A heterobifunctional reagent, N-succinimidyl 3-(2-pyridyldithio)propionate, was synthesized. Its N-hydroxysuccinimide ester group reacts with amino groups and the 2-pyridyl disulphide structure reacts...Full Text Available
Nucleoside 3'-phosphoramidite and chlorophosphite reagents have been found to react with the lactam function of guanine. This reaction caused unsatisfactory results when oligodeoxyribonucleotides containing...Full Text Available
The effects of thiol-specific reagents on the amplitude of the electro-olfactogram (E.O.G.) responses elicited from frog olfactory mucosa by pulses of odorant vapours was studied. The impermeant thiol-specific...Full Text Available
The adsorption interaction of different types of demulsifiers and the oils of Western Siberia is covered. The high adsorption capacity of Separol-5084 and disolvan-4490 reagents is established. The positive role of this phenomen in breaking aqueous oil emulsifiers is theoretically substantiated and experimentally confined.
Samples of geothermal scale formed from Magmamax No. 1 and Woolsey No. 1 wells in the Imperial Valley, Calif., were exposed to concentrated and dilute solutions of common laboratory reagents. The time of exposure and temperature of the reagent were also varied. Several reagents easily dissolved significant amounts of the scale. An in situ test was performed with marginal success.
The need for material standards in the field of clinical immunology, together with the mode of operation of the combined World Health Organization/International Union of Immunological Societies programme...Full Text Available
Hydrophobic labelling is frequently used in the study of membrane-inserted domains of intrinsic proteins. However, the published procedures, fail to incorporate sufficient radioactivity into membrane immunoglobulins of B lymhocytes to permit investigation of their subunit structures and associations with other proteins. In order to increase the specific radioactivity of ["1"2"5I]iodonaphtylazide ["1"2"5I]INA), an improved method for the synthesis of the reagent was developed. In addition, the optimal conditions for labelling B lymhpocytes with ["1"2"5I]INA and commercially available reagent 3-(trifluoromethyl)-3-(trifluoromethyl)-3-(3'-["1"2"5Iliodophenyl)diazirine (["1"2"5I]TID were isolated and analysed in detail by SDS-PAGE. The usefulness of the two reagents for the investigation of lipid-embedded domains of membrane proteins is discussed. (author). 28 refs.; 4 figs.
The goal of the invention is to increase the effectiveness of the isolation process through increasing the waterproofing of the stratum. The cited goal is achieved by isolating water influx into a well through introduction of a chemical reagent into the stratum. To interact with the stratum, an alloy of titanium and iron is introduced into the stratum as the chemical reagent with subsequent pumping of hydrogen into the stratum at 100 to 200C.
A new reagent 7-(6-Br-2-henzthiazolilazo)-8-oxyquinoline-5-sulphoacid has been studied spectrophotometrically. Dissociation constants have been determined in 50% acetone (pK_1=2.5 and pK_2=5.9) and 50% dioxane (pK_1=1.7 and pK_2=6.1) as well as molar extinction coefficients of the reagent dissociated form in the same solvents (71.1.10"3 and 72.4.10"3). The conditions have been studied of complexing the reagent with ions of uranium (6), zinc (2), and manganese (2) in 50% dioxane (pH 2.5-4.5) and the properties of the formed complexes.
Amidination of aldolase, glyceraldehyde-3-phosphate dehydrogenase, tryptophan synthetase B protein, L-arabinose isomerase, and the catalytic subunit of E. coli aspartate transcarbamylase...Full Text Available
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
Beta silicon carbide is an excellent candidate semiconductor material for demanding applications in high power and high temperature electronic devices due to its high breakdown voltage, relatively large band gap, high thermal conductivity and high melting...
Phosphoramidite reagents can phosphitylate guanine bases at the O6-position during solid phase synthesis and serious chain cleavage occurs if the base phosphitylation is not eliminated before the iodine/water...Full Text Available
The report gives results of the measurement of dissolution rates of reagent CaCO3 and commercial limestones (9 types/19 grinds) at constant pH and solution composition by batch titration with HC1. Conditions were selected to simulate flue gas desulfurizat...
The asymmetric organocatalytic α-sulfenylation of substituted piperazine-2,5-diones is reported, with cinchona alkaloids as chiral Lewis bases and electrophilic sulfur transfer reagents....Full Text Available
Trypanothione reductase (TryR) is a key enzyme involved in the oxidative stress management of the Trypanosoma and Leishmania parasites, which helps to maintain an intracellular reducing environment...Full Text Available
The passage of a vascular-injected paramagnetic contrast reagent (CR) bolus through a region-of-interest affects tissue 1H2O relaxation and thus MR image intensity. For longitudinal...Full Text Available
The French strategy of high level radioactive aqueous waste management is an incorporation in glassy fission products containers. Therefore, nitric acid soluble organic reagents needed for minor actinides and lanthanides selective separation from fission product solutions have to be sufficiently removed to reach carbon concentrations compatible with calcinator working. Thus, the ability of reagents to be oxidized under concentration conditions with or without denitration becomes a criteria of selection and have been studied. Further, if not working, other operations like hot hydrogen peroxide oxidation, catalyzed or not, are investigated. Reagents involved in this work are mainly complexing products (N-(2-Hydroxyethyl) Ethylene-diamine-tri-acetic Acid), pH keeping reagents (carboxylic acids like citric, glycolic, tartaric and lactic acid) and alkaline species (Tetramethylammonium hydroxide). Behaviour ...
1. An acid ninhydrin reagent was found to react specifically in forming a pink product (Emax. 560mμ) with cysteine. 2. The method was highly sensitive for the determination...Full Text Available
Bacterial artificial chromosome (BAC) clones are effective mapping and sequencing reagents for use with a wide variety of small and large genomes. This report describes the development of a physical...Full Text Available
When decontaminated with continuously replenished CAN-DECON reagent in a once-through system, carbon steel contaminated with "6"0Co during exposure to reducing coolant in stainless steel loops loses up to 90 percent of its radioactivity in the first few minutes. Afterwards, the rate of removal falls to much lower values which persist for many hours to the end of the experiment. The effects of flow rate, temperature and reagent concentration on the initial rates of decontamination indicate that mass transfer in the liquid is an important factor in the decontamination. The decontamination factor is influenced by the initial rate.
It is reported about the adsorptive stripping voltammetric determination of uranium, antimony, tin, vanadium and molybdenum using chloranilic acid as complex forming reagent. The determination limits are in the l{sup 1}-range. (orig.) [Deutsch] Es wird ueber die Bestimmung von Uran, Antimon, Zinn, Vanadium und Molybdaen durch Adsorptions-Stripping-Voltammetrie mit Chloranilsaeure als Komplexbildner berichtet. Die Bestimmungsgrenzen liegen im ng l{sup -1} Bereich. (orig.)
The shifts induced by equimolar mixture of typical lanthanide shift reagent such as 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octadionato europium with silver trifluoroacetate in /sup 1/H NMR spectra of aromatic hydrocarbons have been used for analytical purposes; the NMR determination of m- and p-xylenes in mixtures has been chosen as an example. The use has been made of the difference between induced shifts of methyl group signals in the /sup 1/H NMR spectra of m- and p-xylenes. The magnitude of induced shifts of methyl groups signal in m-xylene is always larger than that of p-isomer, irrespective of contents of m- and p-xylenes in mixture.
An hydrazone derivative, 1,2-cyclohexanedione bis-benzoyl-hydrazone (1,2-CHBBH), has been used as a selective reagent for an advanced environmental application consisting of separating the different species of nickel in natural waters by solvent extraction. The effects of pH and reagent concentration on the extraction process were studied, as well as the influence of both organic (humic acids) and inorganic ligands (Cl-). Under natural conditions, organic and inorganic nickel species presented different extraction behaviors, and the variations in extraction yields could be correlated with the concentrations of organic complexes in the samples, allowing the separation of labile and non-labile nickel species in both fresh and marine waters.
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).
A study has been made of the colour reaction involved in the interaction or rare-earth elements with the reagent orthanyl K, the optimum conditions for the reaction being: pH=4.0-4.5 and lambda=660-670 nm. The ratio of components in the complex is Me:R=1:2. Consideration of the relative optical density values of the complex solutions as a function of the serial number of the rare-earth elements made it possible to recommend orthanyl K as a selective reagent for determining La, Ce, Pr and Nb in a mixture of Tu, Yb, Lu and Y oxides. The molar extinction coefficients, the sensitivity of the reaction and the concentration limits where Beer's law applies were calculated. Lanthanum was determined in a binary mixture with thulium and yttrium. (author).
This paper briefly describes an industrial application of the foam decontamination process applied to large volume components. The process is based on the filling of the component with liquid foam containing suitable chemical reagents, and a circulation loop enables its continuous recycling. The process was successfully validated during the decontamination of a graphite gas-cooler representing a developed area of 1000 m{sup 2}. A decontamination factor up to 190 was obtained leading to a residual activity below 1 Bq/cm{sup 2}. The process only produced 6 m{sup 3} of effluent i.e. about ten times less than for a chemical solution technique. (authors) 2 refs.
A spectrophotometric study has been made of the complex formation of vanadium (3) with arsenazo(1), arsenazo(3) and some monosubstituted derivatives of chromotropic acid and sulphanylamides. In acid medium vanadium (3) reacts with each of these reagents to produce a 1:1 complex. Optimum conditions of the complex formation was found. The effect of H"+ on the complex formation of vanadium (3) with chromotropic acid derivatives was established. It was found by the graphical method that the formation of the complex is accompanied by the elimination of one proton. Patterns were found of the influence of the nature of substituents in the organic compound on the ionization constants of acid groups and stability of complexes. Molar extinction coefficients, equilibrium constants of the formation reactions and instability constants for the complexes were calculated. The structure of complexes was suggested. Similar behaviour of all the reagents was ...
The application of kinetic probes that allow one to determine relative reactivities of biologically relevant substrates with oxidizing intermediates in the Fenton reagent (H2O2 plus Fe2+ in acidic aqueous...Full Text Available
This article describes the preparation of 5-nitroisatin and of 5-chloroisatin from isonitrosoacetanilide in a single step, using readily available and inexpensive reagents. These reactions require around 90 minutes and may be carried out as an undergraduate experiment, providing an opportunity to discuss the electrophilic aromatic substitution mechanism, as well as spectroscopic techniques for product identification. (author)
The synthesis of (/sup 14/C)-10,11-Epoxy-(2E,6E)-farnesyl diazoacetate in one vessel, starting from (/sup 14/C)-glyoxylic acid, is described. This compound is useful as a potential photoaffinity labeling agent for juvenile hormone binding sites.
N,N-Dialkyl-P-phenylphosphonamidous iodides are formed in the reactions of phenylphosphonus diiodide with silylated secondary amines. N,N-Dialkyl-P-phenylphosphonamidous iodides react with electrophilic reagents (methyl iodide, benzenesulfonyl azide, and phenyl azide) by the usual schemes with the formation of alkylation and oxidative-imination products. Iodine catalyzes the disproportionation of morpholinophenylphosphinous iodide into dimorphomorpholinophenylphosphinous iodide with iodine are iododimorpholinophenylphosphonium triiodide and phenylphosphonous diiodide.
An evaluation was made of the effectiveness of the action of reagents used for cleaning cyan-containing waste water for conditioning of the overflow of copper concentrate thickners of the Belousovskiy enrichment before sorption extraction of gold by activated charcoal. It was established that conditioning of the overflow by iron sulfates (II), copper and zinc diminshes, and by hypochlorite increases the capacitance of the activated charcoal for gold.
