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Sample records for radiochemical reagent determination

  1. Determination of Np-237 by radiochemical neutron activation analysis combined with extraction chromatography.

    PubMed

    Kalmykov, St N; Aliev, R A; Sapozhnikov, D Yu; Sapozhnikov, Yu A; Afinogenov, A M

    2004-01-01

    A procedure for determination of 237Np, 238Pu, 239,240Pu and 241Pu in environmental samples is described. Neptunium-237 is determined using radiochemical neutron activation analysis with pre- and post-irradiation chemistry based on solvent extraction and extraction chromatography. 238Pu, 239,240Pu is determined using alpha spectrometry and 241Pu by liquid scintillation spectrometry. The vertical profiles of 237Np, 238Pu, 239,240Pu in bottom sediments from the Black Sea are presented.

  2. Phosphorus Determination by Derivative Activation Analysis: A Multifaceted Radiochemical Application.

    ERIC Educational Resources Information Center

    Kleppinger, E. W.; And Others

    1984-01-01

    Although determination of phosphorus is important in biology, physiology, and environmental science, traditional gravimetric and colorimetric methods are cumbersome and lack the requisite sensitivity. Therefore, a derivative activation analysis method is suggested. Background information, procedures, and results are provided. (JN)

  3. Phosphorus Determination by Derivative Activation Analysis: A Multifaceted Radiochemical Application.

    ERIC Educational Resources Information Center

    Kleppinger, E. W.; And Others

    1984-01-01

    Although determination of phosphorus is important in biology, physiology, and environmental science, traditional gravimetric and colorimetric methods are cumbersome and lack the requisite sensitivity. Therefore, a derivative activation analysis method is suggested. Background information, procedures, and results are provided. (JN)

  4. Protein binding studies with radiolabeled compounds containing radiochemical impurities. Equilibrium dialysis versus dialysis rate determination

    SciTech Connect

    Honore, B.

    1987-04-01

    The influence of radiochemical impurities in dialysis experiments with high-affinity ligands is investigated. Albumin binding of labeled decanoate (97% pure) is studied by two dialysis techniques. It is shown that equilibrium dialysis is very sensitive to the presence of impurities resulting in erroneously low estimates of the binding affinity and in inconsistent results at varying albumin concentrations. Dialysis rate determination is less sensitive to impurities.

  5. Radio-UHPLC: a tool for rapidly determining the radiochemical purity of technetium-99m radiopharmaceuticals?

    PubMed

    Kryza, David; Janier, Marc

    2013-08-01

    Determining the radiochemical purity (RCP) of technetium-99m ((99m)Tc) radiopharmaceuticals using the method described in the package insert is a time-consuming process, requiring particular attention in order to achieve accurate RCP results. The purpose of this study was to evaluate whether radio-ultra high performance liquid chromatography (radio-UHPLC) may be an alternative method for RCP testing of (99m)Tc-tetrofosmin, (99m)Tc-MAG3 and (99m)Tc-sestamibi. Results obtained using radio-UHPLC were in excellent agreement with the standard method, with total analysis time being reduced to less than 3 min.

  6. Quantitative radiochemical method for determination of major sources of natural radioactivity in ores and minerals

    USGS Publications Warehouse

    Rosholt, J.N.

    1954-01-01

    When an ore sample contains radioactivity other than that attributable to the uranium series in equilibrium, a quantitative analysis of the other emitters must be made in order to determine the source of this activity. Thorium-232, radon-222, and lead-210 have been determined by isolation and subsequent activity analysis of some of their short-lived daughter products. The sulfides of bismuth and polonium are precipitated out of solutions of thorium or uranium ores, and the ??-particle activity of polonium-214, polonium-212, and polonium-210 is determined by scintillation-counting techniques. Polonium-214 activity is used to determine radon-222, polonium-212 activity for thorium-232, and polonium-210 for lead-210. The development of these methods of radiochemical analysis will facilitate the rapid determination of some of the major sources of natural radioactivity.

  7. Selenium determination in whole human blood by radiochemical neutron activation analysis: preliminary results in Argentina.

    PubMed

    Hevia, Sonia Edith; Martín de Portela, María Luz Pita; Resnizky, Sara Manuela

    2002-09-01

    In Argentina there are no values regarding the content selenium in food or its effect on nutritional status. Neutron activation analysis and a radiochemical separation scheme for selenium has been adjusted for blood samples from healthy adult individuals. Fasting whole blood was collected, lyophilized, packed, and irradiated in a nuclear reactor. Selenium was determined by a radiochemical separation. The method was validated using certified reference materials. The selenium concentrations (mean value +/- SD) from five pools and from 22 individual samples were 0.070 +/- 0.020 microgram/ml and 0.071 +/- 0.014 microgram/ml, respectively, ranging between 0.047 to 0.105 microgram/ml. These preliminary results show values close to those published for the population living in areas with adequate selenium intake, but lower values than those published for the USA population. However, it will be necessary to carry out nutritional status studies in other areas of Argentina, taking into account the geographic and topographic diversity of the country.

  8. Quantitative radiochemical methods for determination of the sources of natural radioactivity

    USGS Publications Warehouse

    Rosholt, J.N.

    1957-01-01

    Study of the state of equilibrium of any natural radioactive source requires determination of several key nuclides or groups of nuclides to find their contribution to the total amount of radioactivity. Alpha activity measured by scintillation counting is used for determination of protactinium-231, thorium-232, thorium-230, and radium-226. The chemical procedures for the separations of the specific elements are described, as well as the measurement techniques used to determine the abundances of the individual isotopes. To correct for deviations in the ore standards, an independent means of evaluating the efficiencies of the individual separations and measurements is used. The development of these methods of radiochemical analysis facilitates detailed investigation of the major sources of natural radioactivity.

  9. The variable reagent blank: protein determination as a model.

    PubMed

    Bozimowski, D; Artiss, J D; Zak, B

    1985-10-01

    Three total protein assays were analyzed to determine the extent of deviation encountered when a constant measured reagent blank is compared to a continuously decreasing true reagent blank. This blank effect owes its regressive nature to the consumption of the active reagent ingredient by the protein reactive species, variably and sometimes, with certain reactants, nonlinearly in the presence of increasing protein concentrations. However, the blank effect of interest here is apparent only when the reagent and the reagent-protein complex present overlapping spectra and therefore absorb at the wavelength of measurement. Thus it was found that while the biuret and the Coomassie brilliant blue assays produced pronounced differences in the variable true reagent blanks, the Folin-Ciocalteau reaction did not develop a deviation from the true blank since the reagent blank does not absorb to any extent at the assay wavelength. In this manner, the latter procedure could serve as a marker against which the former two blank reactions can be shown to display relatively excessive deviations.

  10. (Radiochemical limnology)

    SciTech Connect

    Olsen, C.R.

    1989-09-27

    The 24th Congress of the International Association of Theoretical and Applied Limnology (SIL) was organized to provide an opportunity for about 2000 scientists representing more than 50 countries to present and discuss their research results on theoretical and applied limnology. The traveler was a co-organizer and co-chair of a special workshop/symposium at this meeting entitled Radiochemical Limnology.''

  11. Radiochemical determination of 237NP in soil samples contaminated with weapon grade plutonium

    NASA Astrophysics Data System (ADS)

    Antón, M. P.; Espinosa, A.; Aragón, A.

