Energy Technology Data Exchange (ETDEWEB)

We provide two examples to illustrate how electronic structure calculations contribute to our understanding of vacancies and their role in determining material properties. Diffusion and elctromigration in aluminium are known to depend strongly on vacancies. Electronic structure calculations show that the vacancy-impurity interaction oscillates with distance, and this leads to an explanation for both the increased elctromigration resistance and the slow impurity diffusion for copper in aluminium. Calculations of vacancies in plutonium have been used in conjunction with positron annihilation lifetime measurements to identify the presence of helium-filled vacanies. Helium stabilization of vacancies can provide the precursors for subsequent vacancy-related changes in materials properties.

Science.gov (United States)

PMID:7075772

British Library Electronic Table of Contents (United Kingdom)

There is proposed the nonlinear model of dose dependence saturation of the yield strength on the base of the vacancy and interstitial barrier interaction in this work. Processes of mutual recombination of vacancy and interstitial barriers and formation of vacancy and interstitial clusters are taken into consideration. In the framework of the model, the analytical equations corresponding to the evolution of the barrier densities and yield strength are obtained. It is shown that the yield strength of irradiated materials decreases with the increasing intensity of barrier recombination processes, the dependence being nonlinear. Also it is shown that the model is valid both for low doses and large doses on the stage of radiation hardening.

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

International Nuclear Information System (INIS)

In this letter, the effect of vacancies generated by preirradiated laser on dopant diffusion and activation in preamorphized silicon substrate has been studied. Laser-induced melting in silicon was used to generate excess vacancies near the maximum melt depth before silicon substrate amorphization and subsequent boron implantation. We demonstrate that by matching the preirradiated laser melt depth with the implant amorphize depth, it can effectively reduce the silicon self-interstitials released from the end-of-range defect band. The results show great suppression in boron transient enhanced diffusion and significant removal of end-of-range defects. This is attributed to the recombination of laser-generated excess vacancies with preamorphizing induced free silicon interstitials at the end-of-range region.

International Nuclear Information System (INIS)

Angular dependence from L_3-subshell to M-shell vacancy transfer probabilities for selected heavy elements from Au to U have been measured by using a Si(Li) detector coupled to a model 1024 computerized multi-channel analyzer. Because the angular dependence from L_3-subshell to M-shell vacancy transfer probabilities is not found in the literature, to the best of our knowledge there are no experimental values for worked elements. Therefore, the results for the elements obtained in the present study constitute the first experimental measurements; the comparison has been not made with other experimental and theoretical results. It has been observed that angular dependence from L_3-subshell to M-shell vacancy transfer probabilities increase with increasing cos #theta#.

International Nuclear Information System (INIS)

Data on the recovery of Tsub(c) for several neutron irradiated A-15 compounds are presented. A model for the mechanism of recovery is suggested and has been applied to isothermal annealing data at 550"0C on a sample of Nb_3Ge and to isochronal annealing (200"0C-900"0C) data on V_3Si, Nb_3Ge and Nb_3Sn subjected to varying doses of fast neutrons and on Nb_3Al of various compositions subjected to the same dose. The recovery is assumed to take place by vacancy assisted reordering and occurs in several stages. The major low temperature stage is attributed to irradiation induced vacancies, while at high temperatures there are depleted and recovery is ascribed to the motion of thermal equilibrium vacancies. Activation energies deduced for these processes, approximately 1 eV for vacancy motion and approximately 1-2 eV for vacancy formation, are consistent with what is known about diffusion ...

Energy Technology Data Exchange (ETDEWEB)

Enhanced superlattice disordering in nonstoichiometric AlAs/GaAs quantum wells exhibits weak temperature dependence because of the decay of the supersaturated concentration of group-III vacancies. We present a formalism for transient enhanced diffusion in nonstoichiometric materials with which we can extract migration enthalpies {ital H}{sub {ital m}} by assuming that the vacancy decay is thermally activated with an enthalpy {ital H}{sub {ital a}}. By analyzing the electroabsorption from the quantum-confined Stark effect for a set of isochronal and isothermal anneals, we extract a migration enthalpy {ital H}{sub {ital m}}=(1.8{plus_minus}0.2) eV for group-III vacancies, as well as an activation enthalpy {ital H}{sub {ital a}}=(0.7{plus_minus}0.2) eV for vacancy annihilation. {copyright} {ital 1996 American Institute of Physics.}

UK PubMed Central (United Kingdom)

A high performance liquid chromatography (HPLC) procedure suitable for the simultaneous determination of the molecular size and concentration of macromolecular hyaluronate and proteoglycans in synovial...Full Text Available

UK PubMed Central (United Kingdom)

Denaturing high-performance liquid chromatography (DHPLC) has been used extensively to detect genetic variation. We used this method to detect and identify Yersinia pestis KIM5 ciprofloxacin-resistant...Full Text Available

UK PubMed Central (United Kingdom)

An anion-exchange column technique for extraction of antibiotics from serum proteins has been developed for use in the assay of cephapirin, cefotaxime, and cefoxitin by high-pressure liquid chromatography....Full Text Available

Energy Technology Data Exchange (ETDEWEB)

We measure the transient enhanced diffusion of shallow molecular-beam-epitaxy grown marker layers of Sb and B due to deep MeV Si{sup +} ion implants at very high doses ({approx}10{sup 16}cm{sup {minus}2}). We expect the near-surface region of these implants to be vacancy rich, and we observe transient enhanced diffusion of Sb (the classic vacancy diffuser). The large enhancements imply a significant vacancy supersaturation ({approx}700 at 740{degree}C). Double implantation of the high-dose MeV Si followed by a shallow (40 keV) Si implant and annealing produces a greatly reduced number of {l_brace}311{r_brace} defects compared to a 40 keV implant into virgin Si, again consistent with a vacancy-rich region in the near-surface region of an MeV implant. However, the shallow B marker layers also show transient enhanced diffusion for the same MeV implant under similar annealing conditions, implying that an ...

Energy Technology Data Exchange (ETDEWEB)

This paper reports that the point defect model for steady-state passive films formed anodically on metal s in aqueous environments has been extended to include irreversible dissolution of the film and the irreversible generation and annihilation of cation and oxygen vacancies at the metal/film and film/solution interfaces. THe model yields a number of diagnostic criteria that can be used to identify the majority (vacancy) charge carrier and to characterize the kinetic nature of the interfacial vacancy generation and annihilation processes. We use these criteria to show that the steady-state passive film that forms on nickel in acidic phosphate buffer solutions is a cation conductor and that cation transport from the metal to the solution involves irreversible ejection of cations from the film. On the other hand, the passive film that forms on tungsten in the same environment under steady-state conditions is found to be an ...

Energy Technology Data Exchange (ETDEWEB)

The {delta} {yields} {alpha}{prime} martensitic transformation in Pu-1.9 at.% Ga occurs when the alloy is cooled below about -100 C. This transformation exhibits anomalous behavior, where the isothermal transformation proceeds atypically with double-C kinetics. Recent work has revealed that an ambient temperature isothermal hold (referred to as conditioning) prior to the transformation has different effects depending on whether transformation proceeds in the upper- or lower-C of the double-C: the amount of transformation is increased with conditioning in the upper-C, while the transformation in the lower-C seems to be engendered by conditioning. The mechanism by which conditioning affects the low-temperature {delta} {yields} {alpha}{prime} transformation is thus of great importance to understanding the transformation itself as well as the general circumstances that can affect a martensitic phase transformation. Using differential scanning calorimetry measurements, ...

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).

Energy Technology Data Exchange (ETDEWEB)

The aim of this work is to account for the effects of the high temperature oxidation of metals on their microstructure and their mechanical properties. 'Model' materials like pure nickel, pure iron and the Ni-20Cr alloy are studied. Nickel foils have been oxidised at 1000 C on one side only in laboratory air, the other side being protected from oxidation by a reducing atmosphere. After the oxidation treatment, the unoxidized face was carefully examined by using an Atomic Force Microscope (AFM). Grain boundaries grooves were characterised and their depth were compared to the ones obtained on the same sample heat treated in the reducing atmosphere during the same time. They are found to be much deeper in the case of the single side oxidised samples. It is shown that this additional grooving is directly linked to the growth of the oxide scale on the opposite side and that it can be explained by the diffusion of the vacancies produced at the oxide ...

International Nuclear Information System (INIS)

Research and development activities are reported on absorption spectroscopy, calorimetry, electrolysis, emission spectroscopy, fluorimetry gas chromatography, infrared spectroscopy, liquid chromatography, liquid scintillation counting, mass spectroscopy, microscopy, radiometric analysis, and thermal analysis. A group of miscellaneous projects are also described.

International Nuclear Information System (INIS)

The effect of the #+-# 0.75 T external magnetic field on the K_#alpha#_1, K_#alpha#_2, K_#beta#_'_1 and K_#beta#_'_2 x-ray production cross sections and radiative vacancy transfer probabilities from K-shell to L2 and L3 subshells and M-shell for ferromagnetic Nd, Gd and Dy and paramagnetic Eu and Ho have been investigated, using the 59.5 keV incident photons. K-shell fluorescence yields and K x-ray intensity ratios for these elements have been determined in the external magnetic field also. The K x-rays from different targets were detected using a high-resolution Si(Li) semiconductor detector. For B = 0, the present experimental results were compared with the experimental and theoretical data in the literature. The results show that K-shell fluorescence parameters such as photoionization cross section, fluorescence yield, radiation rates, vacancy transfer probabilities and spectral linewidth can change owing to the applied magnetic field. ...

International Nuclear Information System (INIS)

Structural variations in 39-MeV alpha-particle irradiated (Tsub(irr) = 60 deg C) polycrystalline molybdenum during post-irradiation annealing were studied by X-ray and TEM methods. Despite the high density of irradiation induced defects in the structure of the specimen X-ray measurements showed zero relative lattice parameter change after an irradiation dose of 1.1 x 10"-_2 dpa. However, during the annealing #delta#a/a was changed in the positive range, exhibiting two peaks - at 100 and 300 deg C - whereas the damage structure detected by TEM indicated no changes. Analysis of the results leads to the conclusion that in the range 100 to 250 deg C migration of isolated vacancies and their annihilation at interstitial clusters as well as possible formation of new vacancy clusters occur. The second peak on the #delta#a/a temperature dependence curve is related to the transformation (probably, thermal disintegration) of vacancy ...

International Nuclear Information System (INIS)

The evolution of metallic substance atomic structure is studied on temperature variation including crystal heating up to melting points, a crystal- liquid phase transition and initiation of a high-density liquid specific structure. It is marked that heat induced changes of simple metal structure can be described as changes around a natural elementary cell which is common for both a crystal and a liquid and consists of a central atom and Z_1 atoms of the first coordination sphere. On this basis the vacancy model of melting is verified. Concentrations of melting vacancies are determined by coordination numbers in the form of Z_1/(1+Z_1)"2 which are the same for both a crystal and a natural elementary cell. The size of natural elementary cells is in an agreement with that of the coordination sphere featured in the liquid and phase transition statistical theory. Calculated data are given for a number of metals, Cs, Eu, Ni, V included

Energy Technology Data Exchange (ETDEWEB)

The measurements of the K X-ray intensity ratio I(K{sub {beta}})/I(K{sub {alpha}}) for the 17 elements Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Br, Rb, Sr, Y, Zr, Nb and Mo have been done following ionization by 59.5keV {gamma}-rays from a {sup 241}Am point source. Ratios of emission probabilities of Auger electrons and the vacancy transfer coefficients have been extracted in terms of the intensity ratios. It is found that the present results agree well with earlier fitted values and the semi-empirical values.

British Library Electronic Table of Contents (United Kingdom)

The thermodynamic characteristics of sorption of the isomeric tricyclo[5.2.1.02.6]decane (tetrahydrodicyclopentadiene, TDCPD) molecules were for the first time determined experimentally and by molecular statistical methods under the conditions of gas-adsorption chromatography on graphitized thermal carbon black and gas-liquid chromatography on stationary liquid phases of different polarities (Apiezon L and Carbowax 20M). The effects of the chemical nature of sorbents on the retention of the TDCPD isomers are considered. A procedure for calculating the thermodynamic characteristics of adsorption of molecules with a complex structure is suggested within the framework of the atom-atom approximation of the semiempirical molecular statistical theory of adsorption for the example of isostructura...

International Nuclear Information System (INIS)

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. (author).

