A method is described for determination of aluminium, cadmium, cobalt, chromium, copper, calcium, magnesium, sodium, potassium, manganese, nickel, lead, strontium, zinc, titanium and vanadium in iron ore. After dissolution, a 1 gram sample of iron ore is applied to a column of AGI-X8 anion exchange resin (chloride form), in 100 ml of 7M HCl. Aluminium, chromium, calcium, magnesium, sodium, potassium, manganese, nickel, lead, strontium, titanium and vanadium are eluted with 7M HCl; iron, copper and cobalt are eluted with 0.5M HCl; cadmium and zinc are eluted with 2M HNO_3. Iron is subsequently removed from copper and cobalt by a solvent extraction with methyl isobutyl ketone. The elements are determined in the eluates by atomic absorption spectrometry, except for titanium and vanadium, which are determined spectrophotometrically.

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The reference method used to analyse polychlorodibenzo-p-dioxins (PCDDs), polychlorodibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (dl-PCBs) is chromatography with high resolution mass spectrometry (GC-HRMS). It is interesting to check the suitability of screening methods that are faster and less expensive. Different matrices (milk, fish oil, chicken compound feed, pork tissue, chicken tissue, sepiolitic clay, whole egg and herring tissue) were analysed in the frame of the European project DIFFERENCE1. One of the aims of this project is to optimise screening methods. The CALUX bio-assay was one of the screening techniques used. This paper presents the extraction and purification methods used for the analyses. The CALUX results for dioxins and for dl-PCBs were compared to the corresponding GC-HRMS results.

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Thirty bacterial isolates were obtained from different sources and sites at Jeddah, Saudi Arabia, on chitin agar medium; 9 of the 30 isolates were cultured in liquid medium containing chitin as sole carbon and nitrogen sources. Isolate SM21, which was isolated from shrimp shells, showed the best growth and chitinase production in liquid medium. According to its morphological, physiological and biochemical characteristics, SM21 belongs to the genus Streptomyces and was identified as Streptomyces anulatus SM21. Identification was confirmed using 16S rDNA analysis. The chitinase enzyme was precipitated with 80% NH4SO4 and purified using DEAE-cellulose ion exchange chromatography followed by Sephadex G-100 gel filtration. The molecular weight determined using sodium dodecyl sulfate polyacrylam...

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{gamma}-Butyrolactone-based electrolytes have been used as the operating electrolytes for aluminum electrolytic capacitors. The chemical stability of these electrolytes at elevated temperatures has been examined by monitoring the decrease in their electrolytic conductivities. The deteriorated electrolytes were analyzed by gas and liquid chromatography and the conductivity decrease was directly correlated with the loss of acid components. In quaternary ammonium hydrogen maleate/{gamma}-butyrolactone electrolytes, the maleate anion decomposed by decarboxylation resulting in a complex polymer containing polyester and polyacrylate structures. Quaternary ammonium benzoate/{gamma}-butyrolactone electrolytes decomposed by SN2 reactions giving alkyl benzoates and trialkylamines. The deterioration of the carboxylate salt/{gamma}-butyrolactone electrolytes was accelerated by electrolysis. (orig.)

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The kinetics of biosorption and desorption of lindane by live activated sludge and the fungus R. arrhizus was studies. The results from the use of live activated sludge suggest that besides biosorption, other lindane removal mechanisms acted in parallel. Most probably, biodegradation. A relationship between biodegradation and bisorption-desorption was established. Mass spectroscopy and gas chromatography studies suggested the presence of lindane biodegradation by products. Lindane accumulated by the live activated sludge could be desorbed while being biodegraded at the same time. Values for lindane biokinetic constants were estimated. Biosorption of lindane by live R. arrhizus is a rapid and reversible process with no indication of biodegradation. Values for the lindane biotransformation kinetic coefficients were estimated. (orig.).

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Abstract Jicama (Pachyrhizus erosus L.) is a root-based legume that has been cultivated in Mexico for centuries. Pectic polysaccharide from de-starched jicama pomace was extracted using an autoclave-assisted process and physicochemically characterized. The extracted polysaccharide (1.0 g L-1) was used for the formation of polyelectrolyte complexes (PECs) with water-soluble chitosan (WSCh; 0.5, 1.0 and 2.0 g L-1). The extraction yield of jicama pectic polysaccharide was 22.8 wt% (dry basis) and infrared spectroscopic analysis showed that it was methoxylated to a small degree. Thermogravimetric analysis indicated that this biopolymer was very stable, its weight loss being 51.2% after heating at 479 C. Anion-exchange chromatography showed it to have a wide and heterogeneous charge density. Th...

International Nuclear Information System (INIS)

Techniques of chemical analysis, amino acid sequencing and autoradiography are being used to study the frequency of incorporation of normally noncoded amino acids into hemoglobins and seminal fluid proteins. We are studying, by the sequencing of radiolabeled proteins followed by the recovery of ["3H] isoleucine phenylthiohydantoin by high-performance liquid chromatography, the frequency at which normally noncoded isoleucine is incorporated into hemoglobin because of base-substitution mutations versus translational errors. Irradiation increases the isoleucine content of human hemoglobin and the frequency of substitution of isoleucine for specific amino acids in rabbit hemoglobin. Studies to date indicate that these techniques have been developed sufficiently for initial analysis of the potential of drugs and environmental pollutants to induce base-substitution mutations in mammalian somatic cells.

International Nuclear Information System (INIS)

Anion-exchange chromatography of element 105, dubnium (Db), produced in the "2"4"8Cm("1"9F, 5n)"2"6"2Db reaction is investigated together with the homologues Nb and Ta, and the pseudo-homologue Pa in 13.9 M hydrofluoric acid (HF) solution. The distribution coefficient (K_d) of Db on an anion-exchange resin is successfully determined by running cycles of 1702 chromatographic column separations. The result clearly indicates that the adsorption of Db on the resin is significantly different from that of the homologues and that the adsorption of anionic fluoro complexes of these elements decreases in the sequence of Ta#approx#Nb>Db#>=#Pa. (orig.)

British Library Electronic Table of Contents (United Kingdom)

A recently developed hydrodistillation?solvent microextraction (HD?SME) method coupled to gas chromatography?mass spectrometry (GC?MS) was applied to the analysis of volatile components of aerial parts of Echinophora cinerea (Boiss). By the use of a simplex optimization method, the effects of extraction time, sample weight and microdrop volume on the extraction efficiency of the method were optimized. In the optimized conditions, 3??L of n-heptadecane was suspended in the headspace of 6?g of hydrodistillating sample, using a microsyringe. After 7?min, the solvent was retracted back into the syringe and directly injected into the GC?MS injection port. The HD?SME method was compared to a conventional hydrodistillation technique. In general, the extraction with HD?SME was relatively faster an...