The review is devoted to the use of ionic liquids as solvents, immobilized organocatalysts and reagents in reactions involving carbon acids and 1,3-dipoles, which are widely used to prepare practically valuable organic compounds of various classes. The characteristic features of processes in the presence of ionic liquids, the effects of the structure of cations and anions on the regio-, stereo- and enantioselectivities of reactions and methods of recovery of ionic liquids are considered.
The presence of water in export coals increases transport and handling costs. Coarse (+0.5 mm) coal constitutes the majority of the product, and small changes in its final moisture content will have a significant effect on overall product moisture. An on-line moisture monitor was installed on a product belt immediately after a coarse coal centrifuge to continuously measure the moisture content of the coal from a single centrifuge. Basic studies were also conducted with a laboratory centrifuge specifically designed to characterize various coarse coal samples in terms of their water retention capacity. The moisture of the coarse coal (typically 6 to 9%) was found to vary by at least 1% at a particular plant, and by a number of percentage points between plants. An empirical model has been developed which can explain about 80% of the moisture variation from the 25 samples investigated. The rank of the coals ranged from 0.7 to 1.65% mean reflectance. The model identified four principle ...
Interchangeable technology from Flexicon Liquid Filling, a business division of Watson-Marlow Pumps Group, has helped family-run diagnostic reagent manufacturer, Hart Biologicals Ltd, to accommodate business growth with the recent upgrade to a tabletop bottle filling and capping machine. A peristaltic dispensing pump is crucial for succes
Microwaves improve the rate of many chemical reactions either interacting with the solvent, when the reaction is carried out in solution, or with the surface of a solid substrate where a suitable reagent is dispersed (dry chemistry). A few examples of chemical reactions positively affected by microwaves are described: particularly interesting are those concerning polymers and radio-pharmaceuticals.
The isomeric composition of bicyclo(3.3.1)nonadienes was investigated by GLC and PMR spectroscopy with silver-lanthanide shift reagents. The absence of stereospecificity in the hydrogenation of 3,7-dimethylenebicyclo(3.3.1)nonane by hydrogen adsorbed on Raney nickel was demonstrated. This is explained by the sequence of the isomerization and then hydrogenation processes.
The current methods used by the tissue analysis program at LASL for the determination of americium and plutonium in autopsy tissue are described. Problems affecting radiochemical yield are discussed. Included are problems associated with sample preparation, separation of plutonium from large amounts of bone ash, and reagent contamination. The average "2"4"2Pu tracer yield for 1800 Pu determinations is 78 +- 12%. The average "2"4"2Am tracer yield is 85 +- 7% for 40 determinations.
The current methods used by the tissue analysis program at LASL for the determination of americium and plutonium in autopsy tissue are described. Problems affecting radiochemical yield are discussed. Included are problems associated with sample preparation, separation of plutonium from large amounts of bone ash, and reagent contamination. The average /sup 242/Pu tracer yield for 1800 Pu determinations is 78 +- 12%. The average /sup 242/Am tracer yield is 85 +- 7% for 40 determinations.
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).
Research is described in the development of organometallic reagents in which the boron was attached to a nonreactive organic or inorganic matrix such as polystyrene, silica, or alumina. We developed the synthesis of oxygen-15 labelled butanol, which has been found to be a valuable blood flow agent in humans. We have also developed a series of polymeric borane derivatives which were used to prepare nitrogen-13 labelled amines.
Several lanthanide shift reagents (LSR) were synthesized from praseodymium, europium, dysprosium, and terbium using ethylenediaminetetraacetic acid, trans-1,2-diaminocyclohexane-N,N,N[prime],N[prime]-tetraacetic acid, and diethylenetriaminepentaacetic acid for the purpose of separating overlapping [sup 31]P FT-NMR spectral signals of dissolved organic phosphorus compounds present in concentrated lake-water samples. The extent of change in signal position and line width of several known phosphorus compounds dissolved in pure water was examined as a function of solution pH and the molar ratio of LSR to phosphorus. Praseodymium ethylenediaminetetraacetate (PrEDTA) was determined to be the most effective LSR. Concentrated lake-water samples mixed with PrEDTA were examined with [sup 31]P FT-NMR. The use of PrEDTA provided separation of overlapping signals, indicated that phosphorus compounds were becoming isolated from the solution environment during sample ...
Following the successful application of hydrostatic pressure in mechanistic investigations of organic reactions, chemists have launched a vigorous effort to apply this tool to substitution reactions of coordination compounds. The authors began to study pressure effects in the NMR spectra of keton-lanthanide combination with the hope that the increase shifts anticipated might enhance the utility of the method, perhaps even expand its applicability to new classes of compounds. 5-Phenyl- and 5-tert-butyladamantan-2-one, piperidine, tetrahydrofuran, and cyclopentanol exhibited pressure-reduced lanthanide-induced shifts with Eu(fod)/sub 3/; Yb(fob)/sub 3/ and the shielding reagent Pr(fod)/sub 3/ showed the same effect with adamantanone. Solvent variations (CD/sub 2/Cl/sub 2/, CCl/sub 4/) caused minor changes in the magnitude of these shifts but did not reverse any. With the objective of learning whether these effects are due to a suppressed equilibrium population or to ...
This project will determine whether electrolytic dialysis has promise in the separation of charged particles in an aqueous solution. The ability to selectively move ions from one aqueous solution to another through a semipermeable membrane will be studied as a function of emf, amperage, and particle electrical charge. The ions selected for the study are Cl{sup -} and SO{sub 4}{sup 2-}. These ions are of particular interest because of their electrical conduction properties in aqueous solution resulting with their association with the corrosive action of metals. The studies will be performed with commercial membranes on solutions prepared in the laboratory from reagent salts. pH adjustments will be made with dilute reagent acid and base. Specific objectives of the project include testing a selected membrane currently available for electrolytic dialysis, membrane resistance to extreme pH conditions, the effectiveness of separating a mixture of two ...
This paper deals with an industrial application of the foam decontamination process applied to large volume components. The work presented below was achieved within the context of a CEC contract. The objective of this 4-year programme was to study, develop and demonstrate an effective in-situ decontamination process using foams containing suitable chemical reagents. Laboratory tests were first performed to optimize the chemical formulation of the foams. Pilot tests were then conducted to study the hydrodynamic features of the fluids and to adapt a technique of permanent foam circulation. With these tests completed, it was essential to validate the foam process on an industrial scale and on a representative nuclear component. The objective was successfully achieved. The process was effectively validated during the decontamination of a graphite-gas cooler representing a developed area of 1000 m{sup 2}. Results were quite convincing since the residual activity of the ...
It may result in acute radiation syndrome after body is exposed to ionizing radiation. The one of long-term effects of irradiation injury is leukemia. The bone marrow cells (BMC) transplantation including stem cells is the only effective therapy for acute radiation syndrome patients. Recently, with the advancement of stem cell research that the stem cells have multipotential and can convert each other, it may supply the new stem source for the irradiation injury patients. At the same time with the further research of radioprotective reagents, the hematopoietic stem cells proliferation after irradiation injury is promoted
Transformation of row material to the consumption goods proceeds by the succession of various technologies using energy and chemicals. Relative contribution of both factors is broadly varied. The chemical reagents are not per se consumption goods and their production is auxiliary. Maximal usage of chemicals is observed in conventional technologies. On the contrary radiation technology does not need chemicals. Therefore usage of radiation technology leads to diminution of chemical processing and hence to the attenuation of the technological press on the environment. As examples the radiation technological methods in conversion of coal and biomass are considered. (author).
HgTe rod-shape composed of crystalline particles has been prepared by a hydrothermal method, and characterized by means of X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transition electron microscopy (TEM). The effects of capping agents, reductants, reaction temperatures, and reaction times on crystal structures and shapes of HgTe have been investigated. The results showed that the CTAB as capping agent plays a crucial role in the hydrothermal process. The synthesis procedure is simple and uses less toxic reagents than the previously reported methods.
The report contains highlights of the achievements of the IAEA Co-ordinated Research programme on Evaluation on the Use of Bulk Reagents for the Production of "9"9Tc_m Radiopharmaceutical and Kits, the participants' summary reports (Argentina, Chile, Greece, India, Indonesia, Japan, Malaysia, Portugal, Russian Federation, Thailand, Uruguay, United States of America), recommended product protocols for five compounds and the participants' recommendations regarding continued support and further directions of co-ordinated research work. Refs, 6 figs, 8 tabs, 6 schemes.
Scientists at JPL have developed chemical and biological techniques using microspheres filled with drugs, electron-opaque metals, or radioactive, fluorescent, magnetic or electrically charged materials to label specific groups of cells. Synthetic polymeric microspheres are coupled with specific antibodies to form reagents called immunomicrospheres, which can seek out and attach themselves to any specific group of cells. These cell-labeling techniques, therefore, open new avenues not only to the basic study of cells but also to the diagnosis and treatment of many diseases, including cancer.
The report is divided into three sections. The first section contains a general introduction to ion exchange resins used in various processes, the second section describes characteristic properties of the polymer materials and the inter relation between them. This will, in turn, be useful to interpret the data obtained from the various tests carried out on the resins in the laboratory. In the third section of the report, are given the details of each method used for a particular test to be carried out on a routine basis. Each method describes the principle involved, the reagents and apparatus used in the experiment, the actual procedure and calculations and recording of the data. 3 refs. (author).
Radian Corporation was contracted to investigate duct injection and ESP phenomena in a 1.7 MW pilot plant constructed for this test program. This study was an attempt to resolve problems found in previous studies and answer remaining questions for the technology using an approach which concentrates on the fundamental mechanisms of the process. The goal of the study was to obtain a better understanding of the basic physical and chemical phenomena that control: (1) the desulfurization of flue gas by calcium-based reagent, and (2) the coupling of an existing ESP particulate collection device to the duct injection process. Process economics are being studied by others. (VC)
Radian Corporation was contracted to investigate duct injection and ESP phenomena in a 1.7 MW pilot plant constructed for this test program. This study was an attempt to resolve problems found in previous studies and answer remaining questions for the technology using an approach which concentrates on the fundamental mechanisms of the process. The goal of the study was to obtain a better understanding of the basic physical and chemical phenomena that control: (1) the desulfurization of flue gas by calcium-based reagent, and (2) the coupling of an existing ESP particulate collection device to the duct injection process. Process economics are being studied by others. (VC)
This work is the first active crossflow filter testing of the new strontium-permanganate process for Envelope C at the Savannah River Technology Center. Extreme filtration difficulties with the ferric hydroxide precipitation led to investigations of other chemistries with simulants. The current process includes the isotopic dilution by precipitation from inactive strontium nitrate addition. A permanganate strike to replace ferric reagents was found to provide practical filterability and good lanthanide or transuranic decontamination. That work had been supported with simulant and active beaker testing.
The Purex process and the fluorescence spectrometry are first recalled, then uranyl fluorescence is studied in a pure nitric medium without other elements to establish a theoretical model, allowing the description of uranium fluorescence signal with a general equation. The influence of different parameters (temperature, inhibitors, dynamic quenching of iron and cerium) is investigated to develop the model. A quantitative analysis method without addition of reagents is proposed to validate the model.