British Library Electronic Table of Contents (United Kingdom)

The degradation of irradiated human insulin in aqueous solutions was investigated in order to protect the protein against ionizing radiation. The influence of the drug concentration, excipients and irradiation temperature were studied.Aqueous solutions at pH 2 were irradiated by gamma rays or by accelerated electrons. Two different high-performance liquid chromatography (HPLC) methods were used: reverse-phase high-performance liquid chromatography (RP-HPLC)/UV and size exclusion liquid chromatography (SEC/UV) to investigate both the fragmentation and the formation of higher molecular weight proteins.In solution without excipients irradiated at ambient temperature at 10kGy, the loss of human insulin is almost complete. Addition of radio-protecting excipients (free radicals scavengers) and c...

British Library Electronic Table of Contents (United Kingdom)

Phycocyanin - a major phycobiliprotein constitutively produced by many cyanobacteria hold several promising applications in diagnostics, biomedical research, and therapeutics. This paper discusses a novel rapid method for the purification of cyanobacterial phycocyanin (C-PC) from Phormidium fragile using hydrophobic interaction chromatography. The protein was extracted and concentrated by grinding under liquid nitrogen and ammonium sulfate fractionation. C-PC was purified by single step hydrophobic interaction chromatography. Purified phycocyanin showed absorbance maximum (lmax) at 624nm. The criterion of purity (R) achieved was 4.52. Phycocyanin to phycoerythrin and phycocyanin to allophycocyanin purity ratio were 3.85 and 7.49, respectively. The purified protein showed a pI of 5.2 and ha...

International Nuclear Information System (INIS)

The oxygen vacancies distribution in the rigid lattice and the thermally activated motion of oxygen atoms are studied in La1-xSrxGa1-xMgxO3-x (x=0.00; 0.05; 0.10; 0.15 and 0.20) compounds. For that 71Ga, 25Mg and 17O NMR was performed from 100 K up to 670 K, and ion conductivity measurements were carried out up to 1273 K. The comparison of the electric field gradients at the Ga- and Mg-sites evidences that oxygen vacancies appear exclusively near gallium cations as a species trapped below room temperature in local clusters, GaO5/2-#square#-GaO5/2. These clusters decay at higher temperature into mobile constituents of the structural octahedra Ga(O5/6#square#1/6)6/2. At the same time, the nearest octahedral oxygen environment of magnesium cations persists at different doping levels. The case of two adjacent vacant anion sites is found highly unlikely within the studied doping range. The thermally activated oxygen motion starts to develop above ...

Energy Technology Data Exchange (ETDEWEB)

Amorphization and a dual implant technique have been used to manipulate residual defects that persist following implantation and post-implant thermal treatments. Residual defects can often be attributed to ion-induced defect excesses. A defect is considered to be excess when it occurs in a localized region at a concentration greater than its complement. Sources of excess defects include spatially separated Frenkel pairs, excess interstitials resulting from the implanted atoms, and sputtering. Preamorphizing prior to dopant implantation has been proposed to eliminate dopant broadening due to ion channeling as well as dopant diffusion during subsequent annealing. However, transient-enhanced diffusion (TED) of implanted boron has been observed in pre-amorphized Si. The defects driving this enhanced boron diffusion are thought to be the extended interstitial-type defects that form below the amorphous-crystalline interface during implantation. A dual implantation process was applied in an ...

International Nuclear Information System (INIS)

M shell x-ray production cross sections in thick targets of Pb, Th and U by K x-rays of Rb, Nb and Mo respectively have been measured. As the incident K x-ray energies are above the L_3 edge but below L_2 edge energies of the respective target elements under reference, the M x-rays are produced not only due to direct interaction of incident photons with M shell electrons but also due to the shift of the L_3 subshell vacancies to the M shell. The experiment has been performed using a double reflection geometrical setup with a 1 Curie"2"4"1Am gamma ray source and a Si (Li) x-ray spectrometer. The measured values have been compared with those calculated using known values of M and L_3 subshell photoionisation cross sections and fluorescence yields etc., wherever possible. The component of the percentage contribution due to shift of L_3 subshell vacancies to M shell to the total M shell x-ray emission were evaluated and it is seen that the shift of ...

International Nuclear Information System (INIS)

Within the tight binding framework, a study is made of how the disorder affects the electronic properties of A-15 compounds. In particular it is shown that for compounds of two transition metals in the A-15 structure, the vacancy formation affects the density of states only in the low energy region or in the high energy region, in opposition with the isolated chain model of Labbe and Friedel. It is concluded that interchain interactions are important. (U.K.).

International Nuclear Information System (INIS)

A post-irradiation annealing study was conducted with use of reactor pressure vessel(RPV) steel A533B C1.1 base metal irradiated to a dose of 4.84x10"1"8 n/cm"2 at about 380 deg C. Microhardness and positron annihilation (PA) methods were used to obtain better understanding of the recovery of radiation hardening. Isochronal anneal experiments indicated that two recovery processes occur during annealing of irradiated specimens. The first recovery process occurs in the temperature of 280-305 deg C. The variations of Ip, Iw and R parameters indicated that the formation of vacancy clusters by vacancy aggromeration and the annihilation parameters measured indicated that the dissolution of carbon atoms decorated around vacancy-type defects and possible precipitates, and the annihilation of monovacancies give rise to the second recovery process. It was further indicated that radiation anneal hardening (RAH) in the range of 305-405 ...

UK PubMed Central (United Kingdom)

The metabolism of DDT has been followed in pure lines of laboratory-reared resistant and susceptible anophelines using gas-liquid chromatography. Relatively large amounts of DDE were formed in...Full Text Available

UK PubMed Central (United Kingdom)

A fast and sensitive LC-ESI-MS method is described for the comparative quantification of 16 estrogen metabolites based on the derivatization of estrogens with a novel derivatizing reagent, N-methyl-nicotinic...Full Text Available

UK PubMed Central (United Kingdom)

A cholinesterase was partially purified from bush bean (Phaseolus vulgaris L.) roots by using acridinium-based ligand affinity chromatography. The procedure gave a 78-fold increase in specific activity,...Full Text Available

UK PubMed Central (United Kingdom)

This study was conducted to determine by gas chromatography (GC) and mass spectrometry (MS) the identity and the quantity of volatile N products produced during the helium-purged in vivo...Full Text Available

UK PubMed Central (United Kingdom)

Antibodies of the IgM type present in rabbit anti-epiglycanin antiserum were purified by (NH4)2SO4 precipitation and by ion-exchange, affinity and gel-filtration chromatography. After papain treatment...Full Text Available

UK PubMed Central (United Kingdom)

Ion filtration chromatography on diethylaminoethyl-Sephadex A-25 has been used to separate two isozymes each of triose phosphate isomerase, glyceraldehyde 3-phosphate dehydrogenase, glycerate 3-phosphate...Full Text Available

UK PubMed Central (United Kingdom)

A Sepharose-coupled 19S human thyroglobulin has been used as an immunoadsorbent to isolate anti-thyroglobulin autoantibodies and to evaluate the antigen-antibody interactions. With the system proposed...Full Text Available

UK PubMed Central (United Kingdom)

Phenylalanine hydroxylase was purified from crude extracts of human livers which show enzyme activity by usine two different methods: (a) affinity chromatography and (b) immunoprecipitation with an...Full Text Available

UK PubMed Central (United Kingdom)

Attention has shifted from the treatment of colorectal cancer (CRC) to chemoprevention using aspirin and folic acid as agents capable of preventing the onset of colon cancer. However, no sensitive...Full Text Available

UK PubMed Central (United Kingdom)

The aim of the present study was to describe the physicochemical characteristics of streptococcal T antigen. T protein isolated from Streptococcus pyogenes type 12 (R53/1077, Colindale) and purified...Full Text Available

UK PubMed Central (United Kingdom)

In this study we have profiled the free sterol content of cerebrospinal fluid by a combination of charge tagging and liquid chromatography-tandem mass spectrometry. Surprisingly, the most abundant cholesterol...Full Text Available

UK PubMed Central (United Kingdom)

Human IgG specific for beta-endorphin was identified by enzyme-linked immunoabsorbent assay and isolated by affinity chromatography. From a sample of 27 subjects, three individuals with major depression...Full Text Available

UK PubMed Central (United Kingdom)

1. ATP sulphurylase from Saccharomyces cerevisiae was purified 140-fold by using heat treatment, DEAE-cellulose chromatography and Sepharose 6B gel filtration. 2. The enzyme was stable...Full Text Available

Energy Technology Data Exchange (ETDEWEB)

The effects of temperature and the use of macroreticular resins were studied in lithium isotope separation by an ion-exchange method. The isotope separation factors obtained decreased by increasing the temperature, and the factors for macroreticular resins were identical with those for the usual gel-type resins. However, the performance of isotope separation per unit band length in displacement chromatography was found to be improved by increasing the temperature and using macroreticular resins, because accelerating the interphase mass transfer caused the reduction of HETP (Height Equivalent to a Theoretical Plate).

Energy Technology Data Exchange (ETDEWEB)

The relative contributions of interstitials and vacancies to diffusion of a dopant A in silicon are specified by the interstitial fraction of diffusivity, f{sub A}. Accurate knowledge of f{sub A} is required for predictive simulations of Si processing during which the point defect population is perturbed, such as transient enhanced diffusion. While experimental determination of f{sub A} is traditionally based on an underdetermined system of equations, we show here that it is actually possible to derive expressions that give meaningful bounds on f{sub A} without any further assumptions but that of local equilibrium. By employing a pair of dopants under the same point-defect perturbance, and by utilizing perturbances very far from equilibrium, we obtain experimentally f{sub Sb}{le}0.012 and f{sub B}{ge}0.98 at temperatures of {approximately}800{degree}C, which are the strictest bounds reported to date. Our results are in agreement with a theoretical expectation that ...

International Nuclear Information System (INIS)

In this paper, we show that boron transient enhanced diffusion can be reduced to different extents by varying the distribution of nitrogen atoms in the junction. This is attributed to the relative location of nitrogen atoms with respect to boron profile and end-of-range defect band, affecting the interactions between dopants and defects upon annealing. In addition, variations in boron dopant activation and deactivation are also observed. Similar to fluorine co-implantation, it is proposed that nitrogen atoms react with vacancy point defects to form nitrogen-vacancy clusters that will trap the interstitials emitted from end-of-range defects. However, we report that the interstitial sink efficiency of nitrogen atoms is not as good as the co-implanted carbon atoms, which is noticed from the dopant deactivation curves. In terms of extended defect evolution, the results clearly indicate that end-of-range defects can be stabilized by choosing the ...

Energy Technology Data Exchange (ETDEWEB)

We demonstrate that the excess vacancies induced by a 1 MeV Si implant reduce the excess interstitials generated by a 40 keV Si implant during thermal annealing when these two implants are superimposed in silicon. It is shown that this previously observed reduction is dominated by vacancy annihilation and not by gettering to deeper interstitial-type extended defects. Interstitial supersaturations were measured using B doping superlattices (DSL) grown on a silicon-on-insulator (SOI) substrate. Implanting MeV and keV Si ions into the B DSL/SOI structure eliminated the B transient enhanced diffusion normally associated with the keV implant. The buried SiO{sub 2} layer in the SOI substrate isolates the deep interstitials-type extended defects of the MeV implant, thereby eliminating the possibility that these defects getter the interstitial excess induced by the keV Si implant. {copyright} {ital 1999 American Institute of Physics.}

British Library Electronic Table of Contents (United Kingdom)

The alloying effects on K to L shell vacancy transfer probabilities (?KL) in 3d transition metals have been carried out by X-ray fluorescence studies of various alloy compositions. K X-ray intensity ratios of Ti, Cr, Fe, Co, Ni, and Cu elements in the FexNi1?x, FexCr1?x, NixCr1?x, FexCryNi1?(x+y), TixNi1?x, TixCo1?x, and CoxCu1?x alloys have been measured following excitation by 22.69keV X-rays from a 10 mCi 109Cd radioactive point source and ?KL values for alloying elements have been determined from these ratios. The spectrum of characteristic K-X-ray photons from samples were detected with a high resolution Si(Li) detector coupled to a 4 K multichannel analyzer. The present investigation makes it possible to ...

Energy Technology Data Exchange (ETDEWEB)

Depth resolved positron annihilation studies on Pd/Si thin film system have been carried out to investigate silicide phase formation and vacancy defect production induced by thermal annealing. The evolution of defect sensitive S-parameter clearly indicates the presence of divacancy defects across the interface, due to enhanced Si diffusion beyond 870 K consequent to silicide formation. Corroborative glancing incidence X-ray diffraction (GIXRD), Auger electron spectroscopy (AES) and Rutherford backscattering spectrometry (RBS) have elucidated the aspects related to silicide phase formation and Si surface segregation.