    2006-01-01

    The Palomares terrestrial ecosystem (Spain) constitutes a natural laboratory to study transuranics. This scenario is partially contaminated with weapon-grade plutonium since the burnout and fragmentation of two thermonuclear bombs accidentally dropped in 1966. While performing radiometric measurements in the field, the possible presence of 237Np was observed through its 29 keV gamma emission. To accomplish a detailed characterization of the source term in the contaminated area using the isotopic ratios Pu-Am-Np, the radiochemical isolation and quantification by alpha spectrometry of 237Np was initiated. The selected radiochemical procedure involves separation of Np from Am, U and Pu with ionic resins, given that in soil samples from Palomares 239+240Pu levels are several orders of magnitude higher than 237Np. Then neptunium is isolated using TEVA organic resins. After electrodeposition, quantification is performed by alpha spectrometry. Different tests were done with blank solutions spiked with 236Pu and 237Np, solutions resulting from the total dissolution of radioactive particles and soil samples. Results indicate that the optimal sequential radionuclide separation order is Pu-Np, with decontamination percentages obtained with the ionic resins ranging from 98% to 100%. Also, the addition of NaNO2 has proved to be necessary, acting as a stabilizer of Pu-Np valences.

  12. Determination of uranium, thorium, and 18 other elements in high-purity molybdenum by radiochemical neutron activation analysis

    SciTech Connect

    Theimer, K.H.; Krivan, V. )

    1990-12-15

    A radiochemical neutron activation analysis technique for the determination of uranium and thorium in high-purity molybdenum via the indicator radionuclides {sup 239}Np for U and {sup 233}Pa for Th has been developed. Simultaneously, the elements Ag, Co, Cr, Cs, Cu, Fe, Ga, In, Ir, K, Mn, Na, Ni, Rb, Ru, Sc, Se, and Zn can be determined, too. The elements Hf, Sb, Ta, Sn, and W were determined by instrumental neutron activation analysis. The radiochemical separation is performed by anion exchange on a Dowex 1 {times} 8 column from a 20 M HF/3% H{sub 2}O{sub 2} medium. A limit of detection of 4 ng/g for uranium and 40 pg/g for thorium can be achieved. For the other elements, the limits of detection are between 1 pg/g and 100 ng/g. A modified more selective separation of the indicator radionuclide of Th, {sup 233}Pa, allows improvement of the limit of detection for Th by a factor up to 5. This technique was applied to the analysis of high-purity molybdenum, and the results of a number of elements were compared with those of other techniques.

  13. Determination of trace halogens in rock samples by radiochemical neutron activation analysis coupled with the k0-standardization method.

    PubMed

    Ozaki, Hiromasa; Ebihara, Mitsuru

    2007-02-05

    Radiochemical neutron activation analysis coupled with the k0-standardization method (k0-RNAA method) was applied to silicate rock samples for the simultaneous determination of trace halogens (Cl, Br and I). Analytical results obtained by the k0-RNAA method for geological standard rocks and meteorite samples agreed with those determined by the conventional comparison method conducted in the same set of experiments, suggesting that the k0-RNAA method is as reliable as the conventional method. Our data for these samples are in good agreement with their literature values except for rare cases. Detection limits calculated under the present experimental condition are sufficiently low for Cl and Br but not for I for typical geologic and meteoritic samples. The k0-RNAA method coupled with longer neutron-irradiation is expected to yield satisfactorily low detection limits for halogens including I in these samples.

  14. Evaluation of radiochemical neutron activation analysis methods for determination of arsenic in biological materials.

    PubMed

    Paul, Rick L

    2011-01-01

    Radiochemical neutron activation analysis (RNAA) with retention on hydrated manganese dioxide (HMD) has played a key role in the certification of As in biological materials at NIST. Although this method provides very high and reproducible yields and detection limits at low microgram/kilogram levels, counting geometry uncertainties may arise from unequal distribution of As in the HMD, and arsenic detection limits may not be optimal due to significant retention of other elements. An alternate RNAA procedure with separation of arsenic by solvent extraction has been investigated. After digestion of samples in nitric and perchloric acids, As(III) is extracted from 2 M sulfuric acid solution into a solution of zinc diethyldithiocarbamate in chloroform. Counting of (76)As allows quantitation of arsenic. Addition of an (77)As tracer solution prior to dissolution allows correction for chemical yield and counting geometries, further improving reproducibility. The HMD and solvent extraction procedures for arsenic were compared through analysis of SRMs 1577c (bovine liver), 1547 (peach leaves), and 1575a (pine needles). Both methods gave As results in agreement with certified values with comparable reproducibility. However, the solvent extraction method yields a factor of 3 improvement in detection limits and is less time-consuming than the HMD method. The new method shows great promise for use in As certification in reference materials.

  15. Densitometric determination of (+)-catechin and (-)-epicatechin by 4-dimethylaminocinnamaldehyde reagent.

    PubMed

    Glavnik, Vesna; Simonovska, Breda; Vovk, Irena

    2009-05-15

    We report the optimization of a sensitive, selective and robust derivatization method using 4-dimethylaminocinnamaldehyde (DMACA) for densitometric determination of (+)-catechin and (-)-epicatechin. The separation of these compounds was achieved by thin-layer chromatography (TLC) on cellulose plates developed with water. With DMACA in HCl, both compounds gave blue bands, while under the same conditions, vanillin produced a fast fading red coloration of bands. Quantitation at 655nm showed that for both compounds the calibration curve was linear from 2 to 12ng and polynomial from 2 to 30ng, and the repeatability of chromatography of 20ng was 3.5% (RSD, n=6). The visible limit of detection of both standards was 1ng, but the densitometric limit of detection was lower (0.2ng). The optimized DMACA reagent is superior to the more frequently used vanillin reagent and is applicable also for determination of mixtures containing other catechins ((-)-catechin, (-)-epicatechin gallate, (-)-epigallocatechin gallate, procyanidin A2, procyanidin B1 and procyanidin B2).

  16. Arsenazo III as a spectrophotometric reagent for determination of lead.

    PubMed

    Michaylova, V; Kuleva, N

    1980-01-01

    Arsenazo III is proposed as a spectrophotometric reagent for the determination of lead. The complex formation begins at pH > 2 and is greatest at pH 4-6. The molar absorptivity of the complex has a mean value of 2.8 x 10(4) 1.mole(-1).cm(-1) at 600 nm and remains nearly constant in the pH range 4-8. The ionic species taking part in the reaction are studied and the equilibrium constants for the different possible reactions are calculated. According to the values obtained, the reaction of PbOH(+) with H(5)L(3-) is predominant. The reaction studied is applied for the determination of micro amounts of lead in technical aluminium.

  17. SAM Radiochemical Methods Query

    EPA Pesticide Factsheets

    Laboratories measuring target radiochemical analytes in environmental samples can use this online query tool to identify analytical methods in EPA's Selected Analytical Methods for Environmental Remediation and Recovery for select radiochemical analytes.

  18. Quercetin as colorimetric reagent for determination of zirconium

    USGS Publications Warehouse

    Grimaldi, F.S.; White, C.E.

    1953-01-01

    Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50?? of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K1 = 0.33 ?? 10-5 and K2 = 1.3 ?? 10-9. Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

  19. Kinetic spectrophotometric determination of certain cephalosporins using oxidized quercetin reagent

    NASA Astrophysics Data System (ADS)

    Saleh, Gamal A.; El-Shaboury, Salwa R.; Mohamed, Fardous A.; Rageh, Azza H.