Simple hydroxamic acids are shown to be useful reagents for the separation of Np and Pu from U within simplified, single cycle Purex flowsheets. They are compatible with the use of centrifugal contactors and laboratory scale flowsheet trials with aceto-hydroxamic acid have demonstrated high actinide recoveries and decontamination factors on products for active feeds of up to 40 wt.% Pu. They therefore show many ideal characteristics for Pu and Np recovery within flowsheet options for actinide recovery in advanced fuel cycles. Furthermore, in order to optimise the routing of Np with the Pu product in advanced flowsheets, additional studies of Np extraction in the primary co-decontamination contactor, prior to U/Pu partition, have been undertaken, combining experiment, modelling and flowsheet tests. (author)
This experiment is carried out in the series of the investigation on the damage mechanism of carbon steel. In this paper, the damage situation is considered by structure observations. The test were carried out in 600degC-1200degC temperature range, in blowing an argon gas. The reagents are Na{sub 2}O, Na{sub 2}O{sub 2} and NaOH. From structure observations, the holes are observed on the surface of iron-base material in some test conditions. This result is indicated that the selective reaction occurs. The selective reaction is more obvious as the time exposed to the high temperature is longer. It is considered that the selective reaction occurs after the chemical reaction between iron-base material and sodium compound. The areas, in which Mn-concentration is higher, are observed in products on the surface of specimen. (author)
The synthesis and structures of three new compounds are reported. [Mg2{PhP(Se,O)Se-Se(O,Se)PPh}2(thf)7(H2O)3] (1), [Mg{PhP(Se,O)Se-Se(O,Se)PPh}(thf)3(H2O)] (2), and [Mn{PhP(Se,O)Se-Se(O,Se)PPh}(thf)3(H2O)] (3) were prepared by treatment of Woollins reagent [PhP(Se)(m-Se)]2 with the corresponding hydrated metal acetates.
The direct addition of nickel powder to the reaction mixtures of 1,3-dialkyl-4,5-dioxoimidazolidine-2-thione (1) with the thionation Lawesson reagent produces [Ni{sup II}(R{sub 2}timdt{sup -}){sub 2}] (R{sub 2}timdt = 1,3-dialkylmidazolidine-2,4,5-trithione). These complexes belong to a new class of nickel-dithiolenes, showing remarkably high absorption ({epsilon} {approx} 80 000 dm{sup 3} mol{sup -1} cm{sup -1}, {lambda} {approx} 1000 nm) in the near-infrared region (near-IR), accompanied by high photochemical stability that makes these complexes promising near-IR dyes.
Motivated by the discovery of superconductivity in alkali and alkaline earth fullerides, this program was undertaken both to understand the nature of and expand the range of materials demonstrating superconductivity. The first approach involved attempts to modify the fullerene cage by incorporating heteroatoms in the structure and the preparation and photophysical properties of nitrogen and sulfur doped fullerenes were studied in detail. The second approach involved examining the stoichiometry and effect of preparative conditions on the behavior of alkali, alkaline earth, lanthanide and mixed ion fullerides. In particular, the authors have elaborated on a technique for making such salts using liquid ammonia or aliphatic amines as solvents. Thirdly, modeling studies were undertaken to predict the properties of heterohedral fullerines and metal - C60 complexes, and theoretical guidelines were developed for understanding the reactivity of the fullerene cage to common addition ...
Interaction of W(6) with sulphonaphtholazoresorcinol (SNAR) in aqueous solution has been studied. Tungsten is determined in the form of sulphonaphtholazoresorcinate by extraction with higher alcohols. The optimum conditions for the formation of a complex of W with SNAR in aqueous solution are as follows: a 10-fold excess of SNAR, concentration of HCl 1-1.5N, ethanol content 5-10 vol.%, time of formation of the complex 30 min. A component ratio for the complex has been established in the case of aqueous solution and extract; molar extinction coefficients are 0.9x10"4 and 1.7x10"4, respectively. The formation constant for the complex being extracted is 2.2x10"2"3. A method has been developed for determination of microgram quantities of W in a vanadium specimen.
The objective of this research was to convert coal into a soluble substance under mild conditions. The strategy involved two steps, first to breakdown the macromolecular network of coal, and second to add hydrogen catalytically. We investigated different basic reagents that could, in priciple, break down coal's structure and alkylation strategies that might enhance its solubility. We examined O- and C-alkylation, the importance of the strength of the base, the character of the added alkyl groups and other reaction parameters. This work provided new information concerning the way in which hydrogen bonding, polarization interactions between aromatic structures and covalent bonding could be disrupted and solubility enhanced. The objective of our research was to explore new organochromium chemistry that might be feasible for the hydrogenation of coal under mild conditions.
A procedure was developed for separating rubidium from irradiated aluminum encapsulated uranium. The separations procedure produces a final ultra-high purity RbCl product for subsequent high performance mass spectrometric analysis. The procedure involves first removing most of the macro-components and fission products by strong base anion exchange using, first, concentrated HCl, then oxalic acid media and second, selectively separating rubidium from alkaline-earth ions and other alkali-metal ions, including cesium, using Bio-Rex-40 cation-exchange resin. The resultant RbCl is then put through a final vacuum sublimation step. Ultra-pure reagents and specially clean glassware are used throughout the procedure to minimize contamination by naturally-occurring rubidium.
A procedure was developed for separating rubidium from irradiated aluminum encapsulated uranium. The separations procedure produces a final ultra-high purity RbCl product for subsequent high performance mass spectrometric analysis. The procedure involves first removing most of the macro-components and fission products by strong base anion exchange using, first, concentrated HCl, then oxalic acid media and second, selectively separating rubidium from alkaline-earth ions and other alkali-metal ions, including cesium, using Bio-Rex-40 cation-exchange resin. The resultant RbCl is then put through a final vacuum sublimation step. Ultra-pure reagents and specially clean glassware are used throughout the procedure to minimize contamination by naturally-occurring rubidium.
Since 1999, several studies on nuclear fuels were realised in C11/C12 Atalante Hot Cell. This paper presents firstly an overview of the apparatus used for fuel dissolution and characterisation like reactor design, gas trapping flask and solid/liquid separation. Then, the general methodology is described as a function of fuel, temperature, reagents, showing for each step, the reachable experimental data: Dissolution rate, chemical and radiochemical fuel composition including volatile LLRN, insoluble mass, composition, morphology, cladding chemical, radiochemical and physical characterisation using SIMS (made in Cadarache/LECA facilities), MEB. To conclude, some of the obtained results on 129I and 14C composition of oxide fuels, rate of dissolution and first results on dissolution studies of RERTR UMo fuel will be detailed. (Author)
We have demonstrated that, with simple pH adjustment, volatile drugs such as methamphetamine, amphetamine, 3,4-methylenedioxymethamphetamine (MDMA), ketamine, and valproic acid could be analyzed rapidly from raw biofluid samples (e.g. urine and serum) without dilution, or extraction, using atmospheric pressure ionization. The ion source was a variant type of atmospheric pressure chemical ionization (APCI) that used a dielectric barrier discharge (DBD) to generate the metastable helium gas and reagent ions. The sample solution was loaded in a disposable glass pipette, and the volatile compounds were purged by nitrogen gas to be reacted with the metastable helium gas. The electrodes of the DBD were arranged in such a way that the generated glow discharge was confined within the discharge tub...
This paper studies the analytical application of europium (III)-morin complex which is formed in alkaline medium and has an intense color. The extent of europium extraction was determined by adding to the extract a morin solution in isoamyl alcohol in a 50-100-fold excess with respect to europium. The dependence of the optical density of the extracts on the ph in the system europium (III)-morin-water-organic solvent for different excesses of the reagent is shown: this indicates formation of two extractable complexes, one being dominant in the pH range 4-7, the other at pH greater than or equal to 8.5. The extraction of the europium (III)-morin complex from alkaline solution is used for direct extraction-photometric determination of europium(III) in compounds of elements having amphoteric properties or forming amines (Zns, Mo0/sub 3/).
A new luminescent europium probe is presented for the determination of phosphate (P) in microtiter plate format. The assay is based on the quenching of the luminescence of the europium-tetracycline (EuTc) 1:1 complex by phosphate using a reagent concentration of 20.8 {mu}mol/L. The probe is excited at 400 nm and displays a large Stokes' shift of 210 nm. The emission maximum is located at 616 nm. The system works best at neutral pH 7 and is therefore suitable for phosphate determination in biological and biochemical systems. The linear range of the calibration plot is from 5 x 10{sup -6} mol/L to 7.5 x 10{sup -4} mol/L of phosphate, and the limit of detection is 3 {mu}mol/L.
We described the use of silica nanoparticles as building blocks for the immobilization of electrogenerated chemiluminescence (ECL) reagent Ru(bpy){sub 3}{sup 2+} and the fabrication of layer-by-layer assembly film by alternating the deposition of the Ru(bpy){sub 3}{sup 2+}-doped silica nanoparticles and Au nanoparticles. UV-vis absorption spectroscopy, scanning electron microscopy (SEM), cyclic voltammetry and ECL were used to characterize the uniform growth of the multilayer film. Since Ru(bpy){sub 3}{sup 2+} could still maintain its ECL property when doped into the silica nanoparticles, the as-prepared multilayer film could be used as an effective ECL sensor, and the sensor showed high sensitivity and good stability.
We described the use of silica nanoparticles as building blocks for the immobilization of electrogenerated chemiluminescence (ECL) reagent Ru(bpy)_3"2"+ and the fabrication of layer-by-layer assembly film by alternating the deposition of the Ru(bpy)_3"2"+-doped silica nanoparticles and Au nanoparticles. UV-vis absorption spectroscopy, scanning electron microscopy (SEM), cyclic voltammetry and ECL were used to characterize the uniform growth of the multilayer film. Since Ru(bpy)_3"2"+ could still maintain its ECL property when doped into the silica nanoparticles, the as-prepared multilayer film could be used as an effective ECL sensor, and the sensor showed high sensitivity and good stability.
We described the use of silica nanoparticles as building blocks for the immobilization of electrogenerated chemiluminescence (ECL) reagent Ru(bpy)32+ and the fabrication of layer-by-layer assembly film by alternating the deposition of the Ru(bpy)32+-doped silica nanoparticles and Au nanoparticles. UV-vis absorption spectroscopy, scanning electron microscopy (SEM), cyclic voltammetry and ECL were used to characterize the uniform growth of the multilayer film. Since Ru(bpy)32+ could still maintain its ECL property when doped into the silica nanoparticles, the as-prepared multilayer film could be used as an effective ECL sensor, and the sensor showed high sensitivity and good stability.
Natural rubber (NR) and its derivatives as renewable and biodegradable materials have attracted considerable attention because of the serious pollution problems caused by synthetic materials and a shortage of resources. A new semi-interpenetrating polymer network (semi-IPN) based on epoxidised natural rubber and polyvinyl alcohol containing maleic acid as a crosslinking reagent was synthesized and characterized by FTIR, XRD, SEM, swelling ratio in both distilled water and toluene, and mechanical properties. The curing time and dose of maleic acid were varied from 10 to 60min, and from 10 to 60% (w/w), respectively. An IR spectroscopic study indicated the presence of an ester linkage at 1730cm-1 in maleic acid crosslinked with PVA in semi-IPN films. In addition, the crystalline content of P...
Using the method of statistic planning of an experiment, the SrSO_4 desulfurization process has been studied in the case of reductive roasting of celestine with the use blast-furnace coke. The main factors that determine the rate of the SrSO_4 desulfurization are the roasting temperature and charge components dispersity. The desulfurization rate increases proportionally to the increase in the roasting temperature and dispersity of the reaction mixture components. To decrease the SrSO_4 desulfurization and the concentration of sulfur-containing components in gases released at rather a high celestine reduction rate, the roasting is recommended to proceed at the temperature of 1100 to 1150 deg, in this case it is necessary to limit the content of small (less than 3.2 mm) fractions of reagents.