Science.gov (United States)

The technology for flue gas desulfurization (FGD) with seawater is widely adopted by coal-fired power plants in coastal areas. SO2 in the flue gas is absorbed by alkaline seawater and transfered in aqueous phase as sulfite (SO3(2-)), and most SO3(2-) is transformed to sulfate (SO4(2-)) after an aeration process. The remaining SO3(2-) in the seawater discharged to sea area may be harmful to marine organism because of its biological toxicity, thus it is necessary to determine the concentration of SO3(2-) in the seawater for desulfurization. In this study, the method of determination of SO3(2-) in the seawater by ion chromatography was investigated. The separation was achieved on an IonPac AS14A column with 14 mmol/L NaOH-12 mmol/L Na2 CO3 solution as the mobile phase at a flow rate of 1.2 mL/min, and the detection was performed by a pulsed amperometric detector. Formaldehyde was added as a protective agent when sampling because the SO3(2-) is easy to be oxidized. To ...

International Nuclear Information System (INIS)

Analysis by gas chromatography-mass spectrometry and high performance liquid chromatography has revealed organic residues in sup(99m)Tc-pertechnetate obtained from "9"9Mo-molybdate by extraction, using the organic solvent methylethylketone (MEK). The organic residues have been identified as either (i) low molecular weight carbonyl compounds such as formaldehyde, acetaldehyde and acetone, presumably caused by the effects of #gamma#-radiation on MEK, or (ii) condensation products resulting from the action of strong alkali on MEK during the extraction process. The quantities of organic residues varied from batch to batch of extracted pertechnetate; up to 40 #mu# mL"-"1 was found. When these compounds were tested, in rats, by addition to a pyrophosphate bone-seeking radiopharmaceutical, the tissue distribution was not significantly different from that in the control, which contained no added compound. Assay for "9"9Tc in MEK-derived pertechnetate ...

International Nuclear Information System (INIS)

The sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy)_3 "2"+] electrogenerated chemiluminescence (ECL) sensor was applied to the reversed-phase high-performance liquid chromatography (HPLC) determination of phenothiazine derivatives (promazine, chlorpromazine, triflupromazine, thioridazine, and trifluoperazine) and erythromycin in human urine samples. In this method, Ru(bpy)_3 "2"+ was immobilized in sol-gel-derived titania (TiO_2)-Nafion nanocomposite films coated on a dual platinum electrode. This method eliminates an extra pump needed for the delivery of Ru(bpy)_3 "2"+ reagent into a reaction/observation zone in front of photomultiplier tube because the immobilized-Ru(bpy)_3 "2"+ is recycled on the electrode surface by an applied potential at +1.3 V versus Ag/AgCl (3 M NaCl) reference electrode. The resulting analytical performances such as detection limit, working range, sensitivity, and measurement precision were slightly worse than those obtained ...

Science.gov (United States)

A liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous determination of the 10 major components of Da-Cheng-Qi decoction (rhein, emodin, aloe-emodin, chrysophanol, rheochrysidin, naringin, naringenin, hesperidin, magnolol and honokiol) in dog plasma. Plasma samples were spiked with internal standard (ibuprofen), acidified with HCl and extracted twice by liquid-liquid extraction using ethyl acetate. Separation was performed on a YMC-Pack ODS-A C(18) column (5 microm, 150 mm x 4.6 mm) and a C(18) guard column (5 microm, 4.0 mm x 2.0 mm) with methanol-water (92:8, v/v) at a flow rate of 0.3 mL/min. The LC/MS system was operated under the multiple reaction monitoring mode using electrospray ionization in the negative ion mode. All analytes showed good linearity over a wide concentration range (r>0.99). The linear range of the calibration curves was 5000-19.53 ng/mL for rhein; 400-3.13 ng/mL for emodin; 800-3.13 ng/mL ...

Energy Technology Data Exchange (ETDEWEB)

A method for the introduction of N-(/sup 3/H)acetyl groups into glycosaminoglycans is described. The procedure is based on (/sup 3/H)acetylation of N-unsubstituted hexosamine residues by treating the polysaccharides with (/sup 3/H)acetic anhydride. Preparations of heparin and heparin sulfate were found to contain significant numbers of N-unsubstituted hexosamine residues, as isolates. In contrast, such units could not be detected in chondroitin sulfate, dermatan sulfate, or hyaluronic acid. These polysaccharides were therefore subjected to partial N-deacetylation by reaction with hydrazine in the presence of hydrazine sulfate. After treatment with (/sup 3/H)acetic anhydride, the specific activities of the resulting labeled polysaccharide preparations ranged between 0.1 X 10/sup 6/ and 0.6 X 10/sup 6/ cpm /sup 3/H/..mu..g of uronic acid. The /sup 3/H-labeled polysaccharide preparations did not differ significantly from the corresponding unlabeled starting materials with regard to ...

Energy Technology Data Exchange (ETDEWEB)

ZnMT has been postulated to function in essential metal homeostasis and metal detoxication. This study was undertaken to evaluate the potential of liver ZnMT to mediate the interaction of Zn and Pb with the Zn metalloenzyme, ALAD. Pretreatment of rats with Zn activated liver ALAD and attenuated the inhibition of ALAD by Pb in vitro and in vivo. Liver cytosol from Zn-pretreated rats injected with /sup 203/Pb was fractionated via gel filtration and anion-exchange chromatography and disclosed that both Zn and /sup 203/Pb co-eluted in the MT fractions. Both purified ZnMT-I and ZnMT-II bound /sup 203/Pb in vitro as shown by gel filtration chromatography. Addition of purified liver ZnMT to purified bovine liver ALAD reaction mixtures increased enzyme activity by 2-fold and prevented inhibition of ALAD by Pb. Addition of apothionein alone decreased the activity of Zn-activated ALAD and also attenuated Pb inhibition of the enzyme. Gel filtration ...

Science.gov (United States)

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)), 17?-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 ...

Science.gov (United States)

The principles of modern pesticide residue chemistry were articulated in the 1950s. Early authors pointed out the advantages of systematizing and standardizing analytical methods for pesticides so that they could be widely practiced and the results could be reproduced from one laboratory to the next. The availability of improved methods has led to a much more complete understanding of pesticide behavior and fate in foods and the environment. Using methods based largely upon gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled increasingly with mass spectrometry (MS) and MS(n) as the detection tool, residues can be measured at parts per billion levels and below in a variety of food and environmental matrices. Development of efficient extraction and cleanup methods, techniques such as ELISA, efficient sample preparation techniques such as QuEChERS, and automated laboratory and field instrumentation has also ...

Energy Technology Data Exchange (ETDEWEB)

We have recently introduced several important improvements in the measurement of distillation curves for complex fluids. The modifications include a composition-explicit data channel for each distillate fraction (for both qualitative and quantitative analysis) and corrosivity assessment of each distillate fraction. The composition-explicit information is achieved with a new sampling approach that allows precise qualitative as well as quantitative analyses of each fraction, on the fly. We have applied the new method to a variety of fluids, including simple n-alkanes, rocket propellant, gasoline, jet fuels, and a hydrocarbon fluid made corrosive with dissolved hydrogen sulfide. In the current contribution, we present the application of the advanced distillation curve method to two samples of crude oil. A primary motivation behind the work is to precisely measure the distillation curves of these oils using our advanced distillation apparatus; these low uncertainty measurements of true ...