    2009-09-01

    A simple, precise and accurate kinetic spectrophotometric method for determination of cefoperazone sodium, cefazolin sodium and ceftriaxone sodium in bulk and in pharmaceutical formulations has been developed. The method is based upon a kinetic investigation of the reaction of the drug with oxidized quercetin reagent at room temperature for a fixed time of 30 min. The decrease in absorbance after the addition of the drug was measured at 510 nm. The absorbance concentration plot was rectilinear over the range 80-400 μg mL -1 for all studied drugs. The concentration of the studied drugs was calculated using the corresponding calibration equation for the fixed time method. The determination of the studied drugs by initial rate, variable time and rate-constant methods was feasible with the calibration equations obtained but the fixed time method has been found to be more applicable. The analytical performance of the method, in terms of accuracy and precision, was statistically validated; the results were satisfactory. The method has been successfully applied to the determination of the studied drugs in commercial pharmaceutical formulations. Statistical comparison of the results with a well established reported method showed excellent agreement and proved that there is no significant difference in the accuracy and precision.

  20. Rapid radiochemical method for determination of actinides in emergency concrete and brick samples.

    PubMed

    Maxwell, Sherrod L; Culligan, Brian K; Kelsey-Wall, Angel; Shaw, Patrick J

    2011-09-02

    A new rapid method for the determination of actinides in emergency concrete and brick samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations or for routine analysis. If a radiological dispersive device (RDD), Improvised Nuclear Device (IND) or nuclear accident occurs, there will be a urgent need for rapid analyses of many different environmental matrices, including building materials such as concrete and brick, to support dose mitigation and environmental clean-up. The new method for actinides in concrete and brick method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride matrix removal step, and a column separation process with stacked TEVA, TRU and DGA Resin cartridges. Alpha emitters are prepared using rare earth microprecipitation for counting by alpha spectrometry. The method showed high chemical recoveries and effective removal of interferences. The determination of actinides in concrete and brick sample analysis can be performed in less than 8h with excellent quality for emergency samples. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory actinide particles are effectively digested.

  1. A radio-high-performance liquid chromatography dual-flow cell gamma-detection system for on-line radiochemical purity and labeling efficiency determination.

    PubMed

    Lindegren, S; Jensen, H; Jacobsson, L

    2014-04-11

    In this study, a method of determining radiochemical yield and radiochemical purity using radio-HPLC detection employing a dual-flow-cell system is evaluated. The dual-flow cell, consisting of a reference cell and an analytical cell, was constructed from two PEEK capillary coils to fit into the well of a NaI(Tl) detector. The radio-HPLC flow was directed from the injector to the reference cell allowing on-line detection of the total injected sample activity prior to entering the HPLC column. The radioactivity eluted from the column was then detected in the analytical cell. In this way, the sample will act as its own standard, a feature enabling on-line quantification of the processed radioactivity passing through the system. All data were acquired on-line via an analog signal from a rate meter using chromatographic software. The radiochemical yield and recovery could be simply and accurately determined by integration of the peak areas in the chromatogram obtained from the reference and analytical cells using an experimentally determined volume factor to correct for the effect of different cell volumes. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Determination of the radiochemical purity of (99m) Tc medronate injection by thin layer chromatography on iTLC-SG: effect of medronate concentration on the value measured.

    PubMed

    Cunnane, Caroline M; O'Brien, Lesley M; Waight, Lynn A; Millar, Alistair M

    2013-05-15

    When using iTLC-SG thin layer chromatography plates to measure radiochemical impurities in (99m) Tc medronate, falsely high values were obtained for (99m) Tc pertechnetate impurity. Preliminary investigations indicated that the mass of (99m) Tc medronate applied to the plate influences the value. The goal of this study was to determine if the concentration of medronate influences the value obtained for (99m) Tc pertechnetate impurity. (99m) Tc medronate was prepared at two concentrations: 4 mg/mL and 0.2 mg/mL. Impurity levels were measured using three stationary phases: dried and undried iTLC-SG and 54SFC paper. Two mobile phases were used: methyl ethyl ketone to detect (99m) Tc pertechnetate and sodium acetate 136 g/L to detect hydrolysed and colloidal (99m) Tc. Sample spot drying and volume were also investigated. With 4 mg/mL samples, the three stationary phases measured similar impurity levels (p > 0.05). With the 0.2 mg/mL samples, higher levels of (99m) Tc pertechnetate were measured with iTLC-SG than with paper (p < 0.05). Neither sample spot drying nor volume was found to affect impurity levels measured. When using iTLC-SG to measure the radiochemical purity of (99m) Tc medronate, an artefactually high level of (99m) Tc pertechnetate impurity is measured when the medronate concentration in the sample is low. The iTLC-SG stationary phase may be unsatisfactory for measuring the radiochemical purity of (99m) Tc medronate. Copyright © 2013 John Wiley & Sons, Ltd.

  3. Determination of sulfur in fly ash and fuel oil standard reference materials by radiochemical neutron activation analysis and liquid scintillation counting

    SciTech Connect

    Li, M.; Filby, R.H.

    1983-12-01

    Sulfur was determined in NBS Coal Fly Ash (SRM 1633) and Residual Fuel Oils (SRM's 1619, 1620a, 1634a) by radiochemical neutron activation analysis (NAA) using the /sup 34/S(n,..gamma..)/sup 35/S reaction. The /sup 35/S was separated from solutions of the standards by either cation-anion exchange on Dowex 50W-X8/Dowex 1-X8 or by adsorption on Al/sub 2/O/sub 3/. Liquid scintillation counting of aqueous solutions was used for /sup 35/S measurement. The /sup 35/Cl(n,p)/sup 35/S interference was corrected for by measurement of chlorine by instrumental NAA. The method may be applied to very small samples of fly ash or air particulates (<10/sup -3/ g). 1 figure, 5 tables.

  4. Neotetrazolium chloride: a new reagent for spectrophotometric determination of manganese.

    PubMed

    Kamburova, M

    1998-08-01

    The interaction of Mn(VII) and the Neotetrazolium chloride has been examined. The ion-associate formed is extracted into 1,2di-chloroethane. The optimum conditions have been established. The molar absorptivity of the complex is (9.1+/-0.08)x10(5) l mol(-1) cm(-1). The sensitivity of the method is 6.04x1010(-5) mug cm(-2). It is possible to extract and determine manganese in the presence of large number of cations and anions. The characteristic values for the extraction and the aqueous phase equilibria were determined: extraction constant K(ex)=3.21x10(9), distribution constant K(D)=33 and association constant beta=9.72x10(7). The method is applicable to analysis of soils and steels.

  5. Kinetic control of reagent dissolution for the flow injection determination of iron at trace levels.

    PubMed

    Bruno, Hernán A; Andrade, Francisco J; Luna, Pablo C; Tudino, Mabel B

    2002-07-01

    A novel methodology for the determination of iron at the ppb level by spectrophotometric flow injection analysis is described. The method is based on the control of the flow dissolution of the colorimetric reagent 1,10-phenanthroline. This is achieved by means of the minimization of the area of contact between the carrier and the solid reagent, thus allowing the use of the fairly soluble organic compound without affecting the reactor lifetime. The reagent is melted inside an acrylic column (3.0 x 0.5 cm id) in such a way that a hollow space is left in the center after cooling. This new design improves some aspects of the performance of the classical solid-phase reactors as no problems related to the increase in the backpressure of the system are evidenced. Furthermore, the total reagent loading of the column is increased as no inert support is needed. A comparison between the performance of this novel methodology and that of the conventional packed reactor was performed and several advantages were observed: the use of higher flow rates, an increase in the reactor lifetime and a decrease in reagent consumption. A mathematical model to fit the concentration profiles of the dissolved reagent as a function of the residence time of the sample within the column is presented. The application of this strategy to the determination of Fe(II) improves the figures of merit in comparison to those obtained with a single-line homogeneous system: the limit of detection is 2 microg Fe L(-1) (3s) and the sensitivity is similar to that of the batch procedure. Results obtained for the determination of iron in natural waters are also presented.