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Energy Technology Data Exchange (ETDEWEB)

The electronic structure of the clusters (V/sub 3/Si/sub 4/)/sup 12 -/, (Nb/sub 3/Sn/sub 4/)/sup 12 -/(Mo/sub 3/Ge/sub 4/)/sup 15 -/ in crystalline V/sub 3/Si, Nb/sub 3/Sn, Mo/sub 3/Ge compounds is calculated by the Extended Hueckel method. The influence of different types of radiation induced defects on the density of states at the Fermi level (the anti-site defects, the displacement of atoms in linear chains, the vacancy-interstitial type defects) is considered.

Energy Technology Data Exchange (ETDEWEB)

For the purpose of optimizing the process of co-implantation of MeV Si ions to reduce boron transient enhanced diffusion and boron-enhanced diffusion in Si, multiple MeV implantations and annealing at different temperatures have been performed. A slight improvement on the suppression of B diffusion is observed by adding a low temperature annealing step after the MeV implantation. No differences in B diffusion are observed when the Si doses are increased from 1 x 10{sup 15} to 1 x 10{sup 16} cm{sup -2}. This dose independent behavior is speculated to be a quasi-steady state of vacancy cluster evaporation.

Energy Technology Data Exchange (ETDEWEB)

Fuel cell vehicles have been identified as the personal transportation technology of the future because of their high efficiency and very low emissions. To achieve the goal of road-ready fuel cell vehicles, great strides must be made in the development of fuel cells, hydrogen production and hydrogen storage technologies, that includes metal-H interaction studies and safety considerations. The interaction between two-hydrogen atoms and a {gamma}-Fe structure containing a vacancy has been studied using a cluster model and a theoretical method. For the study of the sequential absorption, the hydrogen atoms were positioned in their energy minima configurations, near the vacancy. The interactions mainly involve Fe 4s-H 1s atomic orbitals. The contribution of Fe 4p and Fe 3d orbitals is much less important. The Fe-Fe bond is weakened as new Fe-H-H and H-H pairs were formed. The effect of H atoms is limited to its first Fe neighbors. The Fe-Fe bond ...

Energy Technology Data Exchange (ETDEWEB)

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.

Energy Technology Data Exchange (ETDEWEB)

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.

Energy Technology Data Exchange (ETDEWEB)

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).

Energy Technology Data Exchange (ETDEWEB)

A hyaluronic acid binding fraction was purified from the supernatant media of both 3T3 and murine sarcoma virus (MSV) transformed 3T3 cultures by hyaluronate and immunoaffinity chromatography. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis resolved the hyaluronate affinity-purified fraction into three major protein bands of estimated molecular weight (M/sub r,e/) 70K, 66K, and 56K which contained hyaluronate binding activity and which were termed hyaluronate binding proteins (HABP). Hyaluronate affinity chromatography combined with immunoaffinity chromatography, using antibody directed against the larger HABP, allowed a 20-fold purification of HABP. Fractions isolated from 3T3 supernatant medium also contained additional binding molecules in the molecular weight range of 20K. This material was present in vanishingly small amounts and was not detected with a silver stain or with (/sup 35/S)methionine label. The ...

Energy Technology Data Exchange (ETDEWEB)

A transient-enhanced diffusion has been observed during the furnace or rapid thermal annealing of ion-implanted silicon. We have studied this transient in detail and show that, for doses of Group V dopants sufficient to amorphize the silicon, it arises from the trapping of interstitials by dopant atoms during implantation. These are retained during solidphase-epitaxial (SPE) growth, but can be released by additional thermal processing to cause the observed transient and the formation of a band of extended defects. We have measured the enhanced diffusion coefficients and the duration of the transient for Sb-implanted Si by careful furnace annealing experiments. We obtain general expressions which predict the effects of the transient during any thermal processing based on SPE growth (furnace, CW laser, or rapid thermal annealing). We show that there is no analogous mechanism of vacancy trapping by Group III elements.

Energy Technology Data Exchange (ETDEWEB)

The group- V vacancy pair, the so-called E-center, has recently been demonstrated to have, both in Si and Ge, more complicated energy-level schemes in the energy gap than were previously assumed. The E-center in silicon has, in addition to its well-established single-acceptor level in the upper half of the band gap, also a donor level in the lower half of the band gap; this donor level has lain hidden for more than 40 years. The E-center in Ge has an even more complicated level scheme as it induces, in addition to two levels analogous to those found in Si, also a double-acceptor level in the upper half of the band gap. Thus the E-center in Si can exist in three charge states and the E-center in Ge in four.

International Nuclear Information System (INIS)

We have investigated the effect of excimer laser annealing (ELA) on transient enhanced diffusion (TED) and activation of boron implanted in Si during subsequent rapid thermal annealing (RTA). It is observed that ELA with partial melting of the implanted region causes reduction of TED in the region that remains solid during ELA, where the diffusion length of boron is reduced by a factor of #approx#4 as compared to the as-implanted sample. This is attributed to several mechanisms such as liquid-state annealing of a fraction of the implantation induced defects, introduction of excess vacancies during ELA, and solid-state annealing of the defects beyond the maximum melting depth by the heat wave propagating into the Si wafer. The ELA pretreatment provides a substantially improved electrical activation of boron during subsequent RTA.

International Nuclear Information System (INIS)

November was a quiet month in Washington. Although Congress has recessed until 1991, the Senate filled vacancies in party leadership positions created by November's elections. The House is expected to proceed with its changes in early December. The Nuclear Energy Forum was held in Washington, DC on November 11-14 to discuss the status of the nuclear industry in the USA. The Forum, held in conjunction with the American Nuclear Society's annual meeting, assembled a large number of CEO's from US, European, and Far Eastern utilities and vendors. The meeting concluded with an announcement by Philip Bayne, President of NYPA and chairman of the Nuclear Power Oversight Committee (NPOC), of the results of a year-long NPOC study entitled a open-quotes Strategic Plan for Building New Nuclear Power Plants.close quotes.

International Nuclear Information System (INIS)

Up to now, P diffusion in Ge is modeled with an effective diffusivity involving at most a quadratic dependence with the free electron concentration (n). However, recent theoretical studies suggest the existence of a triply negatively charged state for the free vacancy in germanium and experimental data indicate that the E center (PV pair) in Ge has a double acceptor state. These two facts would be consistent with a diffusivity model involving a cubic dependence with n. In this paper the validity of this approach is checked for both pure thermal diffusion (intrinsic and extrinsic) and implanted phosphorus, using either our own experiments or other data available from the literature. Although some discrepancies still exist in some cases for the redistribution of implanted P, it is shown that the introduction of this cubic dependence significantly improves the overall agreement as compared with the usual model.

International Nuclear Information System (INIS)

The highest equilibrium free-carrier doping concentration possible in a given material is limited by the ''pinning energy'' which shows a remarkable universal alignment in each class of semiconductors. Our first-principles total energy calculations reveal that equilibrium n -type doping is ultimately limited by the spontaneous formation of close-shell acceptor defects: the 3- -charged cation vacancy in AlN, GaN, InP, and GaAs and the 1- -charged DX center in AlAs, AlP, and GaP. This explains the alignment of the pinning energies and predicts the maximum equilibrium doping levels in different materials. (c) 2000 The American Physical Society

Energy Technology Data Exchange (ETDEWEB)

In the present study, element interdiffusions at the cofired interface of 9/1 Ag/Pd electrode and lead magnesium niobate (PMN)-based ferroelectrics were investigated using Auger Electron Spectroscopy (AES). Intense interdiffusions at the interface were observed while Ag and Pd could penetrate into the ceramics for about 1 {mu}m. Ag-doping experiments were carried out to further study the effects of Ag diffusion on electrical properties of the ceramics. The results showed that Ag could be incorporated into solid solution of the ceramics as Ag{sup +}. As a whole, the Curie temperature (Tc) and dielectric constant of the ceramics decreased with Ag addition. However, Ag addition had no obvious effect on the insulation resistivity. The results inferred that Ag{sup +} could substitute for Pb{sup 2+} at A site of ABO{sub 3} lattice, thereby oxygen vacancies were generated.

Energy Technology Data Exchange (ETDEWEB)

By ab-initio calculation we show that the (Ga,Fe)N ground state may be changed from anti-ferromagnetic to ferromagnetic by acceptor defect like Ga vacancies. The electronic structures are calculated by using the Korringa-Kohn-Rostoker (KKR) method combined with coherent potential approximation (CPA). We show that we can increase the magnetic moment of Fe in p-type GaN by oxygen co-doping. Mechanism of exchange interactions between magnetic ions in p-type (Ga,Fe)N is also studied. The effect of external magnetic field on the electronic structure of (Ga, Fe)N and p-type (Ga, Fe)N is investigated.

Energy Technology Data Exchange (ETDEWEB)

We have investigated the diffusion of Sb in Si in the presence of defects injected by high-energy implantation of Si ions at room temperature. MeV ion implantation increases the concentrations of vacancies, which induce transient-enhanced diffusion of Sb deposited in Si. We observed a significant enhancement of Sb diffusion. Secondary ions mass spectroscopy has been performed on the implanted samples before and after annealing. Rutherford-backscattering spectrometry has been used to characterize the high-energy implantation damage. By fitting diffusion profiles to a linear diffusive model, information about atomic scale diffusion of Sb, i.e. the generation rate of mobile state Sb and its mean migration length were extracted.

Energy Technology Data Exchange (ETDEWEB)

To study the defect creation induced by electronic processes in refractory oxides, MgO single crystals were irradiated with high energy tin, uranium and lead ions. Optical absorption measurements showed that F-type centers (oxygen vacancies with trapped electrons) were created during irradiation. The total number of centers per unit area of bombarded sample increases linearly with irradiating fluence. The main part of the point defects was found to arise from electronic processes. The concentration of F-type centers induced by ionization increases with the electronic energy losses. Assuming a saturation of point defect concentration at high fluences, F-type center creation cross sections could be estimated. The influence of irradiation temperature and of the velocity of the bombarding ions are discussed.

Science.gov (United States)

Herpes simplex virus type-1 (HSV-1) entry into target cell is initiated by the ionic interactions between positively charged viral envelop glycoproteins and a negatively charged cell surface heparan sulfate (HS). This first step involves the induction of HS-rich filopodia-like structures on the cell surface that facilitate viral transport during cell entry. Targeting this initial first step in HSV-1 pathogenesis, we generated different zinc oxide (ZnO) micro-nano structures (MNSs) that were capped with multiple nanoscopic spikes mimicking cell induced filopodia. These MNSs were predicted to target the virus to compete for its binding to cellular HS through their partially negatively charged oxygen vacancies on their nanoscopic spikes, to affect viral entry and subsequent spread. Our results demonstrate that the partially negatively charged ZnO-MNSs efficiently trap the virions via a novel virostatic mechanism rendering them unable to enter into human corneal ...

Science.gov (United States)

The simultaneous diffusion of Si and the dopants B, P, and As has been studied by the use of a multilayer structure of isotopically enriched Si. This structure, consisting of 5 pairs of 120 nm thick natural Si and {sup 28}Si enriched layers, enables the observation of {sup 30}Si self-diffusion from the natural layers into the {sup 28}Si enriched layers, as well as dopant diffusion from an implanted source in an amorphous Si cap layer, via Secondary Ion Mass Spectrometry (SIMS). The dopant diffusion created regions of the multilayer structure that were extrinsic at the diffusion temperatures. In these regions, the Fermi level shift due to the extrinsic condition altered the concentration and charge state of the native defects involved in the diffusion process, which affected the dopant and self-diffusion. The simultaneously recorded diffusion profiles enabled the modeling of the coupled dopant and self-diffusion. From the modeling of the simultaneous diffusion, the dopant diffusion ...

International Nuclear Information System (INIS)

The possibility of the group preconcentration of Zr(4), Hf(4), Nb(5), and Ta(5) countercurrent liquid chromatography using extraction systems based on di-2-ethylhexylphosphoric acid N-benzoyl-N-phenylhydroxylamine, and tetraoctylethylenediamine (TOEDA) is studied. A method have been proposed for the group extraction of Zr(4), Hf(4), Nb(5), and Ta(5) from solution of geological samples. At the stage of the preconcentration of Zr(40, Hf(4), Nb(5) and Ta(5) with a 0.1 M solution of TOEDA in chloroform from mixture of oxalic (0.01 M) and hydrochloric (0.1 M) acids, matrix components are eluted with a flow of the mobile phase, Then, upon changing the eluent (2.0 M HCl), the four elements mentioned above are extracted to a small (7-8 mL) eluate fraction. The results of determining Zr, Hf, Nb, and Ta by inductively coupled plasma atomic emission spectrometry in the international standard reference material Granite GM after their preconcentration in the system with TOEDA ...