Environmental Research Database

Objectives~%~ To quantify the volatile organic compound (VOC) emissions arising from the composting of a range of municipal and~%~ industrial wastes.~%~~%~ To relate the VOC emissions to the material being processed and the process conditions.~%~~%~ To confirm the findings of the above activites by monitoring full-scale composting operations.~%~~%~ To develop predictive models of VOC emissions in relation to waste feedstock and process conditions.~%~~%~ To produce guidance for plant designers, operators a [continued...]DescriptionA recent study of three composting plants undertaken for the Environment Agency has confirmed earlier work suggesting that waste composting can be a source of volatile organic compound (VOC) emissions. However, these experiments were restricted to garden and kitchen waste composting schemes and it was not possible to measure the effect that the process conditions had on the VOC emissions. ...

International Nuclear Information System (INIS)

The purpose of the present study was to examine the in vitro effects of low-dose cadmium (Cd) on developing cortical cells. The cortical cells removed from fetuses (embryonic day 15) were treated with 10 nM of Cd for 24 h. The effects of Cd on dendritic and synaptic development were immunocytochemically observed with anti-microtubule associated protein-2 (MAP2) and anti-synapsin I antibodies, respectively. Administration of Cd suppressed dendritic as well as synaptic development at 10 nM. By two-dimensional gel electrophoresis and liquid chromatography-tandem mass spectrometric (LC/MS/MS) analysis, we identified three proteins with different expression after Cd-treatment; dihydropyrimidinase-related protein 2 (DRP-2/CRMP-2), 14-3-3-epsillon and calmodulin (CaM). Though the number of identified proteins was small, these proteins are known to be involved in neuronal development. The present study demonstrated the morphological effects as well as affected proteins in ...

International Nuclear Information System (INIS)

The transfer kinetics of the negatively charged glycosphingolipid II"3-N-acetylneuraminosyl-gangliotetraosylceramide (GM_1) were investigated by monitoring tritiated GM_1 movement between donor and acceptor vesicles. After appropriate incubation times at 45 "0C, donor and acceptor vesicles were separated by molecular sieve chromatography. Donors were small unilamellar vesicles produced by sonication, whereas acceptors were large unilamellar vesicles produced by either fusion or ethanol injection. Initial GM_1 transfer to acceptors followed first-order kinetics with a half-time of about 40 h assuming that GM_1 is present in equal mole fractions in the exterior and interior surfaces of the donor vesicle bilayer and that no glycolipid flip-flop occurs. GM_1 net transfer was calculated relative to that of ["1"4C]cholesteryl oleate, which served as a nontransferable marker in the donor vesicles. Factors affecting the GM_1 interbilayer transfer rate included phospholipid ...

International Nuclear Information System (INIS)

Cisplatin (cis-diaminedichloroplatinum [II] is a coordination compound, used in the treatment of several solid tumors. Cisplatin and its hydrolysis products exhibit a great pharmacological effect but are very toxic and probably carcinogenic. The present review summarizes the most important advances in the last years in the techniques employed for the detection and quantification of cisplatin and its hydrolysis products and in the different matrixes studied. The new emerging techniques and their modifications recently developed, fundamentally the combined use of detection and separation techniques for the analysis of platinum species and their impact on the speed, sensitivity and specificity of the analytical determination, with regard to the techniques used in the last century are discussed. High-Performance Liquid Chromatography and Capillary Electrophoresis, coupled with detection methods such as Mass Spectrometry, Inductively Coupled Plasma-Mass Spectrometry, ...

Energy Technology Data Exchange (ETDEWEB)

By improving the currently used lactoperoxidase method, we were able to obtain radioiodinated chicken luteinizing hormone (LH) that shows high specific binding and low nonspecific binding to a crude plasma membrane fraction of testicular cells of the domestic fowl and the Japanese quail, and to the ovarian granulosa cells of the Japanese quail. The change we made from the original method consisted of (1) using chicken LH for radioiodination that was not only highly purified but also retained a high receptor binding potency; (2) controlling the level of incorporation of radioiodine into chicken LH molecules by employing a short reaction time and low temperature; and (3) fractionating radioiodinated chicken LH further by gel filtration using high-performance liquid chromatography. Specific radioactivity of the final {sup 125}I-labeled chicken LH preparation was 14 microCi/micrograms. When specific binding was 12-16%, nonspecific binding was as low as 2-4% in the ...

Energy Technology Data Exchange (ETDEWEB)

Glycosaminoglycans synthesized by cultured rabbit smooth muscle cells were isolated after incorporation of (/sup 3/H)-glucosamine into glycosaminoglycans in the presence or absence of 10% fetal bovine serum. Glycosaminoglycans were quantitated by two-dimensional electrophoresis after proteolytic digestion of the cell layers and media. The results show that the presence of serum has no effect on the chondroitin sulfate, heparan sulfate and dermatan sulfate content of the cell layers. The incorporation of (/sup 3/H)-glucosamine into hyaluronic acid of the cell layers was three times higher in the presence of serum. In the medium , the quantity of hyaluronic was two times higher in the presence of serum while the other glycosaminoglycans remained unchanged. The incorporation of (/sup 3/H)-glucosamine into hyaluronic acid was unaffected by the presence of serum. Specific proteoglycans were isolated from medium after with (/sup 35/S)-sulfate and (/sup 3/H)-serine by isopycnic ...

Energy Technology Data Exchange (ETDEWEB)

The use of ionising radiation for the preservation of food has been under investigation for many years but has yet to receive worldwide acceptance. Although irradiation can be carefully controlled, it is generally accepted that the development of a test or tests for the detection of irradiated food would enhance consumer confidence and might help to enforce labelling regulations. The 2-alkylcyclobutanones are reported to be the only cyclic compounds formed as the products of the radiolysis of saturated and unsaturated triglycerides. The synthesis of 2-dodecylcyclobutanone (DCB) and 2-tetradecylcyclobutanone (TCB), which are formed from palmitic and stearic acid respectively following irradiation, has been carried out and using irradiated chicken meat as the model for a high-lipid containing food, both cyclobutanones have been extracted with hexane and then identified using gas chromatography/mass spectrometry (GC/MS). DCB and TCB have been detected in chicken meat ...

International Nuclear Information System (INIS)

Column chromatography of the petroleum ether and chloroformic extracts of Maytenus Forsskaoliana afforded four compounds: friedilin1, B-amyrin 2, B-sitosterol 3 and betulin 4. The structure of these compounds were established on bases of spectral (IR,MS,H and C-NMR)as well as physical data. Antimicrobial activity for extracts indicated weak potency (200ug/ml) while betulin4 showed a pronounced activity (MIC and MBC 20ug/ml).The cytotoxic activity of beutalin4 significantly indicated promising activity (IC50 40ug/ml) on both HeLa and Hep-2 cells. The pharmacological activity of diferent extracts showed sedative effect, slowing respiration, dose -dependent decrease in the arterial blood pressure by 40.1mm Hg (at adose 200mg /kg),decrease in the heart rate 67.3% (at a dose 50mg /kg)and decrease in the body temperature by 4.2C after 2 hrs (at a dose 200mg /kg). (author)

Energy Technology Data Exchange (ETDEWEB)

The influence of membrane pH gradients on the transbilayer distribution of some common phospholipids has been investigated. The authors demonstrate that the transbilayer equilibrium of the acidic phospholipids egg phosphatidylglycerol (EPG) and egg phosphatidic acid (EPA) can be manipulated by membrane proton gradients, whereas phosphatidylethanolamine, a zwitterionic phospholipid, remains equally distributed between the inner and outer monolayers of large unilamellar vesicles (LUVs). Asymmetry of EPG is examined in detail and demonstrated by employing three independent techniques: ion-exchange chromatography, {sup 13}C NMR, and periodic acid oxidation of the (exterior) EPG headgroup. In the absence of a transmembrane pH gradient ({Delta}pH) EPG is equally distributed between the outer and inner monolayers of LuVs. When vesicles composed of either egg phosphatidylcholine (EPC) or DOPC together with 5 mol % EPG are prepared with a transmembrane {Delta}pH. EPG ...