  6. Reagents regeneration flow injection analysis (RRFIA) for spectrophotometric determination of methamphetamine coupled with solvent extraction.

    PubMed

    Teshima, Norio; Fukui, Nobukazu; Sakai, Tadao

    2005-12-15

    Methamphetamine (MPA), being a stimulant drug, reacts with tetrabromophenolphthalein ethyl ester (TBPEH) to form a red-violet ion associate, TBPEHMPA, in 1,2-dichloroethane (DCE) at pH 9. The maximum absorption wavelength was at 570nm. After measuring, yellow TBPEH with DCE could be regenerated by mixing with the buffer solution at pH 3. The regenerated TBPEH/DCE could be reused as an ion association reagent and extracting solvent. In addition, the reagent regeneration could be performed by the on-line flow injection system and the cyclic flow injection analysis system was demonstrated for the determination of MPA without consumption of ion association reagent and organic solvent. The calibration curve was linear in the range of 0.5-3.5x10(-5)M with good repeatability. The sample throughput was 20h(-1).

  7. A reagent-free tubular biofilm reactor for on-line determination of biochemical oxygen demand.

    PubMed

    Liu, Changyu; Zhao, Huijun; Gao, Shan; Jia, Jianbo; Zhao, Limin; Yong, Daming; Dong, Shaojun

    2013-07-15

    We reported a reagent-free tubular biofilm reactor (BFR) based analytical system for rapid online biochemical oxygen demand (BOD) determination. The BFR was cultivated using microbial seeds from activated sludge. It only needs tap water to operate and does not require any chemical reagent. The analytical performance of this reagent-free BFR system was found to be equal to or better than the BFR system operated using phosphate buffer saline (PBS) and high purity deionized water. The system can readily achieve a limit of detection of 0.25 mg O2 L(-1), possessing superior reproducibility, and long-term operational and storage stability. More importantly, we confirmed for the first time that the BFR system is capable of tolerating common toxicants found in wastewaters, such as 3,5-dichlorophenol and Zn(II), Cr(VI), Cd(II), Cu(II), Pb(II), Mn(II) and Ni(II), enabling the method to be applied to a wide range of wastewaters. The sloughing and clogging are the important attributes affecting the operational stability, hence, the reliability of most online wastewater monitoring systems, which can be effectively avoided, benefiting from the tubular geometry of the reactor and high flow rate conditions. These advantages, coupled with simplicity in device, convenience in operation and minimal maintenance, make such a reagent-free BFR analytical system promising for practical BOD online determination.

  8. Radiochemical solar neutrino experiments

    NASA Astrophysics Data System (ADS)

    Gavrin, V. N.; Cleveland, B. T.

    2011-12-01

    Radiochemical experiments have been crucial to solar neutrino research. Even today, they provide the only direct measurement of the rate of the proton-proton fusion reaction, p+p→d+e++νe, which generates most of the Sun's energy. We first give a little history of radiochemical solar neutrino experiments with emphasis on the gallium experiment SAGE - the only currently operating detector of this type. The combined result of all data from the Ga experiments is a capture rate of 67.6±3.7 SNU. For comparison to theory, we use the calculated flux at the Sun from a standard solar model, take into account neutrino propagation from the Sun to the Earth and the results of neutrino source experiments with Ga, and obtain 67.3-3.5+3.9 SNU. Using the data from all solar neutrino experiments we calculate an electron neutrino pp flux of ϕpp♁=(3.41-0.77+0.76)×1010/(cm-s), which agrees well with the prediction from a detailed solar model of ϕpp♁=(3.30-0.14+0.13)×1010/(cm-s). Four tests of the Ga experiments have been carried out with very intense reactor-produced neutrino sources and the ratio of observed to calculated rates is 0.88±0.05. One explanation for this unexpectedly low result is that the cross section for neutrino capture by the two lowest-lying excited states in 71Ge has been overestimated. We end with consideration of possible time variation in the Ga experiments and an enumeration of other possible radiochemical experiments that might have been.

  9. A quantitative radiochemical method for the determination of the major sources of natural radioactivity in ores and minerals

    USGS Publications Warehouse

    Rosholt, John Nicholas

    1953-01-01

    The determination of Th232, Rn222, and Pb210 by isolation and subsequent activity analysis of some of their short-lived daughter products is described. The sulfides of bismuth and polonium are precipitated out of solutions of thorium or uranium ores, and the alpha particle activity of PO214. PO212 and PO210 is determined by scintillation counting techniques. PO214 activity is used to determine Rn222, PO212 activity for Th232, and PO210 for Pb210.

  10. Chemical Treatment of US Department of Energy High Level and Low Level Waste to Obtain a Pure Radiochemical Fraction for Determination of Californium Alpha-Decay Content

    SciTech Connect

    Dewberry, R.

    2002-12-02

    We have developed a chemical separation technique that allows the radiochemical determination of the californium a-decay content in Department of Energy (DOE) high level wastes from the Hanford and Savannah River sites. The chemical separation technique uses a series of column extraction chromatography steps that use Eichrom Industries' lanthanide and actinide plus 3 oxidation state selective Ln-resin(R) and the transuranic selective plus 4 oxidation state TRU-resin(R) to obtain intermediate product phases in dilute nitric acid. The technique has been demonstrated on three types of authentic DOE high and low level waste samples. We obtain discrimination from Pu a-activity by a factor of over 200 and from Cm-244 a-activity by a factor approaching 1700. Californium recoveries are measured by addition of a Cf-249 spike and are in the range of 50 percent to 90 percent in the synthetic samples and are in the range of 1.4 percent to 48 percent for the authentic DOE waste samples.

  11. Flow injection spectrophotometry using natural reagent from Morinda citrifolia root for determination of aluminium in tea.

    PubMed

    Tontrong, Sopa; Khonyoung, Supada; Jakmunee, Jaroon

    2012-05-01

    A flow injection (FI) spectrophotometric method with using natural reagent extracted from Morinda citrifolia root has been developed for determination of aluminium. The extract contained anthraquinone compounds which could react with Al(3+) to form reddish complexes which had maximum absorption wavelength at 499.0nm. The extract could be used as a reagent in FI system without further purification to obtain pure compound. A sensitive method for determination of aluminium in concentration range of 0.1-1.0mgL(-1), with detection limit of 0.05mgL(-1) was achieved. Relative standard deviations of 1.2% and 1.7% were obtained for the determination of 0.1 and 0.6mgL(-1) Al(3+) (n=11). Sample throughput of 35h(-1) was achieved with the consumption of 3mL each of carrier and reagent solutions per injection. The developed method was successfully applied to tea samples, validated by the FAAS standard method. The method is simple, fast, economical and could be classified as a greener analytical method.

  12. 1-Phenyl-3-methyl-4-benzoylpyrazol-5-one as a group-extraction reagent for spectrophotometric determination of trace elements.

    PubMed

    Mirza, M Y; Nwabue, F I

    1981-01-01

    1-Phenyl-3-methyl-4-benzoylpyrazol-5-one has been examined as a regent for detection and solvent extraction of metal ions. The reagent seems to be promising as a group-extraction reagent for the spectrophotometric determination of copper, nickel, cobalt, manganese, zinc, chromium(VI) and molybdenum(VI).