International Nuclear Information System (INIS)

The interest for medicinal plants has raised again in the last decades, after overcoming a declination period caused by the advances in the researches and development of the synthetic drugs industries. This growing interest has been stimulated mainly by searching cheap and accessible alternative therapies. However, in order to have natural products based treatment in an efficient and safety way, it is necessary to guarantee the plant authenticity, finding adulterations and to assure a low level of microbiological contaminations to avoid damages to consumer's health. The decontamination method should be chosen for eliminating or reduce the microorganisms level without loss of the plant active constituents that would destroy its therapeutic action. At the present work, the possibility of using #gamma# and X electromagnetic radiations to sterilize a Brazilian medicinal plant (Maytenus aquifolium Martius, Celastraceae), which shows anti-ulcer activity, was studied by accomplishing its ...

Energy Technology Data Exchange (ETDEWEB)

Recently we have found that carbon nano-materials have ability to recognize softer actinides(III). In this presentation, separation of americium(III) from lanthanides(III) by chromatography with carbon nano-materials, such as carbon nano-tubes and graphite, has been investigated by batch adsorption experiments and chromatography. The separation factor (SF) between americium(III) and lanthanide(III) was about 2 in the range of pH from 1 to 4 by using carbon nano-tube, graphite and activated charcoal. The separation factor depended on the diameter of carbon nano-tubes. Smaller one, 3-20 nm diameter, showed the best selectivity for americium(III), which separation factor was about 2.0, although larger one, 40-70 nm, showed almost no selectivity. The same behavior has been observed by using graphite powder and activated charcoal although acid- or alkali pretreated activated charcoal which generally has acidic functional group on the edge of carbon ...

Energy Technology Data Exchange (ETDEWEB)

Trichlorfon is an organophosphorus insecticide, which is extensively being used for protection of fruit crops. Trichlorfon is a thermal labile compound, which cannot be easily determined by gas chromatography (GC) and has no suitable group for sensitive detection by high performance liquid chromatography (HPLC). In this study, a {sup 31}P nuclear magnetic resonance ({sup 31}P NMR) has been described for monitoring of trichlorfon without any separation step. The quantitative works of {sup 31}P NMR spectroscopy has been performed in the presence of an internal standard (hexamethylphosphoramide). Limit of detection (LOD) for this method has been found to be 55 mg L{sup -1}, without any sample preparation, and the linear working range was 150-5500 mg L{sup -1}. Relative standard deviation (R.S.D.%) of the method for three replicates within and between days was obtained {<=}9%. The average recovery efficiency was approximately 99-112%. This ...

Energy Technology Data Exchange (ETDEWEB)

Gas-solid chromatography was used to determine the Henry`s law second gas-solid virial coefficients within the temperature range of 314--615 K for ethane, propane, butane, isobutane, pentane, hexane, heptane, chloromethane, dichloromethane, trichloromethane, tetrachloromethane, trichlorofluoromethane (Freon 11), chlorodifluoromethane (Freon 22), dichlorodifluoromethane (Freon 12), methyl ether, ethyl ether, and sulfur hexafluoride with Carbopack B, a microporous carbon adsorbent. The temperature dependence of the second gas-solid virial coefficients of these adsorbates was used in conjunction with analyses based on a graphical method, a single-surface numeric integration method, a single-surface analytic expression method, and a two-surface analytic expression method to determine the gas-solid interaction energies and other parameters. The interaction energies were correlated with a ratio of the critical temperature divided by the square root of the critical ...

Energy Technology Data Exchange (ETDEWEB)

Chlorine is widely used in drinking water disinfection due to be a powerful and not expense disinfection. Although the benefits of disinfection, the formation of stable disinfection by-products of the health concern, is the result of the interaction of aqueous chlorine with natural organic matter presents in water. Disinfection by-products generated in major concentration are trihalomethane and haloacetic acids. Disinfection by-products generated in minor concentration are haloacetonitriles, haloketones,chloral hydrate and chloropicrin and some new groups such as cyanogen halides and trihaloacetaldydes. In this work two analytical methods.: headspace/gas chromatography/electron capture detector and liquid-liquid microextraction/gas chromatography/electron capture detector are studied and compared to determine the minor by-products and to establish finally, a systematic control of them in the different stages of the Water Treatment Plant of San ...

Science.gov (United States)

An analytical method was developed for the determination of eleven agrochemicals [abamectin (as B1a), bifenazate, bifenthrin, carfentrazone-ethyl, cymoxanil, hexythiazox, imidacloprid, mefenoxam, pymetrozine, quinoxyfen, and trifloxystrobin] in dried hops. The method utilized polymeric and NH2 solid phase extraction (SPE) column cleanups and liquid chromatography with mass spectrometry (LC-MS/MS). Method validation and concurrent recoveries from untreated dried hops ranged from 71 to 126% for all compounds over three levels of fortification (0.10, 1.0, and 10.0 ppm). Commercially grown hop samples collected from several field sites had detectable residues of bifenazate, bifenthrin, hexythiazox, and quinoxyfen. The control sample used was free of contamination below the 0.050 ppm level for all agrochemicals of interest. The limit of quantitation and limit of detection for all compounds were 0.10 and 0.050 ppm, respectively. PMID:18593182

Energy Technology Data Exchange (ETDEWEB)

The automotive paints could be generally differentiated by color, layer sequence and chemistry of the paint layers comprising each of the topcoat and the primer system. The successful identification of hit-and-run a and traffic accidental vehicles from evidential paint fragments is greatly facilitated with a comprehensive laboratory collection of reference paint samples and the technique for direct analysis without sample preparation. The Pyrolysis-Gas Chromatography(PGC) is a precise and reliable method for performing both quantitative and qualitative analysis of polymeric materials and forensic samples. Our Forensic Laboratory is conducting the examination and identification of 73 reference paint samples; 4 colors of each domestic automotive make that is poplar in Korea, by Curie Point Pyrolyzer(JHP-3) and GC with capillary column(ultra alloy-5). This method can be used not only to compare paint traces with their suspected sources, but also to identify the type, ...

International Nuclear Information System (INIS)

An ion chromatograph has been modified to automatically sample ten liquid water streams from the secondary side of three pressurized water reactors, Calvert Cliffs, Unit One, Rancho Seco and McGuire, Unit 1. Sampling and measurement is semicontinuous with a cycle time of approximately five hours for 10 locations with sensitivities in the range of 0.1 to 0.5 ppb. The efficiency of the condensate polishing system and subsequent transport of sodium, chloride, and sulfate around the system can be readily followed. Sulfate has been shown to have unusual volatility into the steam phase from the steam generator as well as a tendency to pass through the condensate polisher.

Energy Technology Data Exchange (ETDEWEB)

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 {sup 200}Pb, {sup 201}Pb, {sup 202m}Pb, and {sup 203}Pb radioisotopes in targets from lead with natural isotopic composition, irradiated by 1-GeV protons.

International Nuclear Information System (INIS)

The following are reported: colorimetric determination of Ti in Cr, decontamination of metals by anodic dissolution, computer code for x-ray peak identification, gel-permeation chromatography of CoRezyn 1664 polyester resin, infrared monitoring of gases and vapors, particle size analysis of dusts, nondestructive analysis of Oralloy for removable alpha contamination, dissolution (digestion) of high-fired oxides, assay of U in a Pu-U alloy, measurement of oxide thickness on Pu metal by x-ray diffraction, analysis of precipitated Pu peroxide, differentiation of Dowex SBR and 11 resins, and determination of Pu solubility in simulated lung fluid.

Energy Technology Data Exchange (ETDEWEB)

The investigation of the petroleum contamination in marine organisms requires the trace level quantitative determination of indicative substances to be identified by a fingerprint of petroleum. Polymethylnaphthalene (PMN) and polymethylphenanthrene (PMP) were chosen because of their simple separation from a crude oil by means of an activated charcoal chromatography, their relatively high existence in aromatic compounds, and their persistence relative to other petroleum components in the tissue of oil contaminated marine organisms. The purpose of this paper is to present an activated charcoal chromatographic separation procedure of PMN and PMP in a crude oil and a trace level quantitative analytical method of them in marine organisms by mass fragmentography (MF).

Science.gov (United States)

A short-chain neurotoxin Pseudechis australis a (toxin Pa a) was isolated from the venom of an Australian elapid snake Pseudechis australis (king brown snake) by sequential chromatography on CM-cellulose, Sephadex G-50 and CM-cellulose columns. Toxin Pa a has an LD50 (intravenous) value of 76 micrograms/kg body wt. in mice and consists of 62 amino acid residues. The amino acid sequence of Pa a shows considerable homology with those of short-chain neurotoxins of elapid snakes, especially of true sea snakes. PMID:4091794

Science.gov (United States)

Results of research programs in coal liquefaction are presented. Areas of research include: desulfurization by bioprocessing; characterization of coal liquefaction processes by XAFS spectroscopy; coprocessing of coal with heavy oil and petroleum residuals; liquefaction research in pyrolysis, catalysis and coal dissolution; novel catalysts; data base development; resource evaluation; depolymerization; solvent extraction and chromatography; correlations of liquefaction yields and coal structure. Individual projects are processed separately for the data bases. (CBS)

International Nuclear Information System (INIS)

The retention of radio-Eu, Go, Cs and Sr, at the tracer level, on raw fibers produced from hemp, linen and Jute plants was investigated. The study was conducted from different media including: sea and tap waters, sodium chloride and nitric acid solutions of different Ph. The percentage retention and elution, on prolonged contact, varied from one element to another depending on conditions. Extraction chromatography columns, using these fibers as supporting material were also experimented. Results were discussed together with possible applications. 7 tabs.

International Nuclear Information System (INIS)

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) "1"2"4I labelled iodaryl azides while minimising manipulation of radioactive materials. Purification of the ["1"2"5I]iodoazido photoaffinity labels is achieved by high performance liquid chromatography. (author).

Science.gov (United States)

The plerocercoid stage of the tapeworm Spirometra mansonoides produces a functional analog of human growth hormone (hGH). Among the similarities between plerocercoid growth factor (PGF) and hGH is competition for the same receptors on rabbit liver membranes. To take advantage of this characteristic in a purification scheme for PGF, rabbit liver microsomes were solubilized in Triton X-100 and the hGH receptors were purified over an hGH affinity column. The purified receptors from six rabbit livers were coupled to Affi-Gel-10 to create a receptor affinity column which was used to purify PGF. Chromatography of crude PGF over the receptor column resulted in a 1044 fold increase in specific activity. SDS-PAGE in the presence of 2-mercaptoethanol showed that the affinity-purified PGF contained three protein bands with apparent Mrs of 27.5 K, 22 K, and 16.7 K. Injections of the partially-purified PGF into hypophysectomized rats produced a dose-dependent growth response ...

International Nuclear Information System (INIS)

Oxide superconducting thin films were irradiated with X-rays and ultra-violet (UV) light, and induced radiation effects on electrical and chemical properties were examined by transport measurement, X-ray diffraction analysis (XRD), diamagnetization measurement and X-ray photoemission spectroscopy (XPS). After irradiation for ErBa_2Cu_3O_x films with X-rays emitted from a Rh tube for 100 hours, superconductivity was remarkably damaged, destroying the zero-resistance state. The UV-light irradiation for Bi_2Sr_2CaCu_2O_x films was performed in He gas of about 500 Pa with a low pressure mercury lamp. The superconductivity was gradually degraded with the UV irradiation time up to 70 minutes. In both cases, adequate oxygen-annealing treatments restored superconductivity. The X-ray photoemission spectra showed that the mean Cu valence of the films was decreased approximately from +2 to +1 by the irradiation. From these results we can find that irradiation with the X-ray and the UV-light ...

Energy Technology Data Exchange (ETDEWEB)

The influence of surface oxides of variable composition and nonstoichiometry formed at high temperatures in air on the general corrosion resistance of ferritic chromium steel type 08H17T (Fe-17Cr-1Ti) in weak sulfuric acid has been studied. Anodic passive films formed on steel with different pretreatments have also been examined. The surface oxide of nearly stoichiometric composition formed at 300 C provides for the passive state of steel in sulfuric acid despite its depletion by chromium when compared with that for nonstoichiometric Cr-enriched oxide formed at 600 C. The dissolution and transformation of nonstoichiometric thermal surface oxide in sulfuric acid appear to take place through defect sites, {minus}Fe{sup 2+} ions, and oxygen vacancies of the n-type conductor. The passive film formed on the nonstoichiometric oxide film, which had been produced at 600 C, was found to be more susceptible to open-circuit breakdown compared to the native oxide and to the ...