International Nuclear Information System (INIS)

Degradation of "1"4C terbufos was studied under greenhouse conditions. A mixture of "1"4C labelled compound (2.48 x 10"4 Bq of O-ethyl-1- "1"4C) und unlabelled compound (0.09 g of the granule formulation Counter 10 G) was applied to pots containing 750 g of sandy loam clay Ultisol soil with 4.9% organic matter and a cation exchange capacity of 7.6. Two treatments were established, one where maize (cultivar Cristiani) was grown and the other without plants. The soil and plants were extracted at 0, 4, 8, 16, 32 and 64 days and analyzed by a liquid scintillation counter, gas chromatography-flame photometric detector (GC-FPD) and autoradiography. The total "1"4C compounds extracted on day 64 were 31 #+-# 5.6% of the radioactivity applied in the treatments with plants and 46.1 #+-# 1.1% without plants. From the autoradiography results it can be concluded that all times the compounds identified by this technique were terbufos, terbufos sulphoxide and terbufos sulphone. ...

International Nuclear Information System (INIS)

Cobalt-60 gamma radiation has been found to be an effective means of immobilizing stationary phases onto gas and liquid chromatographic supports. The ability of a phase to crosslink was determined to be highly dependent on its chemical structure. Gamma radiation was employed to immobilize Se-30, a methylsilicone, and 216 PS onto Chromosorb WHP for packed column chromatography. The resultant columns exhibited increased thermal stability and a high degree of efficiency. Several blended phases containing varying ratios of Se-30:216 PS were also immobilized onto chromatographic packings. This work was further extended to the immobilization of Se-30 and 216 PS onto fused silica capillaries via gamma radiation. Columns exhibited excellent efficiency and improved thermal stability. An investigation into the role of immobilization of polymeric phases for HPLC was undertaken. Results indicate that gamma radiation can immobilzied polyoctadecylsiloxane and polyoctylsiloxane ...

International Nuclear Information System (INIS)

The transfer kinetics of the monosiaylated glycosphingolipid, GM_1, between different size phospholipid vesicles was measured using molecular sieve chromatography. At desired time intervals, small unilamellar donor vesicles were separated from large unilamellar acceptor vesicles by elution from a Sephacryl S-500 column ["3H]-GM_1 net transfer was calculated relative to ["1"4C]-cholesteryl oleate, which served as a nontransferable marker in the donor vesicles. The initial GM_1 transfer rate between 1-palmitoyl-2-oleoyl phosphatidylcholine vesicles at 45"0C deviated slightly from first order kinetics and possessed a half time of 3.6 days. This transfer half time is an order of magnitude shorter than that observed from the desiaylated derivative of GM_1. The transfer kinetics are consistent with the authors recent electron microscopic results suggesting a molecular distribution of GM_1 in liquid-crystalline phosphatidylcholine bilayers.

International Nuclear Information System (INIS)

A radioimmunoassay is described for the molluscan neuropeptide, Phe-Met-Arg-Phe-NH"2(FMRFamide). The antibody used is C-terminal-specific and shows slight but significant (1-2%) cross-reactivity with chicken pancreatic polypeptide (APP). The assay has been used to identify in rat brain extracts a pair of molecules that may represent mammalian counterparts of FMRFamide. Their concentrations were highest in spinal cord and hypothalamus (>10 pmol.g"-_1) and lowest in cerebellum and striatum (<3.5 pmol.g"-_1). The two immunoreactive peptides were separated on CM ion-exchange chromatography where they appeared to be less basic than FMRFamide. On Sephadex G50 gel filtration one eluted in a similar position to FMRFamide and the other slightly earlier suggesting it may be of higher molecular weight. The rat immunoreactive components do not correspond to previously described neuropeptides or hormones, and may be members of a new group of mammalian neuropeptides with ...

Energy Technology Data Exchange (ETDEWEB)

In this 150-day study, chicken manure, kenaf, and white rot fungus were added to soil microcosms in an attempt to enhance the degradation of polychlorinated biphenyls. The soil was contaminated with commercial PCB mixtures. Dishes were ammended with 5% dry weight chicken manure, 1% dry weight kenaf, and 1% dry weight kenaf plus Phanerochaete chrysosporium inoculant. PCB concentrations were determined at 30 day intervals by soxhlet extraction and gas chromatography analyses. Preliminary results of microbial populations and PCB degradation are presented. At 90 days, the microcosms amended with chicken manure had significantly higher populations of bacteria, fungi, and actinomycetes. However, at 120 days, these soils underwent great reductions in actinomycete and bacterial populations. Through 60 days, the concentration of the PCBs Aroclor 1242 and 1248 had its greatest reduction in the kenaf amended soils. The concentration of Aroclor 1260 either increased or stayed ...

International Nuclear Information System (INIS)

For ages, herbs have been used as medicine and food. Nowadays, the interest in phytotherapeutics is increasing as well as the consumer attention. Some biochemical compounds synthesized by plants as alkaloids, phenolics, flavonoids, essential oils, tannins and vitamins, influence the composition of these plant pharmacologicals, which may produce various reactions in the human body. The microbial contamination in these raw plant materials is common, and the radiation processing is one appropriate technique for the reduction of microorganism. In herbs used as food products, the changes in total #beta#-carotene and flavonoids upon the radiation treatment were tested. The powdered and dehydrated herbs were irradiated with "6"0Co gamma rays applying doses of 0, 10, 20 and 30 kGy. The botanical species investigated were rosemary (Rosmarinus officinalis Linne), watercress (Nasturtium officinale R. Br), artichoke (Cynara scolymus Linne) and sweet basil (Ocimum basilicum Linne). The alterations ...

International Nuclear Information System (INIS)

Three high density polyethylene (PE) samples of different origins, with weight average molar masses ranging from 38 to 63 kg mol"-"1 and displaying a semi-ductile behavior with strain at break ?_R values of the order of 100-140%, were gamma irradiated under nitrogen for doses up to 33.3 kGy. Steric exclusion chromatography and rheometry allowed to quantify the crosslink density X. This later reached values ranging from 4.6 to 9.0x10"-"3 mol kg"-"1, i.e. situated below the gelation point. Differential calorimetry, density measurement and small angle X-rays scattering showed the absence of significant changes in the crystalline morphology, especially lamellar dimensions. Tensile testing revealed an unexpected trend towards brittle regime of fracture while yield stress increases significantly at low doses. It appeared that branching disfavors cavitation during yielding, but this effect is not favorable to ductility.