Americium extraction in different oxidation states in two-phase aqueous system based on polyethylene glycol is investigated. Conditions for quantitative extraction of americium (3) and americium (5) from ammonium sulfate solutions within pH=3-5 interval in the presence of arsenazo 3 are found. Composition of the produced americium complexes with reagent is determined; americium (3) interacts with arsenazo 3 in ammonium sulfate solutions with the formation of MeR and Me_2R composition complexes. Absorption spectrum characteristics of americium (3) and- (5) complexes with arsenazo 3 in ammonium sulfate solutions and extracts based polyethylene glycol aqueous solutions are given. Molar extinction coefficients of americium complexes with arsenazo (3) in these solutions are determined.
The nuclear energy cycle requires the recycling of nuclear fuel, water, chemical reagents, and the volume reduction of radioactive liquid wastes. A fundamental technique for continuous recovery of water using a thin-film evaporator was examined. Appropriate recovery measurements were: an evaporator heat temperature of 323 K, a feed rate of 0.23 cm"3 x s"-"1, a vacuum pressure of 15 mmHg (2 kPa), and impeller rotational speeds of 500#approx#600 rpm (min"-"1). The concentration of trace technetium and rhenium in aqueous solutions was also studied. A decontamination factor of 10"5 for rhenium was obtained. (author)
Research was conducted by the Bureau of Mines to determine the feasibility of using electrokinetic densification to dewater Bayer process red mud, magnetic black and prepared by pressure digestion of red mud in the presence of ferrous sulfate, and magnetic black mud formed by simulated Bayer digestion of Jamaican bauxite with added ferrours sulfate. Tests showed that the solids content of presettled muds could be increased from 25 pct to approximately 40 to 48 pct by gravity draining followed by electrodewatering for approximately 48 h. Electrodewatering may not be practical because of increased reagent and processing costs and because the muds must be thoroughly wasted prior to electrodwatering to remove dissolved ions and decrease mud conductivities.
The effect of a series of complexing and reducing agents on the extraction-chemical behavior of technetium as applied to extraction splitting of uranium and plutonium in the Purex process was examined. Kinetic parameters of the catalytic decomposition of N2H5NO3 under the action of Tc in the presence of these agents were evaluated. Variation of the ratio of the oxidized and reduced Tc species in the course of the process and in the hydrazine-free systems was determined. Reagents preventing oxidation of the reduced technetium and decomposition of N2H5NO3 in nitric acid solutions (acetohydroxamic acid, hydroxylamine, ascorbic acid, etc.), inhibiting the reduction of Tc with hydrazine nitrate (H2O2, HN3, etc.), and known as complexing agents toward quadrivalent actinides but indifferent to Tc...
In the past shredder fluff from automobile recycling was discarded in landfills, but shrinking landfill space and the partly hazardous content of the fluff as well as its caloric value, all resulted in efforts to turn this waste problem into an energy resource. In order to produce a fuel, the inorganic compounds have to be removed. Extensive analyses and particle size measurements were made on fluff from various shredder. For optimal separation all particles are reduced to a uniform, relatively small size. In a subsequent combined screening and air classification process, successful separation into organic and inorganic fractions is achieved. The inorganic fraction is treated in a heavy media or an eddy-current separator to recover the valuable metals, while the organic fraction is now suitable for thermal processing, such as fluidized bed gasification and using the resulting carbon as a chemical reagent.
Normal butylamine compounds are studied as salt-free wash reagents for degraded solvent used in PUREX process in spent fuel reprocessing. The solvent wash tests were carried out with two types of butylamine compounds, n-butylamine oxalate and n-butylamine bicarbonate, by counter-current mode using a small size mixer-settler composed of two 4-stage wash steps. Di-n-butyl phosphoric acid (HDBP), the main degradation product from TBP, was removed from real degraded solvent with decontamination factor of 2.5 {approx} 7.9. The study on electrolytic decomposition of butylamine compounds was also conducted for waste treatment.
A new strontium metal-organic framework, [Sr2(BTEC)(H2O)4] 2H2O (1) (H4BTEC=benzene-1,2,4,5-tetracarboxylic acid), has been successfully synthesized by mixing the starting reagents. The single-crystal structure analysis showed that compound 1 displayed three-dimensional structures containing inorganic motifs with two-dimensional layers pillar-connected through organic linkers and forming water-coordinated neutral framework. Further studies revealed that compound 1 was insoluble in water and that it emitted strong luminescence at approximately 437nm after dehydration.
In the Advance Coal Liquefaction Concept Proposal (ACLCP) carbon monoxide (CO) and water have been proposed as the primary reagents in the pretreatment process. The main objective of this project is to develop a methodology for pretreating coal under mild conditions based on a combination of existing processes which have shown great promise in liquefaction, extraction and pyrolysis studies. The aim of this pretreatment process is to partially depolymerise the coal, eliminate oxygen and diminish the propensity for retograde reactions during subsequent liquefaction. The desirable outcome of the CO pretreatment step should be: (1) enhanced liquefaction activity and/or selectivity toward products of higher quality due to chemical modification of the coal structure; (2) cleaner downstream products; (3) overall improvement in operability and process economics.
In the Advance Coal Liquefaction Concept Proposal (ACLCP) carbon monoxide (CO) and water have been proposed as the primary reagents in the pretreatment process. The main objective of this project is to develop a methodology for pretreating coal under mild conditions based on a combination of existing processes which have shown great promise in liquefaction, extraction and pyrolysis studies. The aim of this pretreatment process is to partially depolymerise the coal, eliminate oxygen and diminish the propensity for retograde reactions during subsequent liquefaction. The desirable outcome of the CO pretreatment step should be: (1) enhanced liquefaction activity and/or selectivity toward products of higher quality due to chemical modification of the coal structure; (2) cleaner downstream products; (3) overall improvement in operability and process economics.
The effect of method of sulfur addition on the hydrocracking activity of coal liquefaction catalysts was investigated using a high-pressure differential thermal analyser. The three methods of sulfur addition were: 1) physical mixing of 10 wt% elemental sulfur with red mud; 2) pre-sulfidation of red mud with hydrogen sulfide; 3) use of reagent grade pyrite. The pre-sulfided catalyst was slightly less active than the catalyst prepared by physical mixing, and both of these were changed to pyrrhotite in the course of use. Although the pyrite catalyst exhibited activity at markedly lower temperatures than those required for the other two catalysts, conversions were lower than had been expected. This is thought to be due to a different catalytic mechanism being involved. 13 references.
A means of determination of a ctive hydrogen of hydroxyl, carboxyl, sulfhydryl, amino, amido and sulfonamido groups by chemical ionization mass spectrometry using ammonia and trideuterioammonia as reagent gases is described. The method is based on exchange of active hydrogen for deuterium occurring during the chemical ionization process using trideuterioammonia, with comparison of m/z for ammonium adduct [M + NH1]+ and trideuterioammonium adduct [M--nH + nD + ND4]+, or of protonated molecular ion [M + H]+ and deuteronated molecular ion [M--nH + nD + D]+ yielding the number of active hydrogens. Applications have been made to several classes of biologically important compounds. PMID:427257
One chemical reagent, hydrazine hydrate, was discovered to accelerate the growth of semiconductor nanocrystals (cadmium telluride) instead of additional energy, which was applied to the synthesis of high-quality CdTe nanocrystals at room temperature and ambient conditions within several hours. Under this mild condition the mercapto stabilizers were not destroyed, and they guaranteed CdTe nanocrystal particle sizes with narrow and uniform distribution over the largest possible range. The CdTe nanocrystals (photoluminescence emission range of 530-660 nm) synthesized in this way had very good spectral properties; for instance, they showed high photoluminescence quantum yield of up to 60%. Furthermore, we have succeeded in detecting the living Borrelia burgdorferi of Lyme disease by its photoluminescence image using CdTe nanocrystals.
As coal becomes more and more important as a power plant fuel in this time of energy shortage and the combustion of high-sulfur coals that would impair air quality, efforts have been made to devise efficient processes to control sulfur dioxide emission. Besides desulfurization before combustion, flue gas desulfurization is considered the most promising method that could also be applicable to all other fossil fuels. In this article, the flue gas desulfurization processes are briefly reviewed, and processes with highest use and with high potential for future use are compared from technical and economical points of view. In the selection of a desulfurization process, it is very important to consider the capacity of the plant, fuel type and fuel-to-sulfur ratio, availability and price of the reagent to be used, type, price, and market of side products, disposal problems of wastes, and environmental factors.
The evolution of "humanized" (i.e., free of animal sourced reagents) and ultimately chemically defined culture systems for human embryo stem cell (hESC) isolation and culture is of importance to improving their efficacy and safety in research and therapeutic applications. This can be achieved by integration of a multitude of individual approaches to replace or eliminate specific animal sourced reagents into a single comprehensive protocol. In the present study our objective was to integrate strategies obviating reliance on some of the most poorly defined and path-critical factors associated with hESC derivation, namely the use of animal immune compliment to isolate embryo inner cell mass, and animal sourced serum products and feeder cells to sustain hESC growth and attachment. As a result we report the derivation of six new hESC lines isolated by outgrowth from whole blastocysts on an extracellular matrix substrate of purified human laminin ...
Silanization of the silica gel surface in the synthesis of silica gel polyamine composites uses (chloropropyl)-trichlorosilane (CPTCS). It is possible to substitute a molar fraction of reagent CPTCS with methyltrichlorosilane (MTCS), creating a mixed silane surface layer. Two types of silica gels were modified with a series of MTCS:CPTCS molar ratios. Solid-state CP/MAS 29Si and 13C NMR spectroscopies were used to evaluate the surface silane composition. Surface silane coverage was markedly improved for the resulting gels. When polyamines were grafted to the resultant MTCS:CPTCS silane layers, it was shown that the decrease in the number of propyl attachments to the polyamine resulted in increased quantities of ''free amines''. Optimum MTCS:CPTCS ratios were determined for three polyamines grafted onto one silica gel. A substantial free amine increase was observed for poly(allylamine) (PAA). Metal uptake studies show increases in ...
Silanization of the silica gel surface in the synthesis of silica gel polyamine composites uses (chloropropyl)-trichlorosilane (CPTCS). It is possible to substitute a molar fraction of reagent CPTCS with methyltrichlorosilane (MTCS), creating a mixed silane surface layer. Two types of silica gels were modified with a series of MTCS:CPTCS molar ratios. Solid-state CP/MAS 29Si and 13C NMR spectroscopies were used to evaluate the surface silane composition. Surface silane coverage was markedly improved for the resulting gels. When polyamines were grafted to the resultant MTCS:CPTCS silane layers, it was shown that the decrease in the number of propyl attachments to the polyamine resulted in increased quantities of ''free amines''. Optimum MTCS:CPTCS ratios were determined for three polyamines grafted onto one silica gel. A substantial free amine increase was observed for poly(allylamine) (PAA). Metal uptake studies show increases in ...
Full text.National programs of neonatal screening were introduced in most countries and have proved their effectiveness against different types of retardation in children. Congenital hypothyroidism is one of the most common causes of physical and mental retardation in children. Programs of screening have shown that the incidence of this disorder is ethnic-background: it is low in Africans: 1-32000 whereas it is 1-3500 and 1-5000 in Hispanic and European newborns respectively. No previous mass screening programs were done in Lebanon. For this purpose, this program was introduced in collaboration with the IAEA. Cord blood is spotted into circles on filter paper just after delivery. These samples are air-dried at room temperature and kept at 4 degree C. They are then collected from hospitals to be screened. In the laboratory, all samples are assayed for IRMA TSH first. Those showing high or borderline TSH level (20mU/L) are then assayed for RIA TT4. Only those showing straight forward ...