International Nuclear Information System (INIS)

Radio frequency (RF) plasma nitriding using different input plasma processing powers (250-600 W) improves the surface of titanium by forming hard phases of TiN, Ti_2N, and Ti (N) into the surface. The characteristics of the compound layer have been investigated by optical microscopy, microhardness measurements, and X-ray diffraction. The effect of plasma power on the sample temperature, electron temperature, and plasma density was studied using Langmuir double probe. The measured surface hardness value of the compound layer is 2190 HV 0.1 for treated sample at plasma power 500 W. The compound thickness continuously increases as the plasma power increases. The highest nitriding rate of 5.88 #mu#m"2/s was recorded when the input plasma power was adjusted at 550 W. This high nitriding rate of treated titanium samples is ascribed to the high concentration of active nitrogen species in the plasma atmosphere and the formed microcracks near to the surface of the sample during the plasma ...

Energy Technology Data Exchange (ETDEWEB)

It has been discovered that the presence of MoO/sub 3/ lowers the ..cap alpha..-..beta.. transition in Sb/sub 2/O/sub 4/ from 935 to 850/sup 0/C with concurrent dissolution of Mo in the high-temperature (..beta..) form. The structure of Mo-doped ..beta..-Sb/sub 2/O/sub 4/ has been investigated by powder neutron diffraction, extended X-ray absorption fine structure (EXAFS) and Raman spectroscopies, and scanning-electron microscopy (SEM). Cell parameters: a = 12.0571 (12) A, b = 4.8335 (1) A, c = 5.3838 (6) A, ..beta.. = 105.579 (5)/sup 0/, monoclinic, space group C2/c, Z = 4. Combining the results of these techniques leads to the hypothesis that Mo is located interstitially within channels of electron density in the Sb/sub 2/O/sub 4/ structure with concurrent vacancy of two Sb/sup III/ atoms. There is no apparent oxygen deficiency in the resulting structure. 25 references, 6 figures, 3 tables.

International Nuclear Information System (INIS)

A set of equations describing a stress-mediated evolution of the nonequilibrium dopant-defect system has been derived and analyzed. Together with coupled diffusion of dopant atoms and point defects, we consider the drift of all mobile species in different charge states, namely vacancies, self-interstitials, and pairs 'dopant atom-point defect', in the field of stress. It has been shown that stresses may affect the diffusion of dopant atoms mainly in two ways: (1) directly, due to the drift of the pairs in the field of stress; (2) indirectly, by the formation of nonuniform defect distribution due to the drift of point defects. On this basis, various features of doping processes, such as phenomena of 'uphill' impurity diffusion near the surface (within the framework of the first or second mechanisms) and the peculiarities of high concentration phosphorus diffusion (due to the second mechanism), can be explained. Numerical computations of high concentration phosphorus ...

International Nuclear Information System (INIS)

Current advanced CMOS source/drain engineering involves the use of amorphizing implants with 3D geometry. Upon annealing, the induced transient enhanced diffusion (TED) can only be accurately predicted if the amorphized region is correctly modeled, as well as the formation and evolution of extended defects, particularly 3 1 1's and dislocation loops. In addition to the extended defects, already modeled in the atomistic kinetic Monte-Carlo simulator DADOS, we have developed a physically based modeling approach for the implant-induced damage build-up, amorphization and recrystallization, suitable to handle device-size process simulation. It is based on amorphous pockets (3D, irregular shape agglomerates of an arbitrary number of interstitials and vacancies, plus trapped impurities) with a size-dependent activation energy for recombination. The model is able to reproduce experimental aspects like the crystal-amorphous transition temperature and the super linear ...

International Nuclear Information System (INIS)

Classification and ranking of the solid solution on their reaction to the irradiation is suggested on the basis of binary system structure controlled by mixing enthalpy sign, melting temperatures relation of components and solidus curves slope. Several combinations of these characteristics permit to pick out three groups of substitutional elements capable of forming the vacancy-solute atom complexes either low-mobile or fast-mobile ones as compared to monovacancies migration. The radiation hardening (and embrittlement) of binary alloys should be intensified respectively either due to heterogeneous point defect clusters nucleation on solute traps or due to solute atom clusters/ precipitate formation. A local cohesion decrease may also occur especially if low-melting elements (characterized by low surface energy) are segregating on internal sinks or grain boundaries. The predicted specifics of different alloy group under irradiation and during post-irradiation ...

International Nuclear Information System (INIS)

In this paper, we report kinetic Monte Carlo study on the diffusion behavior of boron in silicon crystal, more particularly on the transient enhanced diffusion (TED) of boron in silicon during implantation and annealing. Firstly, the accuracy of our KMC code was verified by investigating the time evolutionary behavior of interstitial (I) and vacancy (V) when a silicon substrate is implanted with silicon dose with an energy of 10 keV and with a dose of 1 X 10"1"4 ions/cm"2. To investigate the influence of native defects (I, V) on boron diffusion, a single and multi boron markers grown by MBE were employed. The simulation results revealed that the precursor of boron cluster (BI_2) is dominant at the initial stage of annealing, which explains the boron TED phenomenon in terms of the concentration of boron complexes and I, V clusters, respectively. The formation of #left brace#311#right brace# defects and dislocation loop were observed from the time-evolutionary study ...

Energy Technology Data Exchange (ETDEWEB)

The volume diffusion of Mo in austenitic CrNiMo(N)-steels was studied using the sandwich method. Accordingly the interdiffusion coefficients of Mo were found to be independent of its concentration for the given steel composition with 12 to 19 wt.% Cr, 12 to 16 wt.% Ni, 0 to 2 wt.% Mo and 0 to 0.27 wt.% N and within the temperature range from 1283 to 1523 K. The diffusivity of Mo is greater than that of Cr, Ni and Fe in such steels. The diffusion parameters of Mo are decreased by alloying addition of nearly 0.25 wt.% N in steel; possibly as a result of lattice expansion or increasing vacancy concentration caused by N. Small variations in Cr and Ni initial contents of examined specimens showed negligible effect on the absolut values of interdiffusion coefficients of Mo. (orig.).

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High concentrations of self-interstitials are trapped by dopant atoms during ion implantation into Si. For group V dopants, these complexes are sufficiently stable to survive solid-phase-epitaxial (SPE) growth but break up on subsequent thermal processing and cause a transient-enhanced diffusion. Dopant diffusion coefficients are enhanced by up to five orders of magnitude over tracer values and are characterized by an activation energy of approximately one half of the tracer values. In the case of group III dopants, any complexes formed during implantation do not survive SPE growth but a second source of self-interstitials becomes significant and leads to similar transient effects. This is the damaged layer underlying the original amorphous/crystalline interface. These observations provide direct evidence for long-range self-interstitial migration in Si, and we believe these are the first observations of the interstitialcy diffusion mechanism with no vacancy ...

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Semiconducting properties of passive films formed on AISI 304 stainless steel grade were investigated by capacitances measurements in chloride containing aqueous solutions for different surface finishes: BA (bright annealing in hydrogen containing atmospheres) and 2B (standard annealing in oxidising atmospheres followed by pickling in acid, then water rinsing). Mott-Schottky analysis shows that for high enough electrode potential, and whatever the surface finish, the films behave like n-type semiconductors. 2B passive film appears to be more donor-doped than BA one and the density of donor states increases with chloride concentration. The electron donor levels are assumed to be generated by negatively charged cations vacancies produced by the chloride ions reaction with the outer passive film. This reaction looks easier for 2B than BA condition, which explains why BA resists better than 2B to pit nucleation.

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Microwave dielectric properties and far-infrared reflectivity spectra of (Zr{sub 0.8}Sn{sub 0.2})TiO{sub 4} ceramics with 1.0mol.% Sb{sub 2}O{sub 5} or WO{sub 3} were investigated in the various sintering atmospheres. The Q{center_dot}f value of the specimens sintered in oxygen atmosphere was enhanced due to the decrease of lattice anharmonic interaction resulting from the decrease of oxygen vacancies, whereas the dielectric constants remained constant regardless of sintering atmosphere. The effects of the sintering atmosphere on the changes of ionic and electronic polarization and the intrinsic microwave losses of the specimens were investigated by using the infrared reflectivity spectra from 50 to 4000cm{sup -1}, which were evaluated using Kramers-Kronig analysis and classical oscillator model. The relative tendency of microwave dielectric properties of the specimens calculated from the reflectivity data was in good agreement with the results by the post-resonant ...

International Nuclear Information System (INIS)

Radionuclides exhibiting in decaying a strong interaction between nucleus and electron shell (especially electron capture and internal conversion) are, in principle, sensitive to their chemical surroundings. Consequently, they can be used to yield chemical information after an appropriate labelling procedure. The information can be extracted from the decay rate variation as well as from their X-ray emission as a response to an inner-shell vacancy creation during nuclear deexcitation. As an example of the former method the relationship between the decay rate of /sup 99m/Tc and the chemical structures of pertechnetate and bis(meso-dimercapto-succinate)oxotechnetate(V) is considered. Lower expectations with respect to measuring techniques are associated with the observation of X-ray emission. For a number of elements (especially 3d transition elements) the K/sub #alpha#//K/sub #betta#/ X-ray intensity ratio was found to be an indicator of the nearest neighbour atoms. ...

International Nuclear Information System (INIS)

In support of Stockpile Stewardship activities, accelerated aging tests on a plutonium alloy enriched with 7.3 at.% of "2"3"8Pu is underway using dilatometry at 35, 50, and 65 deg. C and immersion density measurements of materials stored at 50 deg. C. Changes in density are expected from radiation damage in the lattice and helium in-growth. After 25 equivalent years of aging, the dilatometry data shows that the alloys at 35 deg. C have expanded in volume by 0.11-0.12% and have started to exhibit a near linear expansion behavior primarily caused by the helium accumulation. The average He-to-vacancy ratio from tested specimens was determined to be around 2.55. The model for the lattice damage and helium in-growth accurately represents the volume swelling at 35 deg. C. The density converted from the dilatometry corresponds well to the decreasing density trend of reference plutonium alloys as a function of time.

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As semiconductor device dimensions continue to shrink, the drive beyond 250 nm is creating significant problems for the device processor. In particular, trends toward shallower-junctions, lower thermal budgets and simplified processing steps present severe challenges to ion implantation. In parallel with greater control of the implant process goes the need for a better understanding of the physical processes involved during implantation and subsequent activation annealing. For instance, the need for an understanding of dopant-defect interaction is paramount as defects mediate a number of technologically important phenomena such as transient enhanced diffusion and impurity gettering. This paper will outline the current trends in the ion implantation and some of the challenges it faces in the next decade, as described in the semiconductor roadmap. It will highlight some recent positron annihilation work that has made a contribution to addressing one of these challenges, namely the need ...

Science.gov (United States)

The isomerization of neopentane has been investigated over the 0.76 wt% Pd/SiO{sub 2} catalyst. It is found that after high temperature reduction (HTR, at 873 K) the selectivity for isomerization is much higher than that after low temperature reduction (LTR, at 573 K). A variety of experiments, including kinetic, chemisorption (O{sub 2}, H{sub 2}, and CO), temperature-programmed desorption of H{sub 2}, and X-ray diffraction, showed that this selectivity enhancement cannot be interpreted in terms of H{sub 2} retention by catalyst. Instead, the formation of Pd-Si compound(s) (most probably Pd{sub 3}Si) during HTR seems immediately responsible for the catalytic behavior of HTR Pd/SiO{sub 2} catalysts. A mechanism is proposed for the Pd-SiO{sub 2} interaction in which Pd atoms (or ions) are incorporated into the silica support (via oxygen vacancies) and a new phase of palladium silicide is formed. Regeneration by an oxygen treatment of the HTR sample does not fully ...

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A new atomistic approach to Si device process simulation is presented. It is based on a Monte Carlo diffusion code coupled to a binary collision program. Besides diffusion, the simulation includes recombination of vacancies and interstitials, clustering and re-emission from the clusters, and trapping of interstitials. We discuss the simulation of a typical room-temperature implant at 40 keV, 5{times}10{sup 13} cm{sup {minus}2} Si into (001)Si, followed by a high temperature (815{degree}C) anneal. The damage evolves into an excess of interstitials in the form of extended defects and with a total number close to the implanted dose. This result explains the success of the {open_quote}{open_quote}+1{close_quote}{close_quote} model, used to simulate transient diffusion of dopants after ion implantation. It is also in agreement with recent transmission electron microscopy observations of the number of interstitials stored in (311) defects. {copyright} {ital 1996 American ...