  13. DETERMINATION OF PHTHALATES IN WATER AND SOIL BY TANDEM MASS SPECTROMETRY UNDER CHEMICAL IONIZATION CONDITIONS WITH ISOBUTANE AS REAGENT GAS

    EPA Science Inventory

    Phthalate determination is important because phthalates often are major impurities in samples and can have significant health effects. Tandem mass spectrometry under chemical ionization mass spectrometry conditions with isobutane as the reagent gas was used to determine 11 phthal...

  14. Comparative studies on sulfhydryl determination of soy protein using two aromatic disulfide reagents and two fluorescent reagents.

    PubMed

    Ruan, Qijun; Chen, Yeming; Kong, Xiangzhen; Hua, Yufei

    2013-03-20

    In this study, the sulfhydryl (SH) contents of unheated and heated (90 °C, 5 min) soy protein were detected under different conditions (pH, reagent addition order, SDS/GuHCl concentration, EDTA) using two aromatic disulfide reagents: 5,5'-dithiobis(2-nitrobenzoic acid) (DTNB) and 4,4'-dithiodipyridine (DPS). Two fluorescent alkylating reagents, monobromobimane (mBBr) and N-(1-pyrenyl)maleimide (NPM), were chosen due to their high sensitivity and were also used. Amino acid analysis was used to detect the SH (cysteine) contents of unheated (7.51 ± 0.45 μmol SH/g protein) and heated (1.47 ± 0.10 μmol SH/g protein) soy protein, and similar results were obtained using enzymatic hydrolysis-assisted DPS. The SH content detected by DTNB was affected by pH, denaturant species, and denaturant concentration, and the best results were obtained at pH 7.0 when 6 M GuHCl was added after DTNB. These results were lower than that of the amino acid analysis, however. The SH detected by DPS was not as affected as that of DTNB by pH, denaturant species, and denaturant concentration. Additionally, the results of the amino acid analysis were similar to that of DPS at pH 7.0 in 2% SDS and 4-6 M GuHCl when SDS and GuHCl were added after DPS. EDTA did not have a significant effect on SH detection when DTNB and DPS were added before SDS and GuHCl. Finally, although mBBr and NPM can detect SH in low protein concentrations ((1)/10 of that required for DTNB and DPS), mBBr and NPM overestimated the SH content of soy protein. Therefore, using DPS at pH 7.0 when it is added before SDS and GuHCl is the most reliable method for detecting the SH content of soy protein.

  15. Accurate determination of chlorine, bromine, and iodine in sedimentary rock reference samples by radiochemical neutron activation analysis and a detailed comparison with inductively coupled plasma mass spectrometry literature data.

    PubMed

    Sekimoto, Shun; Ebihara, Mitsuru

    2013-07-02

    Trace amounts of three halogens (chlorine, bromine, and iodine) were determined using radiochemical neutron activation analysis (RNAA) for nine sedimentary rocks and three rhyolite samples. To obtain high-quality analytical data, the radiochemical procedure of RNAA was improved by lowering the background in gamma-ray spectrometry and completing the chemical procedure more rapidly than in conventional procedures. A comparison of the RNAA data of Br and I with corresponding inductively coupled plasma mass spectrometry (ICPMS) literature data revealed that the values obtained by ICPMS coupled with pyrohydrolysis preconcentration were systematically lower than the RNAA data for some reference samples, suggesting that the quantitative collection of Br and I cannot always be achieved by the pyrohydrolysis for some solid samples. The RNAA data of three halogens can classify sedimentary rock reference samples into two groups (the samples from inland water and those from seawater), implying the geochemical significance of halogen data.

  16. Development of radiochemical analysis strategies for decommissioning activities.

    PubMed

    Zapata-García, D; Wershofen, H

    2017-08-01

    Radioactive waste generated in decommissioning activities need be classified according to their radioactive content. The radiological information required by national authorities includes diverse alpha and beta emitters, which can only be determined after a radiochemical separation process. This paper presents the work on the development of radiochemical methods for the simultaneous separation of several radionuclides in concrete, steel and graphite samples, on the basis of individual sample treatments which merge in a common radiochemical separation procedure based on extraction chromatography. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Simple and rapid determination of hydrogen peroxide using phosphine-based fluorescent reagents with sodium tungstate dihydrate.

    PubMed

    Onoda, Maki; Uchiyama, Takefumi; Mawatari, Ken-Ichi; Kaneko, Kiyoko; Nakagomi, Kazuya

    2006-06-01

    A simple batch method for the fluorometric determination of hydrogen peroxide using phosphine-based fluorescent reagents has been developed. A rapid, mild and selective derivatization reaction was achieved by adding sodium tungstate dihydrate to the reaction mixture of hydrogen peroxide and a phosphine-based fluorescent reagent. When 4-diphenylphosphino-7-methylthio-2,1,3-benzoxadiazole was used as a reagent, the derivatization reaction was completed after 2 min at room temperature. The calibration curve was linear between 12.5 and 500 ng hydrogen peroxide in a 10 microL sample solution. This method is accurate and has potential for on-line applications.

  18. A novel high throughput method based on the DPPH dry reagent array for determination of antioxidant activity.

    PubMed

    Musa, Khalid Hamid; Abdullah, Aminah; Kuswandi, Bambang; Hidayat, M Amrun

    2013-12-15

    A stable chromogenic radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) is commonly used for the determination of antioxidant activity. In this paper, DPPH was dried into 96 well microplate to produce DPPH dry reagent array plate, based on which the highly sensitive and high throughput determination of antioxidant activities was achieved. The spectrophotometric characterization of the microplate containing dried or fresh DPPH free radicals was reported. The response of the DPPH dry reagent array towards different standard antioxidants was studied. The reaction for DPPH in fresh or dry reagent array with Trolox was reported and compared. The DPPH dry reagent array was used to study the antioxidant activity of banana, green tea, pink guava, and honeydew and the results were compared to the samples reacted with freshly prepared DPPH. The proposed method is comparable to the classical DPPH method, more convenient, simple to operate with minimal solvent required and excellent sensitivity.

  19. Radiochemical separation of gold by amalgam exchange

    USGS Publications Warehouse

    Ruch, R.R.

    1970-01-01

    A rapid and simple method for the radiochemical separation of gold after neutron activation. The technique is based on treatment with a dilute indium-gold amalgam, both chemical reduction and isotopic exchange being involved. The counting efficiency for 198Au in small volumes of the amalgam is good. Few interferences occur and the method is applicable to clays, rocks, salts and metals. The possibility of determining silver, platinum and palladium by a similar method is mentioned. ?? 1970.

  20. Determination of an international sensitivity index of thromboplastin reagents using a WHO thromboplastin as calibrator for plasma spiked with rivaroxaban.