A simple and rapid laser fluorometric determination of trace and ultra trace level of uranium in a wide variety of low uranium content materials like soil, basic and ultra basic rocks, plant ash, coal fly ash and red mud samples is described. Interference studies of some common major, minor and trace elements likely to be present in different geological materials on uranium fluorescence are studied using different fluorescence enhancing reagents like sodium pyrophosphate, orthophosphoric acid, penta sodium tri-polyphosphate and sodium hexametaphosphate. The accurate determination of very low uranium content samples which are rich in iron, manganese and calcium, is possible only after the selective separation of uranium. Conditions suitable for the quantitative single step extraction of 25 ng to 20 #mu#g uranium with tri-n-octylphosphine oxide and single step quantitative stripping with dilute neutral sodium pyrophosphate, which also acts as fluorescence enhancing ...
Full text: Nuclear material is subjected to chemical processing throughout the entire fuel cycle. Traces of the chemical reagents and solvents are left behind in the nuclear material. So far essentially metallic impurities or light elements have been investigated for their potential in providing clues on the type of process they originate from. In the present investigation, the applicability of anions for attributing nuclear material to a certain chemical process has been investigated. Anions (e.g. nitrate, sulphate, phosphate, chloride) originate from acids or salt solutions that are used for processing of solutions containing uranium or plutonium. The study presented in this paper focuses on yellow cake samples originating from different mines applying different chemical processes for leaching, dissolving and precipitating the uranium. Consequently, the anionic patterns should be different. The concentrations of different anionic species were measured by ion ...
Cytochrome c, labeled with /sup 125/I, has been used by us for staining glycosaminoglycans (GAG) separated by electrophoresis on cellulose acetate strips. As GAG between 1-10 ng could be quantified by autoradiography and densitometry, the reagent is approximately 100-fold more sensitive than currently used non-radiolabeled stains. The authors extend now the use of radiolabeled cytochrome c to the quantification of PG transblotted to solid supports subsequent to separation on polyacrylamine slab gels. Dot blotting used for exploring optimal conditions for detecting PG indicated that because of low background positively charged Nylon 66 was superior to nitrocellulose. Increasing the positive charge of the staining reagent by cationization decreased background radiation even further so that 1 ng PG could be seen readily after 5 hrs of autoradiography. Use of cationized /sup 125/I-cytochrome c has been made in detecting PG of bovine fetal ...
The affinity label 8-((4-bromo-2,3-dioxobutyl)thio)adenosine 5{prime}-triphosphate (8-BDB-TA-5{prime}-TP) reacts covalently with rabbit muscle pyruvate kinase, incorporating 2 mol of reagent/mol of enzyme subunit upon complete inactivation. Protection against inactivation is provided by phosphoenolpyruvate, K{sup +}, and Mn{sup 2+} and only 1 mol of reagent/mol of subunit is incorporated. The authors have now identified the resultant modified residues. After reaction with 8-BDB-TA-5{prime}-TP at pH 7.0, modified enzyme was incubated with ({sup 3}H)NaBH{sub 4} to reduce the carbonyl groups of enzyme-bound 8-BDB-TA-5{prime}-TP and to introduce a radioactive tracer into the modified residues. Following carboxymethylation and digestion with trypsin, the radioactive peptides were separated on a phenylboronate agarose column followed by reverse-phase high-performance liquid chromatography in 0.1% trifluoroacetic acid with an acetonitrile gradient. ...
The project involved several studies of vesicles and micelles and their constituent surfactants. The primary objective of the project was an elucidation of factors involved in the stabilization and destabilization of vesicles and micelles. Work was performed on seven individual studies. Several different types of novel cleavable surfactants were synthesized, including systems with two chains and two head groups, and their aqueous micelles and vesicles were characterized by methods including dynamic laser light scattering (to give aggregate sizes) and differential scanning calorimetry (to give vesicle bilayer phase transition temperatures). A cleavable surfactant is stable under certain conditions but liable under other conditions with respect to cleavage to give nonsurfactant products and/or other surfactants with different properties. The destruction of several cleavable surfactant-derived aggregates was demonstrated, indicating that they have potential as entrapment and release ...
Fission track analysis (FTA) technique for the determination of "2"3"9Pu excreted through urine has been standardized using blank samples, tracer and "2"3"9Pu spikes. Double stage anion exchange separation protocol has been applied and an average radiochemical recovery of "2"3"9Pu of 18% was obtained. An average track registration efficiency of 11 tracks per #mu#Bq of "2"3"9Pu, irradiated to 0.35x10"1"7 neutron fluence was established. Reagent blank urine samples from 11 controlled subjects were analyzed by FTA and an average of 149#+-#14 tracks was obtained. Minimum detectable activity of 34 #mu#Bq L"-"1 of urine sample was obtained and will be useful for monitoring chronic exposure cases handling MOX fuel.
The dispersion of more than 20 vol pct submicrometer ceramic particles within a metallic matrix and the deposition of such a cermet to form a thick and tough coating presents problems. Most of the coating techniques have failed in attempting to homogeneously disperse very fine and hard particles in large amounts while avoiding their decomposition or reaction with the metal matrix during the deposition process. A simple and efficient method has been developed for producing ceramic-containing composite coatings. It consists in synthesizing cermet-based materials and in depositing them by a rapid solidification process, such as thermal spraying. Boride- and carbide-based materials have been successfully obtained by plasma spraying reactive powders comprising the basic reagents. These materials, with a microstructure of submicrometer ceramic particles dispersed in a metallic matrix, exhibit good wear-resistant properties (abrasion and sliding wear). Finally, reactive ...
A series of tests has been carried out to determine the operating conditions required to remove the corrosion deposit from samples cut from Winfrith Steam Generating Heavy Water Reactor (WSGHWR) primary circuit pipework by submerged water jetting. Two types of samples were used - one set subjected to the normal annual reactor decontamination using TURCO reagents, the other set having been given a LOMI treatment in addition. Tests showed that useful decontamination factors could be achieved on both types of sample, but significantly less severe operating conditions were required to decontaminate the LOMI treated samples. A decontamination factor of 10 was achieved on TURCO treated samples at 360 Bar; only 200 Bar was required to achieve the same decontamination factor on LOMI treated samples. No metal erosion of the stainless steel substrate was found to occur at these pressures. (author).
The reaction of the retinylidene Schiff base in bacteriorhodopsin (bR) to the water-soluble reagent hydroxylamine is enhanced by greater than 2 orders of magnitude under illumination. We have used this reaction as a probe for changes in Schiff base reactivity during the photocycle of wild-type bR and mutants defective in proton transport. We report here that under illumination at pH 6, the D85N mutant has a 20-fold lower rate and the D212N mutant has a greater than 4-fold higher rate for the light-dependent reaction with hydroxylamine compared with wild-type bR. In contrast, the reactivities of wild-type bR and the D96N and T46V mutants are similar. It has been previously shown that the D96N and T46V replacements have no significant effect on the kinetics of M formation but have dramatic effects on rate of the decay of M. We therefore conclude that the hydroxylamine reaction occurs before formation of the M intermediate. Most likely it occurs at the L stage of the ...
Plerocercoids of the tapeworm Spirometra mansonoides produce a substance that stimulates growth of experimental hosts. We report purification of plerocercoid growth factor (PGF) to homogeneity by a process involving isolation and solubilization of plerocercoid membranes, isoelectric point selection by chromatofocusing chromatography or preparative isoelectric focusing, and anion-exchange chromatography. A radioreceptor assay (RRA) for human growth hormone (hGH) was used to detect PGF and purity of the 27.5-kDa protein was judged by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). Proteolytic activity was detected in the 27.5-kDa protein by gelatin substrate PAGE. Characterization of PGF as a neutral cysteine proteinase was based on substrate and inhibitor specificities and dependence on pH and thiol-containing reagents. The association of hGH agonist and proteinase activities was shown by comparing RRA and hydrolytic activities in the presence ...
One of our research objectives is to develop chemistry of transition metal chalcogenides which are relevant to new inorganic materials, environmental catalysts, metalloenzymes. In this context, this research project has been aimed at rational syntheses of chalcogenide complexes of electron-deficient transition metals, construction of hetero metallic clusters with high nuclearity, and elucidation of chemical properties characteristic of these metal chalcogenide compounds. We were successful in synthesizing a series of sulfide (selenide)/thiolate complexes of group 4,5 and 6 transition metal elements by making use of C-S bond cleaving reactions and anhydrous chalcogenide reagents. We also achieved construction of unprecedented large chalcogenide clusters of mixed metal systems such as [Cu{sub 4}(dppm){sub 4}MS{sub 4}] [PF{sub 6}]{sub 2} (M=Mo, W), [(Cp*WS{sub 3}Ag{sub 2}){sub 2}({mu}-Br){sub 2}]{sub {infinity}}, and [Cp*{sub 2}Mo{sub 2}Fe{sub 2}S{sub 4}]{sub ...
Plutonium metal is produced by reducing PuF{sub 4} prepared from PuO{sub 2} by fluorination. Both fluorination and reduction are batch processes at the Los Alamos Plutonium Facility. The conversion of plutonium oxide to fluoride greatly increases the neutron yield, a result of the high cross section for alpha-neutron ({alpha},n) reactions on fluorine targets compared to the (more than 100 times) smaller {alpha},n yield on oxygen targets. Because of the increase, total neutron counting can be used to monitor the conversion process. This monitoring ability can lead to an improved metal product, reduced scrap for recycle, waste reduction, minimized reagent usage, and reduce personnel radiation exposures. A new stirred-bed fluorination process has been developed simultaneously with a recent evaluation of an automated neutron-counting instrument for quantitative process monitoring. Neutrons are counted with polyethylene-moderated {sup 3}He-gas proportional counters. ...
Abstract in english The tegument surface of the adult schistosome, bounded by a normal plasma membrane overlain by a secreted membranocalyx, holds the key to understanding how schistosomes evade host immune responses. Recent advances in mass spectrometry (MS), and the sequencing of the Schistosoma mansoni transcriptome/genome, have facilitated schistosome proteomics. We detached the tegument from the worm body and enriched its surface membranes by differential extraction, before subjecting t (more) he preparation to liquid chromatography-based proteomics to identify its constituents. The most exposed proteins on live worms were labelled with impearmeant biotinylation reagents, and we also developed methods to isolate the membranocalyx for analysis. We identified transporters for sugars, amino acids, inorganic ions and water, which confirm the importance of the tegument plasma membrane in nutrient acquisition and solute balance. Enzymes, including phosphohydrolases, ...
Glass produced during the Purex 4 campaigns of the Integrated Defense Waste Processing Facility (DWPF) Melter System (IDMS) and the 774 Research Melter contained a lower fraction of sludge components than targeted by the Product Composition Control System (PCCS). Purex 4 glass was more durable than the benchmark (EA) glass, but less durable than most simulated SRS high-level waste glasses. Also, Purex 4 glass was considerably less durable than predicted by the algorithm which will be used to control production of DWPF glass. A melter run was performed using the 774 Research Melter to determine if the initial PCCS target composition determined for Purex 4 would produce acceptable glass whose durability could be accurately modeled by Hydration Thermodynamics. Reagent grade oxides and carbonates were added to Purex 4 melter feed stock to simulate a higher sludge loading. Each canister of glass produced was sampled and the composition, crystallinity, and durability was ...