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A unified physically based ion implantation damage model has been developed which successfully predicts both the impurity profiles and the damage profiles for a wide range of implant conditions for arsenic, phosphorus, BF{sub 2}, and boron implants into single-crystal silicon. In addition, the amorphous layer thicknesses predicted by this new damage model are also in excellent agreement with experimental measurements. This damage model is based on the physics of point defects in silicon, and explicitly simulates the defect production, diffusion, and their interactions which include interstitial-vacancy recombination, clustering of same type of defects, defect-impurity complex formation, emission of mobile defects from clusters, and surface effects for the first time. New computationally efficient algorithms have been developed to overcome the barrier of the excessive computational requirements. In addition, the new model has been incorporated in the UT-MARLOWE ion ...

British Library Electronic Table of Contents (United Kingdom)

In this study, the influences of cultivar on the phenolic composition and antioxidant properties of 15 different basil varieties was determined. Cultivar had a statistically significant effect on total phenolic levels (p<0.001) and anthocyanin concentrations (p<0.001). Analysis of individual phenolic acid levels by high-performance liquid chromatography showed substantial variations in the phenolic acid profiles among cultivars. Rosmarinic (p<0.001), chicoric (p=0.002) and caffeic (p=0.001) acid concentrations were affected by cultivar, although caftaric acid levels (p=0.083) were not. Nine of the cultivars in this study contained chicoric acid in higher concentrations than rosmarinic acid. These are the first basil cultivars that have been identified in which rosmarinic acid is not the do...

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The use of high-performance ion exchangers allows a trace-matrix-separation (SMT) directly followed by an ion chromatographic (IC) separation of the analytes. Based on the principles described in Part 1, a combined procedure IC-SMT-IC for metallic impurities in Mo and W is presented. Up to 12 metal traces (Fe, Cu, Pb, Zn, Ni, Co, Cd, Ca, Mn, Sr, Mg and Ba) can be determined in one run with 35 min. A special method for traces of U and Th is also given. Detection limits are typically 10-100 ng g{sup -1} in the metal sample. (author). 14 refs.; 10 figs.; 6 tabs.

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The use of microwave in chemistry has known benefits over conventional heating methods, e.g. reduced reaction times, chemical yield improvement and the possibility if reducing or eliminating the use of organic solvents. We describe herein a procedure for the nitration of salicylaldehyde in water using a domestic microwave oven, which can be used as an experiment in the undergraduate chemistry laboratory. The experiment involves safe and rapid preparation and identification of the position isomers by thin layer chromatography and {sup 1}H NMR, or by their melting points. (author)

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When labeled cAMP is incubated with isolated mitochondria from rat liver, it penetrates not only through the outer membrane of the mitochondria but also into the mitoplasts, where it is accumulated chiefly in the matrix. Damage to the mitochondrial membrane by freezing-thawing promotes not an influx but an efflux of cAMP out of the mitoplasts. A substantial part of the labeled nucleotide in all the investigated submitochondrial fractions was identified as intact cAMP by the method of thin-layer chromatography. The transport of cAMP into the mitochondria can explain the activation of their functions by the hormones that activate cytoplasmic adenylate cyclase and by extramitochondrial (cytosol) cAMP, as well as the presence of cAMP-dependent protein kinase and cAMP-phosphodiesterase in the mitochondria.

British Library Electronic Table of Contents (United Kingdom)

Various pyranocoumarins, calophyllolide, inophyllums B, C, G1, G2 and P, from Calophyllum inophyllum (Clusiaceae) leaves of French Polynesia (Austral, Marquesas, Society and Tuamotu archipelagos) have been determined in 136 leaf extracts using a high pressure liquid chromatography-UV-diode array detection (HPLC-UV-DAD) technique. Results show a wide range in chemical composition within trees growing on eighteen islands. The use of multivariate statistical analyses (PCA) shows geographical distribution of inophyllums and indicate those rich in HIV-1 active (+)-inophyllums. Inophyllum B and P contents (0.0-39.0 and 0.0-21.8mgkg-1, respectively) confirm the chemodiversity of this species within the large area of French Polynesia. The study suggests the presence of interesting chemotypes which...

British Library Electronic Table of Contents (United Kingdom)

Abstract:- Increased expression of matrix metalloproteinase (MMP)-2, -3 and -9 has been demonstrated in Crohn-s disease fistulas, but it is unknown whether these enzymes are biologically active and represent a therapeutic target. Therefore, we investigated the proteolytic activity of MMPs in fistula tissue and examined the effect of inhibitors, including clinically available drugs that beside their main action also suppress MMPs. Fistula specimens were obtained by surgical excision from 22 patients with Crohn-s disease and from 10 patients with fistulas resulting from other causes. Colonic endoscopic biopsies from six controls were also included. Total functional MMP activity was measured by a high-pressure liquid chromatography (HPLC)-based, fluorogenic MMP-substrate cleavage assay, and t...

British Library Electronic Table of Contents (United Kingdom)

In order to investigate the antioxidant properties of the polysaccharides from the brown alga Sargassum fusiforme, the crude polysaccharides from S. fusiforme (SFPS) were extracted in hot water, and the lipid peroxidation inhibition assay exhibited that SFPS possessed a potential antioxidant activity. Hence, two purely polymeric fractions, SFPS-1 and SFPS-2 were isolated by the column of DEAE (2-diethylaminoethanol)-Sepharose Fast Flow, with their molecular weights of 51.4 and 30.3 kDa determined by high performance gel permeation chromatography (HPGPC). They were preliminarily characterized using chemical analysis in combination of infrared (IR) and nuclear magnetic resonance (NMR) spectroscopies and found to contain large amounts of uronic acids and ?-glycosidical linkages. The antioxida...

British Library Electronic Table of Contents (United Kingdom)

Background and aimModification of low-density lipoprotein due to oxidative stress is essential in the development of coronary atherosclerosis. Data of specific carotenoids except b-carotene on cardioprotective effects in humans are limited. Methods and resultsThis study examined the associations between plasma concentrations of specific carotenoids and incidence of acute myocardial infarction. The study included 280 incident cases of acute myocardial infarction and 560 matched controls nested within the Singapore Chinese Health Study, a prospective cohort of 63,257 Chinese men and women aged 45-74 years old enrolled in 1993-1998 in Singapore. Retinol and carotenoids in prediagnostic plasma were quantified using high-performance liquid chromatography. High levels of plasma b-cryptoxanthin a...

British Library Electronic Table of Contents (United Kingdom)

Hypertension is one of the most important modifiable risk factors for cardiovascular and cerebrovascular diseases. We investigated the potential antihypertensive effect of the purple passion fruit peel (PFP) extract, a mixture of bioflavonoids, phenolic acids, and anthocyanins, in spontaneously hypertensive rats and human. A high-performance liquid chromatography analysis was performed to identify the active ingredients of the PFP extract. In a rat liver toxicity assay, no hepatotoxicity was observed after 9 hours incubation in the presence of PFP extract (20 ?g/mL). The PFP extract also revealed hepatoprotection against chloroform (1 mmol/L)-induced liver injury. In the experimental model, 24 spontaneously hypertensive rats were divided into 3 treatment groups for a period of 8weeks: cont...

British Library Electronic Table of Contents (United Kingdom)

BACKGROUND AND PURPOSE It is well established that cytochrome P450 2J (CYP2J) enzymes are expressed preferentially in the heart, and that ebastine is a substrate for CYP2J, but it is not known whether ebastine is metabolized in myocardium. Therefore, we investigated its pharmacokinetics in the rat isolated perfused heart. EXPERIMENTAL APPROACH Rat isolated hearts were perfused in the recirculating mode with ebastine for 130-min. The concentrations of ebastine and its metabolites, hydroxyebastine and carebastine, were measured using liquid chromatography with a tandem mass spectrometry. The data were analysed by a compartmental model. The time course of negative inotropic response was linked to ebastine concentration to determine the concentration-effect relationship. KEY RESULTS Ebastine w...

British Library Electronic Table of Contents (United Kingdom)

The results of following the oxidative degradation of a plastic-bonded explosive (PBX 9501) are reported. Into over 1100 sealed containers were placed samples of PBX 9501 and combinations of its components and aged at relatively low temperatures to induce oxidative degradation of the samples. One of the components of the explosive is a poly(ester urethane) polymer and the oxidative degradation of the samples were following by measuring the molecular weight change of the polymer by gel permeation chromatography (coupled with both differential refractive index and multiangle laser light scattering detectors). Multiple temperatures between 40 and 64 degreeC were used to accelerate the aging of the samples. Interesting induction period behavior, along with both molecular weight increasing (cro...

Energy Technology Data Exchange (ETDEWEB)

The concentrations of iron, chromium, zinc, and aluminum were measured by atomic absorption spectroscopy in the lipid-soluble fractions of tar from the process stream of an experimental coal gasifier as part of large study on the health risks of coal gasification. Lipid solubility was inferred from octanol/water-partitioning and benzene-solubility tests. The properties of the lipid-soluble metals were compared to reference compounds by Sephadex LH-20 chromatography. The ability of the lipid-soluble metals to remain lipid soluble after treatment with acid and base was also tested. Lipid-soluble iron, chromium, zinc, and aluminum were present at 360, 12, 3, and 1 ppM, respectively, in the gasifier coal tar. The presence of these metals in lipid-soluble form may have important consequences relative to the potential toxicity of the tar if persons are exposed to it.

International Nuclear Information System (INIS)

Using electrochemical techniques of pH-metry and conductimetry, the choice of a suitable complexing reagent was made amongst ethylene glycol, propylene glycol, dextrose and mannitol for cost-effective separation of isotopes of boron by ion exchange chromatography. Quantitative relationships between pH and concentration; pK_a and concentration of each of these complexing reagents were determined by least square polynomial curve fitting and an attempt was made to determine the formation constants of mannitol-borate complex. The results of experiments carried out for selection; regeneration of a resin; separation factor determinations using batch as well as column techniques and monitoring of band movements using these electrochemical techniques are discussed. (author).

British Library Electronic Table of Contents (United Kingdom)

The effect of four extracts from neem seeds (Azadirachta indica) containing 2000, 5000, 9000 and 10,000ppm of azadirachtin A (AZA), quantified by high-performance liquid chromatography (HPLC) and diluted to 1.25%; 2.5%; 5.0%; 10.0% and 12.8% was verified by in vitro tests with engorged females and larvae of the cattle tick Rhipicephalus microplus. The results from the bioassays with the engorged females showed that the main toxic effect of the extracts was reduction of the reproductive parameters, with a sharp drop in the number of eggs laid and the hatching rate, mainly when the extracts were diluted to 10.0% and 12.8%. The product effectiveness (PE) calculations for all the solutions tested showed that the AZA solution at 10,000ppm (N10) was the most effective. However, statistical analy...

Science.gov (United States)

A practical hands-on course encompassing enzyme purification, biochemical characterization, and crystallization that completed the course work of 350 second-year bachelor students enrolled in molecular biology/biochemistry was given at the Universite Louis Pasteur of Strasbourg (France). The experimental part of the practical dealt entirely with the model protein lysozyme isolated from hen egg-white. It was designed as a research project to give students the possibility to practice biochemical methods such as chromatography, electrophoresis, and spectrophotometry. It also included enzyme activity assay and protein crystal growth that are usually taught in master-level courses. The organization of the practical work and the related experimental procedures are described and discussed.

British Library Electronic Table of Contents (United Kingdom)

The flame retardancy of polybutylene terephthalate (PBT) was studied focusing on the effect of various oxides. Thermo-gravimetric analysis, pyrolysis/gas chromatography/mass spectrometry, and elemental analysis (EA) were used to analyze the flame retardancy, which were observed through the UL-test and a cone calorimeter. Many oxides influenced the flame retardancy and some of them could suppress the flammability of PBT. In particular, the blended-PBTs with ZnO and V2O5 accelerated the degradation and the edges of oxygen consumption were shorter than neat-PBT although the flammability became poorer. The quantitative analysis of the scission products and the results of EA showed that hydrolysis, successive dehydration, and other various reactions changed the scission route to generate less f...

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This article describes the chemical preparation of petroleum additives of the MASK type from samples of concentrated alkylsalicylic acids. The obtained additives contain high contents of calcium alkylsalicylate and respective total alkalinities of 156, 131, and 130 mg KOH/g. Sodium alkylsalicylate concentrates, obtained in the form of an aqueous acetone solution, were converted to alkylsalicylic acids by interaction with hydrochloric acid. The solvent was removed from the upper and lower layers by distillation, and the resulting products were analyzed by liquid chromatography. Service tests were performed on a model formulation of the additive in M-11 oil in a Petter AV-1 test stand unit in comparison with commercial MASK additive. The results indicate that the model additive formulation gives approximately the same corrected piston fouling ratings as the commercial additive.