Energy Technology Data Exchange (ETDEWEB)

A fluidized bed combustor of 0.146 m diameter and 1 m length was fabricated from stainless steel to burn olive cake. Initially, and in order to obtain fluidization, the system was operated under cold conditions using a sand with particle size in the range of 500 to 710 microns. The continuous combustion experiments were carried out under controlled conditions, such that the effects of bed temperature, olive cake feed rate, fluidization velocity, and particle size on combustion efficiency and flue gas composition were investigated. It was found that the combustion efficiency decreases with the bed temperature, fluidization velocity, and the feed rate, while it increases with the particle size used. Further, the gas products analysis carried out using a gas chromatography analyzer have shown a nonmeasured amount of SO2, and small amounts of CO. Finally, the temperature distribution along the bed indicated that the temperature throughout the bed is fairly uniform, ...

Energy Technology Data Exchange (ETDEWEB)

Labelling yield and radiochemical purity, higher than 95%, of sup(99m)Tc-colloid preparations were determined by using the paper chromatography method. Less than 3% of labelled citric acid, added to the preparation as a buffer solution, has been found in sup(99m)Tc-sulphur colloid. High radiochemical purity and optimum size of colloid particles has also been proved by biodistribution studies on experimental animals. The analysis performed has shown that more than 50% of sup(99m)Tc-colloid preparations excreted by urine is sup(99m)TcO/sup -/, the remaining past 50% being protein bound sup(99m)Tc. Biological half-time of excretion of the fast phase is the same for both preparations, i.e. 10 min, while for the slow component it is 120 min in sup(99m)Tc-S-colloid and 160 min in sup(99m)Tc-Sn colloid.

Energy Technology Data Exchange (ETDEWEB)

A procedure for the determination of carboxylic acids (benzoic and C{sub 8}-C{sub 16} aliphatic acids) in oxidised engine oils is described. It is based on a simple and selective derivatisation of the acids with a fluorescent label 9-anthracene-methanol followed by reverse-phase separation on an ODS column with a water-acetonitrile-tetrahydrofuran (20:40:40 by volume) mobile phase and post-column reaction with bis(2,4-dinitrophenyl) oxalate and hydrogen peroxide. The chemiluminiscence emission from the reaction was monitored using a lamina flow-through detector. Analysis of oxidised oils showed that although there was quenching of chemiluminiscence emission by the oil matrix, the acids could be determined over the range 0-0.4% (m/v) in the oil with a detection limit of 0.013% (m/v) (130 pmol on-column with a 20 {mu}l injection) for lauric acid. 8 figs., 2 tabs., 17 refs.

International Nuclear Information System (INIS)

Maytenus ilicifolia Mart. ex Reissek is traditionally used in Brazil for treatment of gastric ulcers. Here we report the phytochemical investigation of an ethanol extract of M. ilicifolia leaves (EEMIL) aiming at the isolation of constituents which were used as chemical markers to monitor an activity-guided fractionation of a lyophilized aqueous extract of M. ilicifolia leaves (LAEMIL). From EEMIL, four flavonoids were isolated, namely the tri-flavonoid glycosides mauritianin (1), trifolin, (2) hyperin (4), and epi-catechin (5). Fractionation of LAEMIL led to 5 fractions which afforded the tetra-glycoside kaempferol derivative (3), and galactitol (6). LAEMIL and its fractions were evaluated in rats for their effects on gastric secretion volume and pH. HPLC (High Performance Liquid Chromatography) analysis revealed that only fractions containing the tri- and tetra-flavonoid glycosides 1 and 3 caused significant increase of gastric volume and pH, thus indicating that ...

Energy Technology Data Exchange (ETDEWEB)

The objective of this work is to improve the process for CO{sub 2} capture by alkanolamine absorption/stripping by developing an alternative solvent, aqueous K{sub 2}CO{sub 3} promoted by piperazine. In Campaign 3 of the pilot plant, the overall mass transfer coefficient for the stripper with 7 m MEA decreased from 0.06 to 0.01 mol/(m{sup 3}.s.kPa) as the rich loading increased from 0.45 to 0.6 mol CO{sub 2}/mol MEA. Anion chromatography has demonstrated that nitrate and nitrite are major degradation products of MEA and PZ with pure oxygen. In measurements with the high temperature FTIR in 7 m MEA the MEA vapor pressure varied from 2 to 20 Pa at 35 to 70 C. In 2.5 m PZ the PZ vapor pressure varied from 0.2 to 1 Pa from 37 to 70 C.

Energy Technology Data Exchange (ETDEWEB)

The present work's objective is to test sampling methodologies applied on the bioremediation processes in situ, involving the establishment of sample replicates, specific laboratory procedures and its results, inedited on the referred technique. Agricultural fertilizers were used, NPK and OSMOCOTE, as biostimulants on mangroves substrates affected by petroleum activities. The tested methodology used on the experiment was based on the monitoring of this technology in aquarium with water from Sao Paulo's river and sediment contaminated by oil, realized in three steps (first pre-test, second pre-test and third pre-test) that happened between the months of August and November of 2007. The physical-chemical parameters were measured with portable devices carefully calibrated and the oil analyzed with gas chromatography. The saturated hydrocarbons (n-alkenes) had an increase on the concentrations for some aquariums and these found results do not permit ...

International Nuclear Information System (INIS)

A method for express determination of "2"3"4"-"2"3"8U, "2"3"8"-"2"4"2Pu, "2"4"1"-"2"4"3Am and "2"4"2"-"2"4"4Cm content in fuel 'hot' particles and spent nuclear fuel is offered. The method is based on precision measurement of a sample #alpha# activity followed by estimate of relative contributions of individual nuclides, or groups of radionuclides, to total activity. Segregation in separate fractions of uranium, plutonium, americium and curium was made with the help of ion-exchange chromatography. Results are presented of "2"3"4"U, "2"3"8U, "2"3"8"Pu,"2"3"9"+"2"4"0Pu, "2"4"1Pu, "2"4"2Pu, "2"4"1"Am, "2"4"2"mAm, "2"4"3Am "2"4"2"Cm and "2"4"4Cm definition in 'hot' particles sampled in Chernobyl NPP surroundings, Opportunities to apply this method for identifying radionuclide content of spent nuclear fuel are discussed.

Energy Technology Data Exchange (ETDEWEB)

We review recent development in separations and mass spectrometric instrumentation for sensitive and high-throughput proteomic analyses. These efforts have been primarily focused on the development of high-efficiency (separation peak capacity of ~103) nanoscale liquid chromatography (nanoLC; e.g., flow rates extending down to ~20 nL/min at optimal separation linear velocities through narrow packed capillaries) in combination with advanced mass spectrometry (MS), including high sensitivity and high resolution Fourier transform ion cyclotron resonance (FTICR) MS. This technology enables MS analysis of low nanogram-level proteomic samples (i.e., nanoscale proteomics) with individual protein identification sensitivity at the low zeptomole-level. The resultant protein measurement dynamic range can reach 106 for nanogram-sized proteomic samples, while more abundant proteins can be detected from complex sub-picogram size proteome samples. The average proteome ...