    PubMed

    Harenberg, Job; Marx, Svetlana; Krämer, Roland; Giese, Christina; Weiss, Christel

    2011-12-01

    Rivaroxaban and other direct factor Xa inhibitors are used at fixed doses without drug monitoring and dose adjustment. Patients may require determination of the anticoagulant effect during treatment. The aim of this study was to develop a method to reduce the differences between thromboplastin reagents and coagulation analysers for determination of the anticoagulant effect of rivaroxaban in human plasma. Purity of rivaroxaban extracted from commercially available drug was confirmed by mass spectrometry, elemental analysis and 1H-NMR spectroscopy. Coagulation times of pooled human plasma spiked with 50-900  ng/ml rivaroxaban were analysed. Thromboplastin reagents, WHO RBT/90, Innovin, RecombiPlasTin 2G, STA Neoplastin Plus, Technoclot PT Plus and Thromborel S, the manual Kolle-Hook method and the KC10 analyser were used. An international sensitivity index (ISI) was determined for each reagent and coagulation method using the RBT/90 thromboplastin reagent as reference. The orthogonal, used for the determination of the ISI of coumarin plasmas, and ordinary regression analyses were compared. The results showed than increasing concentrations of rivaroxaban prolonged coagulation values of all thromboplastin assays linearly (r (2)= 0.96 and r(2) = 0.99, respectively). The coefficient of variation between the slopes of the dilution curves and the ratios of the thromboplastin reagents were reduced using the international normalized ratio (INR) and ISI calculated for rivaroxaban. The ISIs of the thromboplastin reagents ranged from 0.73 to 1.67 as compared with the WHO reagent using the manual technique. The coefficient of variations between the thromboplastin reagents comparing the orthogonal and the ordinary regression analysis were 6.8 versus 3.7% (Kolle-Hook method, P = 0.0011) and 8.5 versus 4.8% (KC10 method, P < 0.0001). Using ISI for vitamin-K antagonist and rivaroxaban, the INRs for the rivaroxaban-containing samples were significantly different for

  1. Automated multiple flow-injection analysis in clinical chemistry: determination of total protein with Biuret reagent.

    PubMed

    Shideler, C E; Stewart, K K; Crump, J; Wills, M R; Savory, J; Renoe, B W

    1980-09-01

    We have examined the feasibility of the automated multiple flow-injection technique for application to clinical chemistry by adapting to this system the biuret method for the determination of total protein. Samples were discretely and rapidly introduced into a continuously flowing, nonsegmented reagent stream by means of an automatic sampler and high-pressure injection valve. Pumps operating at 1380-2070 kPa (200-300 psi) were utilized to introduce the biuret reagent and saline diluent into the system separately at flow rates of 72 and 47 microL/s, respectively. Use of 20-microL sample and a 3.0-s reaction-delay coil was adequately sensitive for analysis for total protein by this method. Samples were analyzed at a rate of 150/h with no detectable between-sample carryover. Within-run precision studies yielded relative standard deviations of 2.5% and less. Total protein values obtained by this method correlated well with those obtained by centrifugal analyzer and bubble-segmented continuous-flow biuret methods.

  2. Spectrofluorometric determination of common epoxides with sodium sulfide and o-phthalaldehyde and taurine reagents

    SciTech Connect

    Sano, A.; Takitani, S.

    1985-07-01

    A spectrofluorometric method has been developed for the determination of common epoxides. Epoxides in ethanol solution gave an intense blue fluorescence (lambda/sub ex/ ca. 345 nm and lambda/sub em/ ca. 440 nm), after the first reaction with aqueous sodium sulfide at 55/sup 0/C for 20 min and followed by the second reaction with taurine and o-phthalaldehyde reagents at pH 8.3. By the proposed method, 1,2-epoxy-3-phenoxypropane and 1,2-epoxyoctane can be determined in the ranges 0.05-3 nmol/100 ..mu..L and 0.1-8 nmol/100 ..mu..L, respectively, with coefficients of variation of 1.6-2.9%. Some other alkylating agents also showed fluorescence by this method. 16 references, 8 figures, 3 tables.

  3. Spectrofluorometric determination of furosemide in some pharmaceutical product using acriflavine as a reagent

    NASA Astrophysics Data System (ADS)

    Qader, Aryan F.; Fakhre, Nabil A.

    2017-09-01

    Simple, inexpensive, rapid and sensitive determination of furosemide spectrofluorometrically was suggested using acriflavine as a new reagent. The method based on the quantitative quenching effect of furosemide on the native fluorescence of acriflavine in presence of Britton-Robinson buffer medium due to the reaction of furosemide with acriflavine to form an ion associated complex. The decrease of acriflavine fluorescence was observed at 505 nm after excitation at 265 nm. the florescence - concentration plot is rectilinear over the range of 2.0-10 µg/ml with correlation coefficient 0.9991 and detection limit 0.2 µg/ml. No interference was observed from the excipients that are commonly present in pharmaceutical formulations. The proposed method was determination of furosemide in some commercial tablets. The results were compared with that of HPLC method revealed with good agreements and no significant differences in the accuracy and precision.

  4. Radiochemical analysis of 93Zr.

    PubMed

    Espartero, A G; Suárez, J A; Rodríguez, M; Piña, G

    2002-01-01

    The zirconium isotope 93Zr is a long-lived pure beta-particle-emitting radionuclide, which is produced by nuclear fission and neutron activation of the stable isotope 92Zr. This element is a constituent of the structural components of nuclear reactor vessels. A selective liquid-liquid extraction method for radiochemical separation of Zr, based on liquid-liquid extraction with 1-(2'-thenoyl)-3,3,3-trifluoroacetone in xylene and a subsequent stripping of 93Zr by an aqueous acid solution, has been developed. The method was utilised to separate Zr from other pure beta-particle and beta-gamma emitters in different kinds of samples. Decontamination factors higher than 99% for the pure beta-particle and beta-gamma emitters and an overall chemical yield of 80% were obtained. The sensitivity of the method allows the determination of the isolated 93Zr by liquid scintillation counting and the minimum detectable activity value obtained was 0.067 Bq over a counting period of 60 min.

  5. [Determination of residual epichlorohydrin and sym-dichloroisopropyl alcohol in cationic etherified reagent by gas chromatography].

    PubMed

    Zhou, Weiyi; Fan, Guoliang; Jiang, Dongfeng

    2004-11-01

    A method for the determination of the residual epichlorohydrin and sym-dichloroisopropyl alcohol in cationic etherified reagent by gas chromatography has been established. Methyl benzoate, which has high extraction efficiency for the two components, was used as extractant. With an HP-5 capillary column, the two components were baseline separated and they eluted before the extractant. The linear ranges achieved were 5 - 590 mg/kg for epichlorohydrin and 21 - 480 mg/kg for sym-dichloroisopropyl alcohol. The limits of detection were 1.2 mg/kg for epichlorohydrin and 2.2 mg/kg for sym-dichloroisopropyl alcohol. Recoveries for epichlorohydrin were 95.93% - 103.42% with relative standard deviations of 2.4% - 10.6% and those for sym-dichloroisopropyl alcohol were 98.54% - 107.40% with relative standard deviations of 6.6% -11.1%. The method is simple, fast, and convenient.

  6. Coulometric trace determination of water by using Karl Fischer reagent and potentiometric end-point detection.

    PubMed

    Cedergren, A

    1974-06-01

    A new approach to the determination of water via the Karl Fischer reaction is described. Iodine is coulometrically generated and the end-point corresponding to a slight excess of iodine, is detected potentiometrically with a non-polarized platinum electrode. Samples of 1-500 mul containing 0.05-200 mug of water were analysed with a standard deviation of 0.015 mug in the range 0.05-20 mug of H(2)O. A specially constructed electrolysis cell was used in combination with an LKB 16300 Coulometric Analyzer and the time for a complete analysis was 1-4 min, depending on sample size. The reagent composition has been optimized in order to enhance the rate of the main reaction and to minimize the extent of side-reactions. Decreasing the temperature reduced the extent of side-reactions. The displacement of end-point potential on dilution was studied and a correction is discussed.