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...

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)

British Library Electronic Table of Contents (United Kingdom)

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.

British Library Electronic Table of Contents (United Kingdom)

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.).

British Library Electronic Table of Contents (United Kingdom)

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 ...

International Nuclear Information System (INIS)

We present accurate tight-binding parametrizations of the first-principles augmented-plane-wave or linear-augmented-plane-wave band structures of LaCuO_3, La_2CuO_4, Ba_2CuO_4, and the high-temperature superconductor YBa_2Cu_3O_7. We discuss the methodology and efficient application of these fits, including as an example our tight-binding coherent-potential-approximation (CPA) calculations of the effects of disorder on the electronic structure of La/sub 2-//sub x/Ba/sub x/CuO/sub 4-//sub y/. Our CPA calculations support the hypothesis of a rigid-band lowering of the Fermi level for La/sub 2-//sub x/Ba/sub x/CuO_4, enhancing the density of states there. However, for La_2BaCuO/sub 4-//sub y/ they yield the interesting result that oxygen vacancies also lower E/sub F/ and raise N(E/sub F/). This is a significant result for the theory of superconductivity in these materials. In addition to CPA calculations, our parametrizations of the band structures should prove to be ...

International Nuclear Information System (INIS)

In this paper we discuss the results of thermoluminescence (TL) studies carried out on freshly quenched crystals of KBr doped with #approx# 50 ppm of Eu"2"+ ions which were X-irradiated at room temperature. The TL glow curve of this phosphor material consists of three glow peaks at 355, 376 and 398 K whose intensities increased as a function of X-irradiation time. The TL glow peaks were analyzed by the total curve-fitting method in order to obtain the characteristic parameters; activation energy, pre-exponential factor and kinetic order. The spectral character of the emission recorded during thermoluminescence was found to be the same for all glow peaks and consists of a broad band centered at #approx# 420 nm. It is proposed that the model of the TL process most consistent with our experimental results is one in which the Eu"2"+ impurity acts as an electron trap during the irradiation process and that the radiation induced center (partner of an center) and the V_k center (partner of an ...

International Nuclear Information System (INIS)

The hardening and embrittlement of reactor pressure vessel (RPV) steels is of great concern in the actual nuclear power plant life assessment. This embrittlement is caused by irradiation-induced damage, like vacancies, interstitials, solutes and their clusters. The current procedure to estimate material properties for the irradiated pressure vessels is based on Charpy-V tests of identical material located at the inner shell of the reactor. But the reason for the embrittlement of the materials is not yet totally known. The real nature of the irradiation damage should thus be examined as well as its evolution in time. Fe-Cu binary alloys are often used to mimic the behaviour of such steels. Their study allows. Identifying some of the defects responsible of the hardening, especially when compared to pure iron or C-micro-alloyed iron. More recently the influence of manganese and nickel in low-Cu RPV steels has become a significant topic. Thus in contrast with the ...

Energy Technology Data Exchange (ETDEWEB)

Point-contact (PC) investigations on the title compound in the normal and superconducting (SC) state (T{sub c}{approx_equal}10.6 K) are presented. The T-dependence of two SC gaps in TmNi{sub 2}B{sub 2}C determined by Andreev-reflection spectroscopy deviates from the BCS behavior in displaying a maximum at about T{sub c}/2. Additional evidence for the presence of a 2nd gap half as large as the main gap is given. For the first time ''reentrant'' features were found in the Andreev-reflection spectra measured in magnetic fields. The PC spectroscopy of the fermion-boson interaction in TmNi{sub 2}B{sub 2}C reveals a pronounced phonon maximum at 9.5 meV and a more smeared one around 15 meV, while at higher energies the PC spectra are almost featureless. Additionally, the intense peak slightly above 3 meV observed in the PC spectra of TmNi{sub 2}B{sub 2}C, is presumably caused by crystalline-electric-field excitations. The peak near 1 meV detected for some ...

Energy Technology Data Exchange (ETDEWEB)

In order to understand the chemistry of altermetal dopants in antimony oxide, the detailed structural characterization of two ..beta..-Sb/sub 2/O/sub 4/ compounds is reported, Mo-doped ..beta..-Sb/sub 2/O/sub 4/ (1.5 metal%) and V-doped ..beta..-Sb/sub 2/O/sub 4/ (5 metal%). The methods used to characterize these materials are X-ray and neutron diffraction, scanning electron microscopy, Mo K-edge extended X-ray absorption fine structure spectroscopy, and elemental analysis. The atomic position of each of these dopants in Sb/sub 2/O/sub 4/ is radically different as is the overall effect on the host structure. Molybdenum does not substitute for Sb atoms, rather the Mo atoms are found in channels of electron density formed by Sb/sup 3 +/ lone pairs. The two nearest Sb/sup 3 +/ are absent and the oxygen stoichiometry is preserved. The formula is Sb/sub 1.97/Mo/sub 0.015/O/sub 4/. Vanadium incorporates substitutionally for the Sb/sup 3 +/ atoms and there are random oxygen ...

Energy Technology Data Exchange (ETDEWEB)

Lithium-ion batteries are becoming more and more important not only for portable electronic devices, but also in prevision of high power electric vehicles. In such an optic, deep studies regarding all the components of a secondary battery are in development. In this study, high voltage cathode materials have been selected. Crystals with spinel structure have a 3D vacancy pathway suitable for Li-ions transport. The material under study was LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} doped with magnesium replacing the nickel. Various samples were synthesized via three different routes: a solid-state method, a modified sol-gel method and a xerogel method. The structure and morphology of the powders were analyzed with HRTEM and XRD. Electrochemical tests were also performed. A wide range of particle sizes (from micro to nanosize) was the result of the different synthesis routes. Unfortunately pure materials were not always obtained. The electrochemical tests showed improvement of ...

Energy Technology Data Exchange (ETDEWEB)

The effect that different chemical and physical atomic environments can have on the relative intensities of radiative electron transitions from the filling of K shell vacancies was investigated. The method used involved the detection of photoionization induced X-ray fluorescence. An experimental system based on a hyper pure germanium detector (HPGE) was used to measure the relative K-L and K-M X-ray yields from the photofluorescence of a series of lanthanide elements and compounds. A background subtraction and peak integration strategy was employed which accounted for scattering in the samples and scattering of the flux from the radioisotope photoionization sources. Analysis of the data resulted in a tabulation of relative K/sub ..beta..//K/sub ..cap alpha../ X-ray intensity ratios. The measured relative K/sub ..beta..//K/sub ..cap alpha../ X-ray intensity ratios were compared to the calculated values predicted by the theoretical development of Scofield and the ...

Energy Technology Data Exchange (ETDEWEB)

Single crystals of trigonal Cr{sub 2}Te{sub 3}, monoclinic Cr{sub 5}Te{sub 8}, and trigonal Cr{sub 5}Te{sub 8} were prepared and the single crystal structures were determined. The structures are related to the NiAs structure type by successive removal of Cr in every second metal atom layer parallel to the c axis. The strong relationship between the structures is evidenced by their very similar X-ray powder patterns. In trigonal Cr{sub 2}Te{sub 3} excess Cr occupies only one of the two possible sites. In monoclinic Cr{sub 5}Te{sub 8} the Cr atoms occupy four different crystallographic sites. The resulting ordering of the vacancies is significantly different from the hitherto reported crystal structures of transition metal chalcogenides M{sub 5}X{sub 8}. A slight increase of the tellurium content leads to an order-disorder transition from the monoclinic to a trigonal phase. The Cr atoms are located on four crystallographically different sites leading to the formation ...

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 ...

Energy Technology Data Exchange (ETDEWEB)

The phenomenology of wire chamber aging is discussed and fundamentals of proportional counters are presented. Free-radical polymerization and plasma polymerization are discussed. The chemistry of wire aging is reviewed. Similarities between wire chamber plasma (>1 atm dc-discharge) and low-pressure rf-discharge plasmas, which have been more widely studied, are suggested. Construction and use of a system to allow study of the plasma reactions occurring in wire chambers is reported. A proportional tube irradiated by an {sup 55}Fe source is used as a model wire chamber. Condensable species in the proportional tube effluent are concentrated in a cryotrap and analyzed by gas chromatography/mass spectrometry. Several different wire chamber gases (methane, argon/methane, ethane, argon/ethane, propane, argon/isobutane) are tested and their reaction products qualitatively identified. For all gases tested except those containing methane, use of hygroscopic filters to ...

Energy Technology Data Exchange (ETDEWEB)

A multifunctional protein kinase, purified from rat liver as ATP-citrate lyase kinase, has been identified as a glycogen synthase kinase. This kinase catalyzed incorporation of up to 1.5 mol of and)2numberSPO4/mol of synthase subunit associated with a decrease in the glycogen synthase activity ratio from 0.85 to a value of 0.15. Approximately 65-70% of the TUPO4 was incorporated into site 3 and 30-35% into site 2 as determined by reverse phase high performance liquid chromatography. This multifunctional kinase was distinguished from glycogen synthase kinase-3 on the basis of nucleotide and protein substrate specificities. Since the phosphate contents in glycogen synthase of sites 3 and 2 are altered in diabetes and by insulin administration, the possible involvement of the multifunctional kinase was explored. Glycogen synthase purified from diabetic rabbits was phosphorylated in vitro by this multifunctional kinase at only 10% of the rate compared to synthase ...

Energy Technology Data Exchange (ETDEWEB)

The mixture of lauric acid and capric acid is a potential latent heat storage material. However, its eutectic melting temperature is quite high for low-temperature thermal energy storage. Addition of naphthalene is proposed. The ternary system lauric acid-capric acid-naphthalene has been investigated by differential scanning calorimetry (DSC), visual polythermal and chromatography of gases. The phase diagram is of an incongruent eutectic type. The eutectic mixture contains 18.4mol% lauric acid, 63.1mol% capric acid and 18.5mol% naphthalene and melts at 13.3{sup o}C. The peritectic mixture contains 32.4mol% lauric acid, 48.2mol% capric acid and 19.4mol% naphthalene and peritectic temperature of 16.2{sup o}C. The incongruent compound was analysed to be CH{sub 3}(CH{sub 2}){sub 10}COOH.CH{sub 3}(CH{sub 2}){sub 8}COOH. The melting temperature of the lauric acid-capric acid-naphthalene eutectic mixture makes it suitable for cooling applications.

Energy Technology Data Exchange (ETDEWEB)

The lipid obtained by the toluene extraction of a dried raw Atlanta sewage sludge by the Soxhlet method, was pyrolyzed over activated alumina at atmospheric pressure. A range of weight hourly space velocities (WHSV) from 0.22-1.60/h and a range of temperatures from 400-480[degree]C were selected. A 70 wt % yield of light liquid hydrocarbons was obtained at a WHSV of 0.46/h and 450[degree]C. The sulfur and nitrogen contents of the pyrolysis products were much lower than products from direct liquefaction of sludge. Infrared spectra and [sup 13]C nuclear magnetic resonance confirmed the absence of carbonyl groups in the products. Gas chromatography showed a uniform hydrocarbon chain length distribution across the C[sub 7] to C[sub 17] mass range. The gas product consisted mainly of carbon dioxide and hydrocarbons. Lauric acid was used as a model to study the decarboxylation. The effects of catalyst loading and catalyst moisture content were investigated for the ...

British Library Electronic Table of Contents (United Kingdom)

We describe a method for the analysis of multi-site phosphorylation in serine/threonine (Ser/Thr)-rich protein sequences. Site-specific mutagenesis was used to introduce tryptic cleavage sites in the serine glutamine/threonine glutamine cluster domain (SCD) of the human checkpoint protein kinase (Chk2). The mutant proteins were shown to autophosphorylate on residues that are inducibly phosphorylated when mammalian cells are exposed to ionizing radiation (serine 33/35, serine 516, threonine 68 and threonine 432). Five Ser/Thr clusters within the SCD were flanked by arginine or lysine residues to produce tryptic peptides for nanospray liquid chromatography (nanoLC)/linear quadrupole ion trap Fourier transform ion cyclotron resonance mass spectrometry. Phosphorylation sites were assigned usin...