Energy Technology Data Exchange (ETDEWEB)

Extra-fine powdered activated charcoal has been used as stationary phase (coating layer) in solid-phase microextraction (SPME). The efficiency and reliability of the prepared device have been investigated for the extraction of some volatile organic compounds such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) from the headspace of water samples. Monitoring of the extracted compounds and further quantitative analysis of the real samples have been performed by capillary GC-FID. Effects of several factors such as temperature, addition of salt, and stirring speed on extraction efficiency and exposure time have been studied. Under optimum conditions, extraction recoveries for these compounds from 50 mL water were >95%. The calibration graphs were linear in the range 5 to 10{sup 4} pg mL{sup -1} and the detection limit for each BTEX compound was 1.5-2 pg mL{sup -1}. The results obtained by use of this porous layer activated charcoal (PLAC)-coated fiber have also been compared ...

Energy Technology Data Exchange (ETDEWEB)

The research had as objective the use of the gamma radiation of the Cobalto-60 as quarantine treatment of the medicinal plant, aromatic and seasoning plants dehydrated infested by Lasioderma serricorne and Plodia interpunctella determining the disinfestation doses to attend the criterion in the not emergency of adults of the species in study and analysing through the Chromatography of Thin Layer the effect of the gamma radiation of the cobalto-60 on the active principle of extract dehydrated of Chamomilla recutita, Pimpinella anisum, Origanum vulgare, Cymbopogon citratus, Ocimum basilicum and Thymus vulgaris. The work was developed in the Laboratorio de Inseticidas in the Instituto Biologico in Sao Paulo in the period of August of 2005 the June of 2007. The radiation source used gamma was an experimental irradiator of Cobalto-60, model Gamacell 220, located in the Instituto de Pesquisas Energeticas e Nucleares - IPEN, located in Sao Paulo. In the period of 30 days ...

Energy Technology Data Exchange (ETDEWEB)

The entrapment of proteins using the sol-gel route provides a means to retain its native properties and artificially reproduce the molecular crowding and confinement experienced by proteins in the cell allowing investigation of the physico-chemical and structural properties of biomolecules at the biotic/abiotic interface. The biomolecules are spatially separated and 'caged' in the gel structure but solutes can freely permeate the matrix. Thus, properties such as the folding of ensembles of individual molecules can be examined in the absence of aggregation effects that can occur in solution studies. Green fluorescent protein from Aequorea coerulescens was used as a model protein to examine the unfolding/re-folding properties of protein in silica gels. The recombinant protein was isolated and purified from Escherichia coli extracts by cell lysis, three-phase partitioning, dialysis, and anion exchange chromatography. The purity of the protein was ...

International Nuclear Information System (INIS)

Full text: HMPAO, a butane monoxime derivative of propylene amine and ECD, ethyl cysteinate dimer, are currently being used as brain imaging agents. In an effort to develop new radiopharmaceuticals for imaging brain, we have synthesized amine and imine derivatives of ethyl cysteinate with butane monoxime, optimized labelling procedure with "9"9"mTc and studied the in vivo behaviour of their "9"9"mTc complexes. Imine derivative of ethyl cysteinate with butane monoxime was synthesized by refluxing equimolar amounts of butane monoxime and ethyl cystinate in dry benzene for 3 hours. The product was purified over silica with 10% ethyl acetate in chloroform as eluent. Amine derivative was prepared by reducing the imine derivative with sodium borohydride. The ligands were characterized by NMR spectroscopy and were found to be pure. The ligands were labelled with "9"9"mTc using stannous chloride as reducing agent. The complexes were characterized by paper chromatography, ...

International Nuclear Information System (INIS)

The mechanism of action of Clostridium difficile enterotoxin A (CA), of Escherichia coli enterotoxin (STa) and of cholera toxin (CT), which are known to cause severe diarrhea, were studied in a preparation of ligated jejunal loops of anesthetized rats in vivo. The toxins were administered intraluminally. Pharmacological agents, which were tested for their potency to influence toxin-related effects, were administered subcutaneously. Net fluid transport was determined gravimetrically, prostaglandin (PG) E_2-output into the lumen, cyclic adenosine monophosphate (cAMP) and cyclic guanosine monophosphate (cGMP) contents in the mucosa were measured by radioimmunoassay, serotonin-(5-HT)-output into the lumen was determined by high performance liquid chromatography. The histopathological effects of CA and CT were examined by light- and scanning electron microscopy. All three toxins caused net fluid secretion (FS). 5-HT_2-(ketanserin) and 5-HT_3-receptor antagonists ...

Science.gov (United States)

Acetylcholine-rich synaptic vesicles were isolated from myenteric plexus-longitudinal muscle strips derived from the guinea pig ileum by the method of Dowe, Kilbinger, and Whittaker [J. Neurochem. 35, 993-1003 (1980)] using either unstimulated preparations or preparations field-stimulated at 1 Hz for 10 min using pulses of 1 ms duration and 10 V . cm-1 intensity. The organ bath contained either tetradeuterated (d4) choline (50 microM) or [3H]acetate (2 muCi . ml-1); d4 acetylcholine was measured by gas chromatography-mass spectrometry. As with Torpedo electromotor cholinergic vesicle preparations made under similar conditions the distribution of newly synthesized (d4 or [3H]) acetylcholine in the zonal gradient from stimulated preparations was not identical with that of endogenous (d0, [1H]) acetylcholine, but corresponded to a subpopulation of denser vesicles (equivalent to the VP2 fraction from Torpedo) that had preferentially taken up newly synthesized ...

International Nuclear Information System (INIS)

A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of "2"3"7Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry. "2"3"8U can interfere with "2"3"9Pu measurement by ICP-MS as "2"3"8UH"+ mass overlap and "2"3"7Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes ...

Energy Technology Data Exchange (ETDEWEB)

A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of {sup 237}Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so ...

Science.gov (United States)

Four trypsin inhibitor homologs, the first known from Dendroaspis angusticeps venom, were characterized using a combination of gel filtration, cation exchange, reverse-phase liquid chromatography, Edman degradation and mass spectrometry. The four toxins comprise two 57 residue and two 59 residue isoforms. The long toxins possess a Lys-Gln N-terminal extension lacked by the short toxins. The only other structural difference is an Arg/His replacement at position 55. The long Arg55 variant is identical to trypsin inhibitor E from the venom of Dendroaspis polylepis. The name epsilon-dendrotoxin is suggested so as to follow the nomenclature of Benishin, C.G., Sorensen, R.G., Brown, W.E., Krueger, B.K., Blaustein, M.P., 1988. Four polypeptide components of green mamba venom selectively block certain potassium channels in rat brain synaptosomes. Mol. Pharmacol. 34, 152-159. Among snake venom protease inhibitors, the epsilon-dendrotoxins are structurally most like the ...

Energy Technology Data Exchange (ETDEWEB)

Research at the interface between biomolecules and inorganic nanocrystals has resulted in a great number of new discoveries. In part this arises from the synergistic duality of the system: biomolecules may act as self-assembly agents for organizing inorganic nanocrystals into functional materials; alternatively, nanocrystals may act as microscopic or spectroscopic labels for elucidating the behavior of complex biomolecular systems. However, success in either of these functions relies heavily uponthe ability to control the conjugation and assembly processes.In the work presented here, we first design a branched DNA scaffold which allows hybridization of DNA-nanocrystal monoconjugates to form discrete assemblies. Importantly, the asymmetry of the branched scaffold allows the formation of asymmetric2assemblies of nanocrystals. In the context of a self-assembled device, this can be considered a step toward the ability to engineer functionally distinct inputs and outputs.Next we develop an ...