Glass produced during the Purex 4 campaigns of the Integrated DWPF Melter System (IDMS) and the 774 Research Melter contained a lower fraction of sludge components than targeted by the Product Composition Control System (PCCS). Purex 4 glass was more durable than the benchmark (EA) glass, but was less durable than most other simulated SRS high-level waste glasses. Further, the measured durability of Purex 4 glass was not as well correlated with the durability predicted from the DWPF process control algorithm, probably because the algorithm was developed to predict the durability of SRS high-level waste glasses with higher sludge content than Purex 4. A melter run, designated Purex 4 Remediation, was performed using the 774 Research Melter to determine if the initial PCCS target composition determined for Purex 4 would produce acceptable glass whose durability could be accurately modeled by the DWPF glass durability algorithm. Reagent grade oxides and carbonates ...
The development and evaluation of a post-column reaction detector sensitive to platinum(II) complexes is presented in which sodium bisulfite is used as the derivatizing agent with potassium dichromate as an activating agent. The influences of mobile phase changes (i.e., pH, organic modifiers, electrolytes), oxygen, metal ions, and order of reagent addition on reaction kinetics and product yield are defined and used in optimization of detector response. Detection at lambda/sub max/ 290 nm results in an on-line post-column sensitivity of 40-60 ng/mL for selected cis-dichloroplatinum complexes and a sensitivity of 300-1200 ng/mL for four (substituted)-malonato-platinum complexes. The reaction detector is used to monitor the kinetics of aquation of cisplatin (CDDP) and to quantitate CDDP degradation in plasma. As the sensitivity for CDDP in plasma is comparable to that achieved from high pressure liquid chromatography (HPLC) effluent fractionation/off-line flameless ...
The synthesis of (3-{sup 15}N)-labeled adenine has been reported by several groups. Each of these syntheses followed essentially the same route, in which the {sup 15}N is introduced by nitration of 4-bromoimidazole under forcing conditions using ({sup 15}N)-HNO{sub 3}. The authors have devised an alternate route which uses an azo coupling reaction for introduction of the {sup 15}N and proceeds through the intermediacy of (5-{sup 15}N)-labeled 5-aminoimidazole-4-carboxamide (AICA). An unrelated route to the (5-{sup 15}N)-labeled 5-amino-imidazole ribonucleoside (AIRs) was recently reported. AICA is a versatile precursor, which is most commonly used for entry into the guanine or isoguanine families, although it is usually used as the AICA-riboside rather than the heterocycle itself. The authors have found that AICA also can be used for the adenine family by cyclization to hypoxanthine using diethoxymethyl acetate in DMF at reflux. Although these conditions are more vigorous than those ...
The interaction of Pu(IV) and Zr(IV) with citric acid in nitric acid solutions (C/sub HNO/sub 3// greater than 0.1 M) of lithium nitrate was studied by the distribution method in the interval of nitrate ion concentrations from 1 to 6 g-eq/liter. A 40 percent solution of TBP in decane was used as the extraction reagent. It was established that within the range of concentrations studied, complex compounds of plutonium and zirconium are formed: PuHCit/sup 2 +/ and ZrH/sub 2/Cit/sup 3 +/. The concentration equilibrium constants of the reactions of formation of these compounds retain a constant value at constant ionic strength and undergo substantial variation when the total concentration of the nitrate ion in solution is varied. The values of the effective equilibrium constants, calculated considering the change in the activity coefficient of the hydrogen ion, retain a constant value within a wide range of nitrate ion concentrations. It was shown that the effectiveness ...
A number of fragment ion onsets from the photoionization of CH/sub 3/SCCSCH/sub 3/ and CH/sub 3/SSSCH/sub 3/ have been measured. In addition, our experiment has been converted to a molecular beam source which will increase the precision of our measurements. Exhaustive oxidation of the divalent sulfur to sulfonic acids serves to quench the effects of quadrupolar broadening and thereby allowing for quantitative evaluation of structurally similar sulfonic acids. W/sub 1/2/ are reduced to < 25 Hz at 19 MHz (57,500 Gauss). Electronegative substituents shield the /sup 33/S nucleus perhaps imploying more efficient 2p-3d..pi.. backbonding between sulfur and oxygen. ..cap alpha..-Hetero substituents of sulfonyl groups do not influence the shift of the /sup 33/S to a dramatic extent. The exception is the dianion of thiosulfate compared to the dianion of sulfate. Lanthanide shift reagents, (Eu(fod)/sub 3/), are potentially useful in distinguishing sulfonyl /sup 17/O shifts ...
Effect of Limestone, iron ore and red mud as a flux for hot coal gasification wastes was examined as they are regarded easily available, pollution-less and less costly. (1) Fusion behavior of ash-iron ore mixture and ash-limestone mixture approximately coincided with that of the reagent; red mud with low iron purity also coincided when the addition was less than 40%. (2) According to a microscopic observation, localized melting of the ash was observed even at 900 - 950/sup 0/C which was lower than the mpt. by almost more than 100/sup 0/C, which was attributed to the formation of iron-based compound. (3) The softening point reduced down to 1000 - 1050/sup 0/C irrespective of type of ash or ion-based flux; they were in the form of slurry; it formed a slurry state by the localized melting of ashes. (4) At above mpt., most of the ash component minerals are liquid and evaporation of CO/sub 2/ or any low boiling point component gets faster. (8 figs, 2 tabs, 7 refs)
The methodology of the drip procedure of the Standard Test Method for Evaluating the Influence of Thermal Insulation on External Stress Corrosion Cracking Tendency of Austenitic Stainless Steel (ASTM C 692-95a) was used to research the effect of halogens and inhibitors on the external stress corrosion cracking (ESCC) of Type 304 stainless steel as it applies to the insulation industry. Simulated insulation extraction solutions were made with pure chemical reagents for the halogens and inhibitors. The results indicated that sodium silicate compounds that were higher in sodium were more effective for preventing chloride-induced ESCC in Type 304 austenitic stainless steel. Potassium silicate was not as effective as sodium silicate. Fluoride, bromide, and iodide may cause ESCC but they were much less active than chloride and could be effectively inhibited by sodium silicate compound. The addition of fluoride ions to the chloride/sodium silicate systems, at the ...
Experience at SRS, ORNL, BNL, and Georgia Institute of Technology involving irradiated aluminum clad fuel and target elements, as well as studies of non-irradiated aluminum indicate that some types of aluminum assemblies can be kept in a continually well-deionized water atmosphere for up to 25 years without problems. SRS experience ranges from 2.75 years for the L-1.1 charge kept in deionized D[sub 2]O[sup 1] to greater than 10 years for assemblies stored in the Receiving Basin for Off-site Fuel (RBOF)[sup 2]. Experience at Georgia Institute of Technology reactor in Atlanta yielded the longest value of 25 years without problems. The common denominators in all of the reports is that the water is continually deionized to approximately 2 M[Omega] (2 [times] 10[sup 6]ohms) resistivity and the containers for the water are stainless steel or other non-porous material. This resistivity value is equivalent to a value of 0.5 micromhos or microSiemens conductivity and is ...
Experience at SRS, ORNL, BNL, and Georgia Institute of Technology involving irradiated aluminum clad fuel and target elements, as well as studies of non-irradiated aluminum indicate that some types of aluminum assemblies can be kept in a continually well-deionized water atmosphere for up to 25 years without problems. SRS experience ranges from 2.75 years for the L-1.1 charge kept in deionized D{sub 2}O{sup 1} to greater than 10 years for assemblies stored in the Receiving Basin for Off-site Fuel (RBOF){sup 2}. Experience at Georgia Institute of Technology reactor in Atlanta yielded the longest value of 25 years without problems. The common denominators in all of the reports is that the water is continually deionized to approximately 2 M{Omega} (2 {times} 10{sup 6}ohms) resistivity and the containers for the water are stainless steel or other non-porous material. This resistivity value is equivalent to a value of 0.5 micromhos or microSiemens conductivity and is ...
A range of additives has been developed for enhancing grafting yields in a variety of systems initiated by ionizing radiation. Cellulose has been adopted as the predominant naturally occurring model backbone polymer in these studies because of its structural relationship to wood which is the reference substrate for the work reported in the related second part of this paper concerning composites. Some experiments have been performed with the other major naturally occurring polymer, wool. For comparison purposes with synthetic materials, some studies have also been performed with polypropylene as trunk polymer. Styrene has been used as a predominant monomer in grafting with some experiments utilizing the acrulates like methyl methacrylate. The role of solvent in grafting has been evaluated. UV has been used as initiator to replace ionizing radiation for certain experiments. The additives used were mineral acids, lithium salts, multifunctional acrylates and their methacrylate analogues, ...
The history of the urinary test papers does not being in the post-war period. As early as the 1880's some practitioners and pharmacists tried to replace the complicated wet-chemical procedures and apparatus by "dry chemistry." The first popular test paper for sugar and albumin originated in England in 1883. Dry reagents for proving hematuria have been available since the beginning of this century. Until the 1930s a wide palette of commercial urine tests with "modern" brand names was established. A methodological breakthrough was created by the spot test chemistry inaugurated by the Austrian, Fritz Feigl, about 1920. Using the capillary properties of filter paper in enhancing color reactions he founded a new area of analytical chemistry. Many of the pioneers were recruited from Jewish scientists. In this lecture is proposed that their emigration and banishment as well as the Second World War have stopped the development of urinary diagnostics on the European ...
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
This report presents and discusses results from Task 5 of the study ''Fate of Mercury in Synthetic Gypsum Used for Wallboard Production,'' performed at a full-scale commercial wallboard plant. Synthetic gypsum produced by wet flue gas desulfurization (FGD) systems on coal-fired power plants is commonly used in the manufacture of wallboard. The FGD process is used to control the sulfur dioxide emissions which would result in acid rain if not controlled. This practice has long benefited the environment by recycling the FGD gypsum byproduct, which is becoming available in increasing quantities, decreasing the need to landfill this material, and increasing the sustainable design of the wallboard product. However, new concerns have arisen as recent mercury control strategies developed for power plants involve the capture of mercury in FGD systems. The objective of this study is to determine whether any mercury is released into the atmosphere when the ...
A fermentation waste, Corynebacterium glutamicum, was successfully employed as a biosorbent for Reactive Black 5 (RB5) from aqueous solution. This paper initially studied the effect of pretreatment on the biosorption capacity of C. glutamicum toward RB5, using several chemical agents, such as HCl, H{sub 2}SO{sub 4}, HNO{sub 3}, NaOH, Na{sub 2}CO{sub 3}, CaCl{sub 2} and NaCl. Among these reagents, 0.1 M HNO{sub 3} gave the maximum enhancement of the RB5 uptake, exhibiting 195 mg/g at pH 1 with an initial RB5 concentration of 500 mg/l. The solution pH and temperature were found to affect the biosorption capacity, and the biosorption isotherms derived at different pHs and temperatures revealed that a low pH (pH 1) and high temperature (35 deg. C) favored biosorption. The biosorption isotherm was well represented using three-parameter models (Redlich-Peterson and Sips) compared to two-parameter models (Langmuir and Freundlich models). As a result, high correlation ...