  7. Rapid Radiochemical Methods for Asphalt Paving Material ...

    EPA Pesticide Factsheets

    Technical Brief Validated rapid radiochemical methods for alpha and beta emitters in solid matrices that are commonly encountered in urban environments were previously unavailable for public use by responding laboratories. A lack of tested rapid methods would delay the quick determination of contamination levels and the assessment of acceptable site-specific exposure levels. Of special concern are matrices with rough and porous surfaces, which allow the movement of radioactive material deep into the building material making it difficult to detect. This research focuses on methods that address preparation, radiochemical separation, and analysis of asphalt paving materials and asphalt roofing shingles. These matrices, common to outdoor environments, challenge the capability and capacity of very experienced radiochemistry laboratories. Generally, routine sample preparation and dissolution techniques produce liquid samples (representative of the original sample material) that can be processed using available radiochemical methods. The asphalt materials are especially difficult because they do not readily lend themselves to these routine sample preparation and dissolution techniques. The HSRP and ORIA coordinate radiological reference laboratory priorities and activities in conjunction with HSRP’s Partner Process. As part of the collaboration, the HSRP worked with ORIA to publish rapid radioanalytical methods for selected radionuclides in building material matrice

  8. Determination of potassium by dry reagent carrier technology: a multicentre evaluation.

    PubMed

    Paschen, K; Hagemann, P; Lang, H R; Cortes, M; Weidemann, G; Toffaletti, J; Burritt, M; Leinberger, R; Tritschler, W; Ramstetter, E

    1993-08-01

    We describe the construction, the reaction principle and the performance of Reflotron K+, a new Reflotron test for the quantitative determination of potassium in serum and heparinized plasma. The reaction principle is based on the introduction of the potassium cation via valinomycin into a non-polar phase; the accompanying loss of protons from the non-polar phase is detected by the colour change of a pH indicator. The multicentre evaluation of the reagent carrier system showed in median CVs of < 0.9% (within-series in heparinized plasmas) and 1.3% (run-to-run in control sera). The recovery in control sera was +/- 4% for seven laboratories. In the method comparison with flame emission spectrometry, using sera and heparinized plasma samples, regression analysis yielded correlations with slopes of 1.00 +/- 0.04 (median slope 1.005) and negligible intercepts. The reagent carrier system showed a linear response in the measuring range 2-12 mmol/l. Bilirubin (up to 513 mumol/l), triacylglycerols (up to 5,7 mmol/l), sodium (135-189 mmol/l) and ammonium ions (up to 590 mumol/l) did not interfere with the test. Comparison with the results from flame atomic emission spectrometry shows that the recoveries of Reflotron K+ and the direct potentiometric method are slightly and similarly influenced by total protein. With a panel of 28 drugs tested, no interference could be detected. Reflotron K+ provides a precise and reliable procedure for the measurement of potassium in serum and heparinized plasma.

  9. Enantiomeric purity determination of acetyl-L-carnitine by NMR with chiral lanthanide shift reagents.

    PubMed

    Kagawa, Miyuki; Machida, Yoshio; Nishi, Hiroyuki; Haginaka, Jun

    2005-08-10

    Enantiomer signal separation of acetyl-carnitine chloride was obtained on a 500 MHz Nuclear Magnetic Resonance (1H NMR) analysis by fast diastereomeric interaction with chiral shift reagents such as chiral lanthanide-camphorato or chiral samarium-pdta shift reagents. Effects of the kinds of chiral shift reagents and the molar ratio of chiral shift reagent to acetyl-carnitine chloride on enantiomer signal separation were investigated and evaluated. Optimization of the experimental conditions provided two significant split signals for the enantiomers, leading to the successful quantitative analysis. Distinguishment of 0.5% of the minor enantiomer (D-form) in acetyl-L-carnitine chloride was found to be possible by 1H NMR with tris[3-(heptafluoropropylhydroxymethylene)-D-camphorato] and praseodymium derivative, (Pr[hfc]3), as chiral shift reagents.

  10. Effects of hirudin on activated partial thromboplastin time determined with ten different reagents.

    PubMed

    Tripodi, A; Chantarangkul, V; Arbini, A A; Moia, M; Mannucci, P M

    1993-08-02

    Hirudin prolongs the APTT when added to normal plasma and the extent of prolongation depends on the type of reagent used. The aim of this study was to compare the dose-response curves of 10 widely used APTT reagents for linearity and parallelism. On each of 10 working days a normal pooled plasma was mixed with increasing amounts of recombinant hirudin (HBW023) ranging from 0 to 5 micrograms/ml and tested for APTT by photo optical coagulometer. Within each working day, clotting times were measured in duplicate and the order of testing with each reagent was changed every day. Results were expressed as ratios of clotting times with hirudin to clotting times without hirudin, and the values plotted against the hirudin concentration on a log-log scale. The dose-response curves for all reagents were linear over 0.3-1.2 micrograms/ml. The reagent-related slopes ranged from 0.225 +/- 0.003 to 0.303 +/- 0.003 (mean +/- SE) and were significantly different. Precision studies indicated that the least sensitive reagent was also the least precise. These findings indicate that the clotting time values obtained for patients treated with hirudin will vary depending on the APTT reagent used.

  11. Effect of dermatan sulphate on activated partial thromboplastin time determined with different reagents.

    PubMed

    Iorio, A; Nucciarelli, F; Renga, C; Nenci, G G; Gianese, F; Agnelli, G

    1997-01-01

    Five widely used activated partial thromboplastin time (APTT) reagents (Actin-FS, Actin-FSL, Hemolab Silimat, IL-Test APTT Ellagic Acid and Thrombofax Activated) were compared for their sensitivity and precision in measuring the effect of dermatan sulphate on blood coagulation. On each of 4 days, aliquots of the same normal human plasma pool were mixed with dermatan sulphate (MF701) at concentrations ranging from 10 to 100 micrograms/ml, and APTT was measured in duplicate with all reagents by a photo-optical coagulometer. The order of testing between and within reagents was changed every day. The relationship of APTT ratio to dermatan sulphate concentration was linear with all the reagents. There were statistically significant differences between reagents in their sensitivity to DS, as reflected by linear regression slopes. IL-Test was the most sensitive reagent. At dermatan sulphate concentrations of 20, 50, and 80 micrograms/ml APTT ratio ranged from 1.5 to 1.7, 1.9 to 2.3 and 2.3 to 2.9, respectively, according to the reagent. The lambda coefficient and coefficient of variation derived from regression analysis, both reflecting assay precision, ranged from 0.57 to 0.71 and from 4.6 to 5.1%, respectively, with all but the least precise reagent. The best sensitivity/precision balance was displayed by IL-Test. The APTT reagent should therefore be standardized, with special regard to sensitivity to DS, when testing the relationship of dermatan sulphate clinical effects to APTT response.

  12. Reagent-free simultaneous determination of glucose and cholesterol in whole blood by FTIR-ATR

    NASA Astrophysics Data System (ADS)

    Li, Zhigang; Lv, Hong; Li, Tianhe; Si, Guangyuan; Wang, Qiaoyun; Lv, Jiangtao; Hu, Xiaofei

    2017-05-01

    Reagent-free determination of multiple analytes is an active and promising field of research in clinical analysis. In this work, the determination of glucose and cholesterol in whole blood using Fourier transform infrared (FTIR) spectroscopy equipped with an attenuated total reflectance (ATR) accessory was performed. A comprehensive sample selection rule in multi space based on SPXY was proposed, termed C-SPXY. The core idea is to make full use of different derivative spectra space to construct the calibration set which preserves the more effective information. On this basis, a partial least squares (PLS) regression fusion modeling method was also presented aiming at improving prediction accuracy of glucose and cholesterol concentration in whole blood samples. Compared with other methods based on single spectra space, the proposed fusion model based on multi spectra space C-SPXY method provides smaller RMSEP values. Experimental results demonstrate that the proposed method and model provides superior predictive power and holds a good application prospect in the field of clinical analysis.