Energy Technology Data Exchange (ETDEWEB)

Dunaliella salina cells were pulse-labeled for 2 min with (/sup 14/C)palmitic acid, (/sup 14/C)oleic acid, or (/sup 14/C)lauric acid in order to trace the pathway of galactolipid biosynthesis and desaturation. Through the use of high performance liquid chromatography it was possible to follow the movement of radioactivity through many individual molecular species of monogalactosyldiacylglycerol (MGDG) and digalactosyldiacylglycerol (DGDG) for periods of 24 h and, in some cases, as much as 120 h. Analysis of the fatty acid fluxes permitted us to refine current views regarding biosynthesis of the predominantly prokaryotic galactolipids. The initial D. salina MGDG molecular species, containing paired oleate and palmitate (18:1/16:0), can follow two metabolic routes. If the palmitoyl chain is desaturated to 16:1, the resulting 18:1/16:1 MGDG is subject to rapid further desaturation to varying degrees, and a part of these products is subsequently galactosylated to DGDG. ...

Energy Technology Data Exchange (ETDEWEB)

The PbII binding characteristics of the previously reported PbII binding proteins of rat kidney cytosol were investigated further. Saturation and Scatchard analysis of /sup 203/Pb binding in whole cytosol and in 40% saturated ammonium sulfate precipitated fractions disclosed a class of relatively high-affinity sites with an apparent Kd of approximately 50 nM and binding capacities of approximately 41 and 9 pmol/mg of protein, respectively. Two /sup 203/Pb binding proteins with approximate molecular masses of 63K and 11.5K daltons and a high molecular weight component (greater than 200K) were isolated by Sepharose-6B column chromatography. The time course of association of /sup 203/Pb with cytosol and the 63K protein showed maximum binding at 18 hr which was stable up to 25 hr at 4 degrees C. The approximate half-time dissociation rate (T 1/2) of specifically bound /sup 203/Pb to the 63K protein was 100 min at 4 degrees C whereas the 11.5K protein showed little ...

Science.gov (United States)

The lipid fractions of residues from historical pharmaceutical ointments were analysed by reversed-phase liquid chromatography coupled with atmospheric pressure chemical ionization and mass spectrometer detection. The residues were contained in a series of historical apothecary jars, dating from the eighteenth century and conserved at the "Aboca Museum" in Sansepolcro (Arezzo, Italy) and at the pharmacy of the "Real Cartuja de Valldemossa" in Palma de Majorca (Spain). The analytical protocol was set up using a comparative study based on the evaluation of triacylglycerol (TAG) compositions in raw natural lipid materials and in laboratory-reproduced ointments. These ointments were prepared following pharmaceutical recipes reported in historical treatises and used as reference materials. The reference materials were also subjected to stress treatments in order to evaluate the modification occurring in the TAG profiles as an effect of ageing. TAGs were successfully ...

International Nuclear Information System (INIS)

In-vitro experiments using "2"0"3Pb were performed to identify the lead binding components in human peripheral blood. The distribution of lead in plasma, in the red cell membrane, and within the red cell was also investigated. Studies of the distribution of "2"0"3Pb in the whole blood showed that at a lead concentration of 2.45 #mu#mol/l (50 #mu#g/100 ml) about 94% of lead had been incorporated by the erythrocytes and 6% remained in the plasma. After extraction of lipid by a methanol/chloroform mixture, about 75% of the lead was found to be associated with the protein fraction. The lipid contained about 21% of the "2"0"3Pb, the remainder being in the aqueous plasma. SDS polyacrylamide gel electrophoresis of blood plasma showed that almost 90% of the "2"0"3Pb was present in the albumin fraction; the remainder was likely to be associated with high molecular weight globulins. Several binding sites were identified on the erythrocyte membrane. The high molecular weight component, about 130 ...

Energy Technology Data Exchange (ETDEWEB)

While tritium exposure to the site-workers in Wolsung NPP is upto about 40 % of the total personnel exposure, Korea Institute of Nuclear Safety has asked tritium removal facility, as one of the requirements for post reactor construction, after operation of four CANDU reactors in Wolsung site. For the purpose of essential removal of tritium from the heavy water system of the heavy water reactors, an experiment of Ar-N{sub 2} cryogenic distillation tower was carried out as a preliminary study for development of liquid-phase catalytic exchange - cryogenic hydrogen distillation process. The steady-state reached after 50 minutes under 90 K in the Ar-N{sub 2} distillation column (inner diameter 20 mm, height 500 mm) packed with Dixon ring ({phi} 3 mm x H 3 mm), and the ratios of Ar-concentration at the top and at the bottom measured by gas chromatography within {+-}1 % relative error was approximately 93 : 3. This value was distillation performances quite higher than ...

Energy Technology Data Exchange (ETDEWEB)

The fixed bed pilot plant, the catalyst testing procedure, and the calculations for conversion and selectivities were previously described in the technical progress report covering the period of 3/16/88 to 6/16/88 for Contract DE-AC22-87PC79812. Conversions and hydrocarbon selectivities were calculated using data from an on-line gas chromatography (GC) analyzer. Alcohol selectivities were calculated using data from an on-line boiling point GC analyzer which analyzed the liquid product. The catalysts were prepared via the steps of impregnation, calcination, and reduction on a special Y-zeolite-derived support. The impregnation step consisted of evaporation of metal salts on to the support from an aqueous solution. For one catalyst (No. 6531-188) the metal salts were evaporated on to the support from a reverse micelle solution containing the metal salts. All the catalysts were calcined for four hours at 450{degree}C. The calcined catalysts were loaded in the reactor ...

International Nuclear Information System (INIS)

Studies are made in this program to enhance our understanding of the role of 5f electrons in chemical bonding. Most of our studies on the macroscopic scale emphasize certain isotopes available from the National Transplutonium Production Program centered at HFIR/TRU -namely, _9_6"2"4"8Cm, _9_7"2"4"9Bk, _9_8"2"4"9Cf, _9_9"2"5"3Es, and _9_9"2"5"4Es. Particular classes of compounds, such as hydrides, chalcogenides, and pnictides are often selected for study on the basis of their utility in bringing out significant chemical differences between the lanthanides and the actinides. High temperature/high pressure experiments on actinide metals and compounds reveal characteristics about the degree of 5f electron localization as a function of atomic number in the series. Magnetic properties of metals and compounds are investigated using ultra-sensitive methods and hydration numbers of ions in solution are investigated by neutron scattering at HFIR. As a result of a recently renewed ...

International Nuclear Information System (INIS)

Arsenic was predominantly present as inorganic arsenite in the fronds of the hyperaccumulator Chinese brake. - Arsenic speciation is important not only for understanding the mechanisms of arsenic accumulation and detoxification by hyperaccumulators, but also for designing disposal options of arsenic-rich biomass. The primary objective of this research was to understand the speciation and leachability of arsenic in the fronds of Chinese brake (Pteris vittata L.), an arsenic hyperaccumulator, with an emphasis on the implications for arsenic-rich biomass disposal. Chinese brake was grown for 18 weeks in a soil spiked with 50 mg As kg"-"1 as arsenate (AsO_4"3"-), arsenite (AsO_3"3"-), dimethylarsinic acid (DMA), or methylarsonic acid (MMA). Plant samples were extracted with methanol/water (1:1) and arsenic speciation was performed using high performance liquid chromatography coupled with atomic fluorescence spectrometry. The impacts of air-drying on arsenic species and ...