The Procedure determining the concentrations of total rare earth and their determination with a new reagent, tribromochlorophosphonazo (CPA-tB), that is 7-[1-(2, 4, 6-tribromo-phenyl) azo]-2-[1-(2-phosphono-4-chloro-phenyl) azo]-chromotropic acid, in high-level liquid waste and some characters of CPA-tB are studied. CPA-tB and its complexes of rare earth elements are stable in the glycol-H_2O system. Adding glycol shifts the absorption spectrum to left and increases the molar extinction coefficient. The molar extinction coefficients are respectively 7.16 x 10"4 (Y), 11.9 x 10"4 (La), 11.7 x 10"4 (Ce, Pr), 11.9 x 10"4 (Nd), 11.6 x 10"4 (Sm, Eu), 11.4 x 10"4 (Gd) and 11.4 x 10"4 (RE) in the glycol-H_2C_2O_4-H_3PO_4-H_2O system at 643 nm. Th interferes severely the determination of total rare earth, and other elements, U(<100 #mu#g), Al(<20 #mu#g), Fe(<400 #mu#g), Ni,Zr(<100 #mu#g respectively) and some anions, MoO_4"2"- (<2800 #mu#g), EDTA(<20 mg), ...
Different technological procedures used for the chemical mining of uranium differ for one thing with a level of the deposit exploitation and for another with the expenditures. It is necessary to find out the highest acceptable value of the costs per unit of production - limit unit costs. This criterion serves both for selection of the minable parts of deposit, and for determination of the exploitation level of the deposit parts. The paper describes a calculation of the costs and their decomposition into the fixed and variable costs. An evaluation of the different variants of the deposit exploitation is based on the variable costs, expressed in the dependence on the parameters of technological procedure. These parameters are either primary, e.g. density of the wells or dosage of reagents, or secondary, e.g. the uranium production. A relation between primary and secondary variables is defined by the technological models. The first economic optimization calculations ...
As a result of the large limestone deposits available in Poland, the low cost of reagent acquisition for the largescale technological use and relatively well-documented processes of flue gas desulfurization (FGD) technologies based on limestone sorbent slurry, wet scrubbing desulfurization is a method of choice in Poland for flue gas treatment in energy production facilities, including power plants and industrial systems. The efficiency of FGD using the above method depends on several technological and kinetic parameters, particularly on the pH value of the sorbent (i.e., ground limestone suspended in water). Consequently, many studies in Poland and abroad address the impact of various parameters on the pH value of the sorbent suspension, such as the average diameter of sorbent particles (related to the limestone pulverization degree), sorbent quality (in terms of pure calcium carbonate [CaCO3] content of the sorbent material), stoichiometric surfeit of CaCO3 in ...
Coal liquefaction investigations required the availability of model compounds for mechanistic investigations. Towards this end, IITRI was funded to develop an approach for the synthesis of one of the target compound. This study was carried out in several phases as outlined here. Initial synthetic investigations on obtaining 2-tetrolol was carried out using high pressure and temperature reduction with Raney nickel catalyst. The next step consisted in incorporation of a hydroxymethyelene group at the C-3 position. This was successfully carried out utilizing 2-tetrolol, formaldehyde, and calcium oxide. An alternate improved method was developed using 3-carboxyl-2-naphthol. This required less time, gave a cheer product in higher yield. Efforts at the introduction of a chloromethylene group only yielded polymeric material or starting material in spite of protection the phenolic group by various groups. They synthesis of 3, 5-dimethyl-6- bromobenzyl chloride was successfully carried out by ...
Coal liquefaction investigations required the availability of model compounds for mechanistic investigations. Towards this end, IITRI was funded to develop an approach for the synthesis of one of the target compound. This study was carried out in several phases as outlined here. Initial synthetic investigations on obtaining 2-tetrolol was carried out using high pressure and temperature reduction with Raney nickel catalyst. The next step consisted in incorporation of a hydroxymethyelene group at the C-3 position. This was successfully carried out utilizing 2-tetrolol, formaldehyde, and calcium oxide. An alternate improved method was developed using 3-carboxyl-2-naphthol. This required less time, gave a cheer product in higher yield. Efforts at the introduction of a chloromethylene group only yielded polymeric material or starting material in spite of protection the phenolic group by various groups. They synthesis of 3, 5-dimethyl-6- bromobenzyl chloride was successfully carried out by ...
One approach in the design of neutral oxotechnetium complexes is based on the simultaneous substitution of a tridentate dianionic ligand and a monodentate monoanionic coligand on a [Tc(V)O]"+"3 precursor. Following this ''mixed ligand'' concept, a novel "9"9"mTc complex with N,N-bis(2-mercaptoethyl)-N'N'-diethylethylenediamine as ligand and 1-octanethiol as coligand is prepared and evaluated as potential brain radiopharmaceutical. Preparation of the complex at tracer level was accomplished by using "9"9"mTc-glucoheptonate as precursor. The substitution was optimized and a coligand/ligand ratio of 5 was selected. Under this conditions the labeling yield was over 80% and a major product (with radiochemical purity > 80%) was isolated by HPLC methods and used for biological evaluation. Chemical characterization at carrier level was developed using the corresponding rhenium complex as structural model. The Re complex was also prepared by substitution method and isolated as a crystalline ...
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, paper electrophoresis ...
The sequence segment 181-200 of the Torpedo nicotinic acetylcholine receptor (nAChR) #alpha#subunit forms a binding site for #alpha#-bungarotoxin (#alpha#-BTX). Synthetic peptides corresponding to the homologous sequences of human, calf, mouse, chicken, frog, and cobra muscle nAChR #alpha#1 subunits were tested for their ability to bind "1"2"5I-#alpha#-BTX, and differences in #alpha#-BTX affinity were determined by using solution (IC_5_0s) and solid-phase (K_ds) assays. Panels of overlapping peptides corresponding to the complete #alpha#1 subunit of mouse and human were also tested for #alpha#-BTX binding, but other sequence segments forming the #alpha#-BTX site were not consistently detectable. The role of a putative vicinal disulfide bound between Cys-192 and -193, relative to the Torpedo sequence, was determined by modifying the peptides with sulfhydryl reagents. Reduction and alkylation of the peptides decreased #alpha#-BTX binding, whereas oxidation of the ...
Tumor-targeted monoclonal antibodies (mAb) might be useful as diagnostic or therapeutic agents when linked to cytotoxic or imaging reagents. Our group is working to test this hypothesis by linking cytocidal and image-producing isotopes to mAb and testing the utility of the radioimmunoconjugates formed in animal model systems. Radioiodines were first employed for these purposes,but unfavorable nuclear properties (half-lives, #gamma#-ray and #beta#-particle energies) and chemical reactivity (deiodination in vivo) limit their utility. Labeling immunoproteins with metallic radionuclides offers more versatility in that the selection of potentially useful radiometals spans the periodic table.Of the metallic radionuclides with physical properties most suited for use with mAb in nuclear medicine, few are more available or desirable than those of bismuth ("2"1"2Bi) and lead ("2"0"3Pb, "2"1"2Pb), as listed in Table 1. "2"1"2Bi or "2"1"2Pb could serve as sources for highly ...
With an objective to clarify the interactions between micropore structure of coal and solvent reagents, a sorption experiment was carried out under solvent saturated vapor pressure. Low-volatile bituminous coal, Pocahontas No. 3 coal, has the aromatic ring structure developed, and makes solvent more difficult to diffuse into coal, hence sorption amount is small. Methanol has permeated since its polarity is high. High-volatile bituminous coal, Illinois No. 6 coal, makes solvent penetrate easily, and the sorption amount was large with both of aromatic and polar solvents. Since brown coal, Beulah Zap coal, contains a large amount of oxygen, and hydrogen bonding is predominant, sorption amount of cyclohexane and benzene having no polarity is small. Methanol diffuses while releasing hydrogen bond due to its polarity, and its sorption amount is large. A double sorption model is available, which expresses the whole sorption amount as a sum of physical sorption amount and ...
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 ...
The sol-gel-immobilized Tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy){sub 3} {sup 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){sub 3} {sup 2+} was immobilized in sol-gel-derived titania (TiO{sub 2})-Nafion nanocomposite films coated on a dual platinum electrode. This method eliminates an extra pump needed for the delivery of Ru(bpy){sub 3} {sup 2+} reagent into a reaction/observation zone in front of photomultiplier tube because the immobilized-Ru(bpy){sub 3} {sup 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 ...
We labelled Lipiodol with yttrium-90 and analysed the biodistribution in rats after intrahepatic arterial injection. An RP-18 column was used to separate {sup 90}Y from strontium-90. {sup 90}Y was retained on the column, which had been pretreated with yttrium-selective extraction reagent, di(2-ethylhexyl) phosphate, while {sup 90}Sr was washed out. A hexadentate nitrogen-donor chelating ligand N,N,N`,N`-tetrakis(2-benzymidazolylmethyl)-1,2-ethanediamine (EDTB) was synthesized by condensation of 1,2-benzenediamine and ethylene diamine tetra-acetic acid (EDTA). Lipiodol was covalently conjugated with EDTB. The final product was obtained by eluting the retained {sup 90}Y from the RP-18 column with EDTB-Lipiodol. Sixteen male rats (Sprague-Dawley) were sacrificed at 1 h, 24 h, 48 h and 72 h (four rats at each time) after injection of approximately 0.1 mCi {sup 90}Y-Lipiodol via the hepatic artery. Samples of liver, spleen, muscle, lung, kidney, bone, whole blood and ...
The novel optical, electronic, and/or magnetic properties of metal and semiconductor nanoparticles have resulted in extensive research on new methods for their preparation. An ideal preparation method would allow the particle size, size distribution, crystallinity, and particle shape to be easily controlled, and would be applicable to a wide variety of material systems. Numerous preparation methods have been reported, each with its inherent advantages and disadvantages; however, an ideal method has yet to emerge. The most widely applied methods for nanoparticle preparation include the sonochemical reduction of organometallic reagents,(1&2) the solvothermal method of Alivisatos,(3) reactions in microemulsions,(4-6) the polyol method (reduction by alcohols),(7-9) and the use of polymer and solgel materials as hosts.(10-13) In addition to these methods, there are a variety of methods that take advantage of the unique properties of a supercritical fluid.(14&15) ...
Tumor imaging using radioiodinated monoclonal antibodies (Mab) suffered from rapid in vivo deiodination. This problem can be circumvented by covalent attachment of a bifunctional chelating group to the Mab followed by chelation with a suitable cationic radionuclide such as In-111. Competition of trace metal contaminants with In-111 for chelating sites, however, is known to lower the labeling yield. Since commercially available reagents may be contaminated with other trace metal ions, the effect of trace metals on Mab-DTPA chelation and the possibility of masking the trace metal effect on the In-111 labeling of Mab-DTPA were, therefore, investigated. Labeling yield of 93% was obtained when 1 mg (20mg/ml) of Mab F(ab')/sub 2/-DTPA (protein to DTPA ratio of --1) was allowed to incubate with 3 mCi In-111 in 2 ml acetate buffer (0.5M, pH 5.5) for 30 min. The yield was drastically decreased to 13-76% when the reactions were carried out with the addition of 1-2 #mu#g of ...
Rabbit antisera raised to human and chicken MHC molecules were used to immunoprecipitate cross-reactive molecules from biosynthetically and cell surface-labeled spleen and/or blood cells of representative vertebrate species. Five major points emerged: 1) There were many nonspecific cross-reactions using these techniques, so various criteria were developed to distinguish these from true MHC-like molecules. 2) Only very small subpopulations of immunogen-specific antibodies cross-reacted with MHC-like molecules in other nonmammalian species. These subpopulations were different for each species and even within a species, sometimes being so limited as to behave like alloantisera. This led to a very scattered pattern of true cross-reactions that sometimes failed to reflect the properties of the bulk antibody population. 3) Antisera containing antibodies to class II beta- and class I alpha-chains cross-reacted better and more widely than those to B-G, class II alpha and, in general, beta ...