Energy Technology Data Exchange (ETDEWEB)

Functionalization of carbon nanotubes is very challenging for their applications. The paper here describes a new method to functionalize multi-walled carbon nanotubes (MWCNTs) as specific affinity adsorbents. MWCNTs were acid purified and pretreated with (3-aminopropyl)-triethoxysilane (APTES) in order to introduce abundant amino groups on the surface of MWCNTs. After the conversion of amino groups to carboxyl groups by succinic acid anhydride, MWCNTs were attached to protein A or aminodextran using 1-ethyl-3,3' (dimethylamion)-propylcarbodiimide as a biofunctional crosslinker. The incorporation of aminodextran as a spacer arm noticeably increased the binding capacity of the APTES-modified MWCNTs for protein A. The application of affinity MWCNTs for purification of immunoglobulin G was then evaluated. The affinity of MWCNTs with AMD spacer exhibited a high adsorption capacity of {approx}361 {mu}g IgG/mg MWCNT (wet basis). About 75% of bound IgG was eluted from affinity MWCNTs ...

Science.gov (United States)

Chlorinated organics are frequently found as harmful soil contaminants and persisted for extended periods of time. A novel approach, named pulsed corona discharge plasma (PCDP), was employed for the degradation of pentachlorophenol (PCP) in soil. Experimental results showed that 87% of PCP could be smoothly removed in 60 min. Increasing pulse voltage, enhancing soil pH, lowering humic acid (HA) in soil and reducing granular size of the soil were found to be favorable for PCP degradation efficiency. Oxidation and physical processes simultaneously contributed to PCP removal in soil and ozone was the main factor in PCDP treatment. C-Cl bonds in PCP were cleaved during PCDP treatment by Fourier transform infrared spectroscopy (FTIR) analysis. The mineralization of PCP was confirmed by total organic carbon (TOC) and dechlorination analyses. The main intermediate products such as tetrachlorocatechol, tetrachlorohydroquinone, acetic acid, formic acid, and oxalic acid were identified by ...

International Nuclear Information System (INIS)

The objective this work was to evaluate the gamma radiation processing for elimination of organic contaminants on industrial wastewater. Standard samples with 17 hydrocarbons (acetophenone, anisole, benzene, chlorobenzene, cyclohexanone, N, N-dimethylaniline, phenol, naphtalene, 1-chloronaphtalene, n-octadecane, p-nitrotoluene, toluene, tetrachloroethane, tetramethylbenzene, n-undecane, m-xylene and o-xylene) was preparated in hexane with total concentration of 1 #mu# g/ #mu# l which was analyzed by gas chromatography. Other sample with the same concentration of these hydrocarbons in acetone was used to contaminate water samples, which were irradiated with gamma radiation from Co-60 between doses 5.0 to 20.0 KGy and dose rate of 1.162 KGy/h. The activity of source was 1470 Ci. Percents destruction of hydrocarbons were: 79.76 % to 5.0 KGy, 85.97 % to 7.5 KGy, 86.24 % to 10.0 KGy, 86.72 % to 12.5 KGy, 88.92 % to 15.0 KGy, 91.74 % to 17.5 KGy and 92.38 % to 20.0 KGy. ...

International Nuclear Information System (INIS)

Volatile compounds produced in flexible food packaging materials (LDPE, EVAc, PET/PE/EVOH/PE) during electron beam irradiation were isolated by purge and trap technique and identified by combined gas chromatography-mass spectrometry (GC/MS), after thermal desorption and concentration. For comparison purposes non-irradiated films were also studied. Film samples were irradiated at low (5 kGy, corresponding to cold pasteurization), intermediate (20 kGy, corresponding to cold sterilization) and high (100 kGy) doses. It was observed that a number of volatile compounds are produced after irradiation in all cases. Furthermore the amounts of all volatile compounds increase with increasing irradiation dose. Both primary (methyl-derivatives etc.) as well as secondary i.e. oxidation products (ketones, aldehydes, alcohols, carboxylic acids etc.) are produced upon irradiation. These products may affect organoleptic properties and thus shelf-life of prepackaged irradiated foods. ...

Science.gov (United States)

The enantiomeric separations of three pesticides fipronil (asymmetric nitrogen), isocarbophos (asymmetric phosphorus) and carfentrazone-ethyl (asymmetric carbon) were studied on cellulose-tri(3,5-dimethylphenylcarbamate) chiral stationary phase using high-performance liquid chromatography under normal phase. The mobile phase was n-hexane with alcohols including ethanol, n-propanol, iso-propanol, n-butanol and iso-butanol as polar modifiers. The flow rate was 1.0 mL/min with UV detection at 280, 225 and 230 nm for fipronil, isocarbophos and carfentrazone-ethyl respectively. The influence of the modifiers and their volume content and temperature from 0 to 50 degrees C on the separations was investigated. The chiral stationary phase showed excellent stereoselectivity for the two enantiomers of fipronil and isocarbophos and certain chiral recognition for carfentrazone-ethyl. Iso-propanol was more suitable for the chiral separation of isocarbophos and ...

Energy Technology Data Exchange (ETDEWEB)

The values of -{delta}G{sub A}{sup O} of n-alkanes on calcite are lower on the stearic acid treated calcite than on the untreated calcite. The value of -{delta}G{sub A}{sup O} of n-alkanes on calcite increase with increasing carbon numbers of n-alkanes. The values of -{delta}G{sub A}{sup O} measured on the treated calcite are significantly lower than those measured on the untreated calcite. The -{delta}G{sub A}{sup O} of n-alkanes on the treated calcite are close to the heat of liquefaction of n-alkanes. All the experimental values of -{delta}G{sub A}{sup O} of n-alkanes on calcite are larger than theoretical entropy decrease particularly for the higher molecular mass n-alkanes. Thus the important entropy decrease observed upon adsorption can not only be attributed to the loss of one degree of freedom of the adsorbed molecules. The values of {gamma}{sub S}{sup D} of the treated and untreated calcite decrease with increasing temperature. {gamma}{sub S}{sup D} for the treated calcite is ...

International Nuclear Information System (INIS)

An assay for the microsomal hydroxylation of lauric acid (LA), based on HPLC with flow-through radiochemical detection, has been developed. Conditions were optimized for resolution and quantitation of three microsomal metabolites of "1"4C-LA, one of which has not been reported previously as a metabolite of LA in mammalian microsomal incubations. These products, 12-(omega)-hydroxy-LA, 11-(omega-1)-hydroxy-LA, and a novel metabolite, 10-(omega-2)-hydroxy-LA, were isolated by HPLC and identified by gas chromatography/mass spectrometry. In the presence of NADPH, the formation of all three metabolites was linear with time and microsomal protein concentration. Hydrogen peroxide also supported the microsomal metabolism of LA, although the ratio of metabolites was substantially different than that produced by NADPH-supported microsomes. Several biochemical probes (metyrapone, #alpha#-naphthoflavone, 2-diethylaminoethyl-2,2-diphenylvalerate hydrochloride, and 10-undecynoic ...

Energy Technology Data Exchange (ETDEWEB)

The effect of combustion conditions on conversion of char nitrogen to N2 was studied in the combustion experiment of char obtained by pyrolysis of coal. Char specimen was prepared by holding ZN coal of Chinese lignite in Ar atmosphere at 1123K for one hour. A batch scale quartz-made fluidized bed reactor was used for combustion experiment. After the specimen was fluidized in reaction gas, it was rapidly heated to start combustion reaction. CO, CO2 and N2 in produced gases were online measured by gas chromatography (GC). As the experimental result, under the incomplete combustion condition where a large amount of CO was produced by consuming almost all of O2, no NOx and N2O produced from char were found, and almost all of N-containing gas was N2. At the final stage of combustion, pyridinic-N disappeared completely, and pyrrolic-N decreased, while O-containing nitrogen complexes became a main component. It was thus suggested that O-containing nitrogen complexes are ...

Energy Technology Data Exchange (ETDEWEB)

An in situ synthesis of ZnS and CdS quantum dots (QDs) in an aqueous solution of sodium hyaluronate (Hyal) produced foils emitting light on excitation with a UV light. The wavelength of emission was only slightly QDs size and more QDs concentration dependent and reached up to {approx}320 nm in the case of ZnS and {approx}400-450 nm in the case of CdS. Nanoparticles remained as non-agglomerated 10-20 nm nanoclusters. CdS/Hyal and ZnS/Hyal-QDs biocomposites were characterized using photoluminescence (PL), IR spectrometric techniques, and Transmission Electron Microscopy (TEM). The absolute molecular weights, radii of gyration, R{sub g}, and thermodynamic properties of the obtained foils are given. Electric resistivity studies performed for the hyaluronic foil in the 100-1000 V range have revealed that the hyaluronate foil has very weak conducting properties and QDs only insignificantly affect those properties as QDs practically did not interact with the foil. Size exclusion ...

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The ruptured offshore oil well 80 miles from Mexican town of Ciudad del Carmen, which poured 8000 barrels of light oil a day into the Gulf of Mexico, provided marine scientists with the opportunity to monitor the spill and see what happens to petroleum hydrocarbons in sea water. Scientists followed changes in viscosity, surface tension, and buoyancy of individual oil globs as they moved through the water and interacted with the surface slick. Using gas chromatography and mass spectroscopy, chemists are gaining an understanding of the unique characteristics of the oil. Computer-generated models projected the slick's movement in the Gulf in response to wind and wave pressures, but the sophisticated system did not give an accurate daily prediction. Immediate damage to fish, turtles, and sea birds was documented by tagging. Long-term effects will take longer to ascertain since 25 years is generally required to flush oil out of sediments. Fishermen do not agree ...

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This study was undertaken to determine if a combined treatment (marinating in natural plant extracts or vacuum) with irradiation could have a synergistic effect, in order to prevent the lipid oxidation resulting in the development of undesirable flavours. The fresh chicken legs were irradiated at 0,3 and 5 kGy. The fatty acids composition of lipids was identified using gas liquid chromatography. The effect of irradiation treatment combined with a pre-treatment on the fatty acids composition was followed. The day after irradiation, ten panallists were asked to evaluate, using the instruction scaling, the overall appearance, the odor, the flavor and the overall acceptability of the samples. The major fatty acids identified in lipids were oleic acid, palmitic acid, palmitoleic acid and stearic acid. Pre-treatments have a significant effect on linoleic acid (C18:2) and higher fatty acids. The unsaturated fatty acids derived from phospholipids appeared to be more ...

Science.gov (United States)

We describe a method for affinity purification of sequence-specific DNA binding proteins that is fast and effective. Complementary chemically synthesized oligodeoxynucleotides that contain a recognition site for a sequence-specific DNA binding protein are annealed and ligated to give oligomers. This DNA is then covalently coupled to Sepharose CL-2B with cyanogen bromide to yield the affinity resin. A partially purified protein fraction is combined with competitor DNA and subsequently passed through the DNA-Sepharose resin. The desired sequence-specific DNA binding protein is purified because it preferentially binds to the recognition sites in the affinity resin rather than to the nonspecific competitor DNA in solution. For example, a protein fraction that is enriched for transcription factor Sp1 can be further purified 500- to 1000-fold by two sequential affinity chromatography steps to give Sp1 of an estimated 90% homogeneity with 30% yield. In addition, the use ...

British Library Electronic Table of Contents (United Kingdom)

This paper presents a comprehensive study of pesticide levels and bio-accumulation characteristics in human adipose tissues among residents of Southeast China. A large number of adipose samples (n=633) were selected for 58 pesticides and were analyzed by high sensitive Gas Chromatography-Tandem Mass Spectrometry (GC-MS/MS). The results showed that POPs pesticides were frequently detected, including 2,4prime-DDD, 2,4prime-DDE, 2,4prime-DDT, 4,4prime-DDD, 4,4prime-DDE, 4,4prime-DDT, a-HCH, b-HCH, g-HCH, d-HCH, hexachlorobenzene (HCB), and mirex. Other detected pesticide species were dicofol, methamidophos and chlordimeform, which have rarely been reported. Comparing to different countries, the concentrations of total DDT and HCH in these three Chinese southeastern sites were in the middle ra...

International Nuclear Information System (INIS)

Paper describes a new procedure to synthesize a pharmaceutical containing "2"1"1At. "2"1"1At"- anion was found to bind strongly with Rh"3"+ cation complexing with a thio-ether ligand - 1,5,9,13-tetratiacyclohexadecane-3,11-diol (16-S4-diol). One made use of "1"3"1I isotope to seek for the optimal conditions of the reaction. The derived complexes were studied by means of the paper electrophoresis, the ion exchange, the surface chromatography. One studied the kinetics of "1"3"1I"- anion binding with Rh(16-S4-diol), the dependence of the yield of "1"3"1I-Rh(16-S4-diol) forming complex on the temperature. the acidity of the reaction mixture and the concentration of the reagents. On the basis of the determined conditions of the synthesis one prepared "2"1"1At-Rh(16-S4-diol) complex by more astatide ("2"1"1At"-) to the equivalent amounts of RhCl_3 and tetra-thio-ether (16-S4-diol). One studied its behaviour

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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 ...