Energy Technology Data Exchange (ETDEWEB)

N/C and S/C ratios show only minor differences between asphaltenes and coal on this basis, the asphaltenes continue to appear to be good surrogates for the characterization of organic acid rain precursors in coal. Alkylmethoxythiophene carboxylic acids (ATCA) are detected in all dichromate oxidation products analyzed to date. Relative concentrations of ATCA compounds are directly proportional to the sample`s bulk organic sulfur contents. Concentrations of ATCA compounds in oxidation products decrease upon repeated oxidation. This may indicate that the thiophenic groups tend to be located in external positions on the coal macromolecular structure and a high proportion of them can be stripped away with only one mild oxidation step. If true, this may make industrial-scale removal of organic sulfur easier than expected. Using analytical micropyrolysis-gas chromatography with a sulfur-selective flame photometric detector, it is possible to easily see a full distribution ...

Energy Technology Data Exchange (ETDEWEB)

A comparison between chicken and rat lung was made for microsomal prostaglandin (PG) synthesis from 1-/sup 14/C-arachidonic acid. Microsomal protein (2.0 mg) from chicken or rat lung was incubated in the presence of 20 ..mu..g of 1-/sup 14/C-arachidonic acid (specific activity = 3 x 10/sup 6/ dpm/..mu..mol for chicken; 6 x 10/sup 6/ dpm/..mu..mol for rat), 0.05 M Tris-HCl buffer (pH = 8.0), 0.5 mM epinephrine, and 1 mM reduced glutathione in a total volume of 0.5 ml in a 37/sup 0/C water bath with shaking for 15 min. After acidification with 1 M HCl to pH 3, prostaglandins were extracted with ethyl acetate. The products of the reactions were separated by reversed phase chromatography, and the radioactivity of each prostanoid fraction was determined. The predominant prostanoid synthesized by chicken lung microsomes was PGE/sub 2/, followed by much lower amounts of thromboxane B/sub 2/ (TXB/sub 2/), PGF/sub 2//sub ..cap alpha../ and PGD/sub 2/. In at lung, ...

Science.gov (United States)

Batch interaction experiments were performed under aerobic conditions to characterize the adsorption behavior and valence speciation of CoEDTA complexes (equimolar at 10 -5 mol/L) in a series of Pliocene subsurface sediments containing various amounts of Fe and Mn oxides. The experiments were performed in 0.003 mol/L Ca(ClO 4 ) 2 with a solids concentration of 500 g/L at variable pH (4-9) and at the natural pH of the sediments (pH = 8.3). Three of these subaerial sediments (Ringold 1, 2, 3) contained significant quantities of extractable Fe and Mn, while the fourth (Ringold 4) was virtually devoid of sesquioxide precipitates. Microscopic and mineralogic analyses of the most heavily encrusted material (Ringold 2) showed that the oxides existed as intergrain cements and contained crystalline goethite and rancieite/todorokite. Adsorption on a synthetic analog sorbent (0.6 mass % ferrihydrite-coated sand) over a range in pH showed that, while both Co(II)EDTA 2- and Co(III)EDTA - sorb ...

Energy Technology Data Exchange (ETDEWEB)

This paper presents the characteristics of selected parameters of organic matter of the Tertiary coal samples and organic matter of Carboniferous rock samples from the Spitsbergen. The coal samples were taken from Central Coal Basin (the Longyearbyen region) and from the Forlandsundet Basin (Oscar II Land, the Kaffioyra region). Samples of dispersed organic matter were collected from Suffolk Pynten and Sergeijevfjellet area in Sorkapp Land. The optical properties of coal samples are different from properties of dispersed organic matter. Macerals of vitrinite group dominate in all of the samples. The average content of vitrinite group macerals is much lower in dipersed organic matter samples than it is in coals. The average content of liptinite group macerals is a little lower, and inertinite group macerals is much higher. The average content of mineral matter is higher in organic matter samples than in coal samples. The average value of vitrinite reflectance and standard deviation of ...

Energy Technology Data Exchange (ETDEWEB)

Chemical composition of fine aerosol particles over the northern Chilean coastal waters was determined onboard the U.S. DOE G-1 aircraft during the VOCALS (VAMOS Ocean-Cloud-Atmosphere-Land Study) field campaign between October 16 and November 15, 2008. SO42-, NO3-, NH4+, and total organics (Org) were determined using an Aerodyne Aerosol Mass Spectrometer, and SO42-, NO3-, NH4+, Na+, Cl-, CH3SO3-, Mg2+, Ca2+, and K+ were determined using a particle-into-liquid sampler-ion chromatography technique. The results show the marine boundary layer (MBL) aerosol mass was dominated by non- sea-salt SO42- followed by Na+, Cl-, Org, NO3-, and NH4+, in decreasing importance; CH3SO3-, Ca2+, and K+ rarely exceeded their respective limits of detection. The SO42- aerosols were strongly acidic as the equivalent NH4+ to SO42- ratio was only ~0.25 on average. NaCl particles, presumably of sea-salt origin, showed chloride deficits but retained Cl- typically more than half the ...

Energy Technology Data Exchange (ETDEWEB)

This study follows previous experimental work showing that the shrinking-core model applies to the pyrolysis (i.e., heating in the absence of oxygen) of particles (diam.{approx}14 mm) of a bituminous coal or a lignite in a fluidized bed at 700-950 {sup o}C. These experimental facts are in accord with the production of volatile matter being endothermic and not thermoneutral, as often assumed. Also, the rate at which volatile matter is produced in the presence of oxygen (i.e., devolatilization) or in its absence (pyrolysis) is demonstrated here to be controlled not at all by mass transfer, but by heat conduction to a moving reaction front inside a coal particle, provided its diameter exceeds {approx}3 mm. The resulting steady-state model of devolatilization indicates that six dimensionless groups are required to describe the rate of(I)coal->char+volatile matter for a nonfragmenting and nonswelling coal. This reaction occurs for a total time of c{sub 1}r{sub 0}+c{sub 2}r{sub 0}{sup ...

Energy Technology Data Exchange (ETDEWEB)

In nuclear fuel, in approximately one quarter of the fissions, one of the two formed fission products is gaseous. These are mainly the noble gases xenon and krypton with isotopes of xenon contributing up to 90% of the product gases. These noble fission gases do not combine with other species, and have a low solubility in the normally used uranium oxide matrix. They can be dissolved in the fuel matrix or precipitate in nanometer-sized bubbles within the fuel grain, in micrometer-sized bubbles at the grain boundaries, and a fraction also precipitates in fuel pores, coming from fuel fabrication. A fraction of the gas can also be released into the plenum of the fuel rod. With increasing fission, and therefore burn-up, the ceramic fuel material experiences a transformation of its structure in the 'cooler' rim region of the fuel. A subdivision occurs of the original fuel grains of few microns size into thousands of small grains of sub-micron sizes. Additionally, larger ...