Thin, elastic foils of good resistance to the air exposure, patented as wound healing aids, were prepared by evaporation of a blend of lecithin (L) and sodium hyaluronan (H) taken under varying proportions. The contact angle for water, glycerol, formamide, ethylene glycol and diiodomethane, was determined for these foils. The contact angle was correlated against the H:L foil composition. For all liquids but formamide the highest contact angle was noted for the H:L = 2:1 (g g{sup -1}) ratio. The contact angles provided estimation of the work of adhesion. At the same L:H ratio the work of adhesion was the lowest. It was suggested that lecithin cross-linked hyaluronan. Since the work of adhesion of the studied liquids was similar to that of diiodomethane, it could be concluded that almost all functional groups on the foil surface were completely blocked. Perhaps, at H:L = 2:1 (g g{sup -1}) a stoichiometric complex of hyaluronic acid with lecithin was formed, and polar functional groups ...
Technology is being developed for preparing functional materials by synthesizing new functional peptides in which non-natural amino acid needed for the functional manifestation is introduced, and by modifying the surface of a base plate such as silica glass by using such peptides. Activities were conducted in the three areas of (1) creation of functional molecules, (2) materialization technology, and (3) comprehensive investigation and research; the activities were carried out independently and parallelly in the first two areas. In (1), design technique for the structures and functions of peptides was developed, as were conformational control technique, synthesis of peptides having optical/electronic functions, peptide synthesis by an enzyme method, and R and D on introduction of non-natural amino acid into peptides; in (2), element technologies were developed such as substrate forming technique (pattern forming and thin film forming technology), substrate modification technique, ...
Three reactive materials were evaluated at laboratory scale to identify the optimum treatment reagent for use in a Permeable Reactive Barrier Treatment System at Rocky Flats Environmental Technology Site (RFETS). The contaminants of concern (COCS) are uranium, TCE, PCE, carbon tetrachloride, americium, and vinyl chloride. The three reactive media evaluated included high carbon steel iron filings, an iron-silica alloy in the form of a foam aggregate, and a peculiar humic acid based sorbent (Humasorb from Arctech) mixed with sand. Each material was tested in the laboratory at column scale using simulated site water. All three materials showed promise for the 903 Mound Site however, the iron filings were determined to be the least expensive media. In order to validate the laboratory results, the iron filings were further tested at a pilot scale (field columns) using actual site water. Pilot test results were similar to laboratory results; consequently, the iron ...
An improved labeling procedure for peptides attached to organometallic 99mTc(III) '4+1' mixed-ligand complexes in which the radiometal is coordinated by a tripodal tetradentate chelator 2,2',2''-nitrilotriethanethiol (NS3) and a monodentate isocyanide ligand is presented. The labeling procedure was evaluated by the synthesis of [99mTc(NS3)(L2-RGD)]. The containing radiopharmaceutically interesting RGD-peptide cyclo[Arg-Gly-Asp-D-Tyr-Lys] was modified with 4-isocyanobutanoic acid (L2) as linker conjugated to N6-Lys to get the monodentate ligand L2-RGD. The structural identity of the 99mTc-conjugate was confirmed by comparison to a Re reference compound. The Tc- and Re-conjugates had matching retention times under identical HPLC conditions. The 99mTc-labeling was performed in a novel one-step procedure using the eluate of a 99Mo/99mTc generator, NS3, the isocyanide modified peptide, SnCl2, Na2EDTA, mannitol and ascorbic acid in the reaction mixture. Using optimized ...
The purpose was to develop a simplified and reliable method of separating free from antibody-bound ligand using a precipitating antibody linked to a cellulose derivative. Dose-response curves and control sera were set up in parallel for various pituitary and placental polypeptides, steroid hormones, insulin, glucagon, triiodothyronine, thyroxine, angiotensin I, calcitonin, gastrin, cyclic AMP, and digoxin. After first-antibody reactions had reached equilibrium, free and bound ligand were separated using a double-antibody solid-phase system in parallel with conventional methods, including dextran-coated charcoal, double-antibody precipitation, single-antibody solid phase, organic solvents, salt precipitation, and anion-exchange resins. The effect of variations in temperature, incubation time, protein content, pH, and amount of separating material added were studied. The results showed that separation was complete within 1 hr for small ligand molecules and within 2 hr for larger ones. ...
The purpose was to develop a simplified and reliable method of separating free from antibody-bound ligand using a precipitating antibody linked to a cellulose derivative. Dose-response curves and control sera were set up in parallel for various pituitary and placental polypeptides, steroid hormones, insulin, glucagon, triiodothyronine, thyroxine, angiotensin I, calcitonin, gastrin, cyclic AMP, and digoxin. After first-antibody reactions had reached equilibrium, free and bound ligand were separated using a double-antibody solid-phase system in parallel with conventional methods, including dextran-coated charcoal, double-antibody precipitation, single-antibody solid phase, organic solvents, salt precipitation, and anion-exchange resins. The effect of variations in temperature, incubation time, protein content, pH, and amount of separating material added were studied. The results showed that separation was complete within 1 hr for small ligand molecules and within 2 hr for larger ones. ...
To reduce the radiation dose that accumulated on the reactor coolant pump, decontamination work was carried out at the Maanshan Nuclear Power Plant. A four-step alkaline permanganate (AP)-CanDecon process was applied to remove the activity on the turning vane diffuser and pump impeller. The first step consisted of 8 h of AP treatment and 7 h of decontamination. It was followed by 2.5 h of AP treatment and 5 h of decontamination. An average decontamination factor of 2.9 was obtained. To understand the corrosion of the decontaminating reagents on the materials, coupons were installed in the decontamination tank. These were as-received and sensitized 304SS, alloy 600, casting stainless steel (CF-8), stellite-6, and carbon steels (A508 and A533). The exposure rates (mR h"-"1) of the carbon steels were approximately five times higher in magnitude than those of the other materials. The decontamination levels (dpm per 100 cm"2) of the A508 and A533 carbon steels were 5432 ...
beta-Bungarotoxin (beta-Bgt), a presynaptic phospholipase A(2) (PLA(2)) neurotoxin isolated from the venom of Bungarus multicinctus, consists of A chain and B chain. The goal of the present study is to explore the functional contribution of the two subunits to the toxicity of beta-Bgt. beta-Bgt was found to induce apoptotic death of SK-N-SH cells via elevating intracellular Ca(2+) and intracellular ROS production. Moreover, an activation of p38 MAPK was associated with the cytotoxicity of beta-Bgt. SB202190 (p38 MAPK inhibitor), N-acetylcysteine (antioxidant reagent), 1,2-bis(2-aminophenoxy)ethane-N,N,N,N-tetraacetic acid (BAPTA) (Ca(2+) chelator) and the inhibitors of Ca(2+) release from intracellular depots (ruthenium red and 2-aminoethoxydiphenyl borate) effectively attenuated the cytotoxicity of beta-Bgt. In sharp contrast to the inability of A chain, B chain was able to induce cytotoxic effects on SK-N-SH cells as beta-Bgt did. Abolishment of PLA(2) activity ...
Acidic constituents in crude oil are associated with the formation of stable emulsions during production and present a challenge for efficient oil recovery and processing. Acid molecules, including naphthenic acids and acidic sulfur in crude oil cause corrosion in refineries and pipelines. Naphthenic acids are also significant because of their surface activity and marginal water solubility, so that they may leach to wastewaters and cause adverse environmental effects. Acidic components of oil are not limited to carboxylic acids but also molecules that contain sulfur and nitrogen. As such, an improved understanding of the chemistry and physics of petroleum at the molecular level is needed in order to understand the range of problems associated with acidic oil components and to design better solutions. The applications of negative-ion electrospray ionization (ESI) Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) for speciation of acidic oil compound classes was ...
There is very little known about the long-term evolution of the MHC and MHC-like molecules. This is because both the theory (the evolutionary questions and models) and the practice (the animals systems, functional assays and reagents to identify and characterize these molecules) have been difficult to develop. There is no molecular evidence yet to decide whether vertebrate immune systems (and particularly the MHC molecules) are evolutionarily related to invertebrate allorecognition systems, and the functional evidence can be interpreted either way. Even among the vertebrates, there is great heterogeneity in the quality and quantity of the immune response. The functional evidence for T-lymphocyte function in jawless and cartilagenous fish is poor, while the bony fish seem to have many characteristics of a mammalian immune system. The organization and sequence of fish Ig genes also indicate that important events in the evolution of the immune system and the MHC ...
One of the refinements of modern Nuclear Medicine is the capacity of providing dynamic and kinetics images of the administered radiopharmaceutical, reproducing its transport mechanism, action sites, receptor binding and excretion route. With the continues technological advances new radiopharmaceuticals have been developed in order to express higher specificity and with higher characters of affinity between receptor/complex. One radiopharmaceutical is formed by a reagent or bio molecule that has in its structure a radioisotope, that has the objectives of carrying it to the organs of affinity or to benign or malign tumoral process. Somatostatin inhibits the growing and proliferation of several tumoral cells. Somatostatin analogs bind to somatostatic receptors that are expressed in different kind of neoplasia DOTA-LANREOTIDE (DOTALAN) is an octapeptide analog to somatostatin. The interest of labeling the bio conjugate with gallium-67 in Nuclear Medicine comes from its ...
Crystallization procedure is considered to have adaptability to new reprocessing process based on the PUREX process because it has an advantage in recovering rather pure uranium from contaminated uranium solution without reagent. NEXT (New Extraction System for TRU Recovery) process has been developed by JNC, and applying the crystallization process unit to NEXT process has a capability to contribute to an improvement of economical efficiency and reduction of liquid waste in NEXT process. Thus following studies were carried out. In crystallization process unit, UNH (Uranyl Nitrate Hydrate)-crystals are washed by a nitric acid solution to get high decontamination factor, but the data on UNH-crystals dissolution by washing procedure is insufficient to evaluate the effectiveness of crystallization process unit. So, in this study, the effect of a nitric acid concentration to UNH-crystals dissolution and decontamination factor was tested. As results, it was found that ...
The improving uranium extraction efficiency of yellow cake production from shale deposit by acid pugging and curing with D263B resin adsorption is described in this paper. The analysis and examination show that the composition of uranium minerals in one of uranium ores is very complex, which directly influence the extraction efficiency of uranium and processing technology. Conventional experimental results indicate that uranium leaching efficiency is changed between 50?60% by conventional agitation method. In this case, acid pugging and curing experiments are employed in order to improving the extraction efficiency. A series of acid pugging and curing experiments are carried out to get parameters for heap leaching in pilot plant experiment. The experiment results by acid pugging and curing technology showed that uranium leaching efficiency can reach to 90% of extraction efficiency mixed with 1% manganese dioxide, 12% sulfuric acid pugging, curing 3 days and leached out with 5 g.L-1 ...
Immunoassays are versatile analytical techniques that had a leading role in various clinical applications, during the last four decades. The studies carried out by Rosalyn Yalow, Solomon Berson and Roger Ekins in the 1960s gave a breakthrough in the development of this novel analytical method. Sensitivity up to femtomolar concentrations, high specificity and universal application to different classes of molecular species made immunoassay a very useful tool in analytical investigation. The expertise acquired by immunochemists in producing antibodies against any antigen and the ability of radiochemists in labeling the antigens with "1"2"5I without affecting the active site are the two main factors responsible for the above development. There are concerns about the safety and health of humans due to the high-level contamination of environment by pesticides, industrial compounds and metals, anabolic steroids in milk and meat products, and presence of mycotoxins in food and feed ...