  13. Interfacial reaction using particle-immobilized reagents in a fluidized reactor. Determination of glycerol in biodiesel.

    PubMed

    Shishov, Andrey; Zabrodin, Andrey; Moskvin, Leonid; Andruch, Vasil; Bulatov, Andrey

    2016-03-31

    A novel fluidized beads strategy for utilization of particle-immobilized reagents in flow analysis was developed in this study. The performance of the suggested strategy was demonstrated by the determination of glycerol in biodiesel. This analytical task was used as a proof-of-concept example. The method is based on on-line extraction of glycerol from biodiesel into aqueous stationary phase of extraction-chromatographic column, followed by elution and spectrophotometric determination in the form of copper glycerate formed in a fluidized reactor of stepwise injection system. The floating of cation exchange resin Dowex(®) 50WX4, saturated with Cu(II) ions in liquid phase, was accomplished by air-bubbling. The linear range was from 100 to 1000 mg kg(-1), and the limit of detection, calculated as 3s of a blank test (n = 5), was found to be 30 mg kg(-1). The method was successfully applied to the analysis of biodiesel and biodiesel-blend (B 20) samples.

  14. Risk-based Strategy to Determine Testing Requirement for the Removal of Residual Process Reagents as Process-related Impurities in Bioprocesses.

    PubMed

    Qiu, Jinshu; Li, Kim; Miller, Karen; Raghani, Anil

    2015-01-01

    The purpose of this article is to recommend a risk-based strategy for determining clearance testing requirements of the process reagents used in manufacturing biopharmaceutical products. The strategy takes account of four risk factors. Firstly, the process reagents are classified into two categories according to their safety profile and history of use: generally recognized as safe (GRAS) and potential safety concern (PSC) reagents. The clearance testing of GRAS reagents can be eliminated because of their safe use historically and process capability to remove these reagents. An estimated safety margin (Se) value, a ratio of the exposure limit to the estimated maximum reagent amount, is then used to evaluate the necessity for testing the PSC reagents at an early development stage. The Se value is calculated from two risk factors, the starting PSC reagent amount per maximum product dose (Me), and the exposure limit (Le). A worst-case scenario is assumed to estimate the Me value, that is common. The PSC reagent of interest is co-purified with the product and no clearance occurs throughout the entire purification process. No clearance testing is required for this PSC reagent if its Se value is ≥1; otherwise clearance testing is needed. Finally, the point of the process reagent introduction to the process is also considered in determining the necessity of the clearance testing for process reagents. How to use the measured safety margin as a criterion for determining PSC reagent testing at process characterization, process validation, and commercial production stages are also described. A large number of process reagents are used in the biopharmaceutical manufacturing to control the process performance. Clearance testing for all of the process reagents will be an enormous analytical task. In this article, a risk-based strategy is described to eliminate unnecessary clearance testing for majority of the process reagents using four risk factors. The risk factors included

  15. New analytical reagents for the determination of sulfur dioxide and carbon monoxide

    SciTech Connect

    Trump, E.L.

    1987-01-01

    Four solid reagent methods were developed for the determination of sulfur dioxide in air, and one method was developed to measure carbon monoxide. When applied to filter paper with acetamide as the humectant and 4-phenylcyclohexanone as a bisulfite absorbent, oxohydroxybis(8-hydroxyquinolinyl-) vanadium (V) changes from yellow to black in the presence of sulfur dioxide. The three other methods, also on a filter paper support, utilized the reduction of bromate to bromine which then changed 3-,3'-, 5-,5'-tetramethylbenzidine from yellow to blue, phenothiazine from white to green, and 4-dimethylamino-4'-,4/double prime/-dimethoxytriphenylmethanol from colorless to red-purple. Quantitative measurements were made by reflectance spectroscopy. The method for carbon monoxide involved the use of tetrakis (acetamide-) Pd(II) ditetrafluoroborate, sodium iodate, and leuco crystal violet all together on a filter paper support. Carbon monoxide reduced the Pd(II)-acetamide complex to metallic palladium. The metallic palladium then reduced iodate to hypoiodous acid, HOI, which, in turn, oxidized leuco crystal violet to crystal violet. The crystal violet color was then measured by reflectance.

  16. Enantiomeric determination of amphetamine and methamphetamine in urine by precolumn derivatization with Marfey's reagent and HPLC.

    PubMed

    Foster, B S; Gilbert, D D; Hutchaleelaha, A; Mayersohn, M

    1998-01-01

    An analytical method was developed for enantiomeric determination of amphetamine and methamphetamine in human urine. The enantiomers were isolated from urine by solid-phase extraction, and diastereomers were formed by derivatization with the chiral Marfey's reagent (1-fluoro-2,4-dinitrophenyl-5-l-aniline amide). The diastereomers were separated by reversed-phase high-performance liquid chromatography in a water/methanol mobile phase and detected by absorbance spectrophotometry at 340 nm. Linear standard curves were obtained for all four enantiomers over a concentration range of 0.16-1.00 mg/L in urine. The detection limit was 0.16 mg/L urine for each enantiomer, and the limit of quantitation was 0.40 mg/L. The urine of 10 decedents was analyzed by this method and by a previously published precolumn derivatization procedure using (-)-1-(9-fluorenyl)ethyl chloroformate (FLEC) as the derivatizing agent and fluorescence detection. Comparison of the results of the two methods by linear regression showed comparable results for both d-amphetamine and d-methamphetamine. Neither method detected the presence of the l-enantiomers in the urine samples.

  17. A combined photocatalytic determination system for chemical oxygen demand with a highly oxidative reagent.

    PubMed

    Zhang, Aiyong; Zhou, Minghua; Zhou, Qixing

    2011-02-07

    This study focuses on the proposal and validation of a combined photocatalytic (PC) system and a three-parameterized procedure for the determination of chemical oxygen demand (COD; PcCOD(combined)), with a highly oxidative reagent utilized as a photoelectron scavenger and signal indicator. The PcCOD(combined) was the functional combination of photon-efficient thin-layer photocatalytic oxidation, conventional bulk-phase photocatalytic oxidation and photocarrier-efficient high-activity photocatalytic reduction in one single photodigestion system, and consequently, this system possessed high photon-utilization efficiency, automatic stirring function and satisfactory determination characteristics. In comparison with the conventional one-parameterized procedure, the three-parameterized procedure introduces the blank and total photocatalytic reduction responses as two of the three significant analytical parameters. Under the optimized pH value of 3.0-4.5 and a rotating rate of 40 rpm, the representative KMnO(4) species was used for the PcCOD(combined) system as the combined high-activity oxidant, and a narrow and reliable analytical linear range of 0-260 mg L(-1) was achieved during the 10 min duration of the determinations. No observable interference of Cl(-) was found at concentration of the ion up to 2000 mg L(-1). A real sample analysis indicated that the measured values for the PcCOD(combined) were all within a relative deviation below 5% of COD(Cr) of the standard method, which further validates the practical feasibility of the proposed PcCOD(combined) system.

  18. Determination of meloxicam using europium sensitized luminescence in the presence of co-luminescence reagents.

    PubMed

    Al-Kindy, Salma Muhamed Z; Al-Habsy, Salim K; Suliman, Fakhr Eldin O; Al-Lawati, Haidar A J

    2012-01-01

    A sensitive time-resolved luminescence method for the determination of meloxicam (MX) in methanol and in aqueous solution is described. The method is based on the luminescence sensitization of europium (Eu(3+)) by formation of ternary complex with MX in the presence of 1,10-phenanthroline as coligand, Tween-80 as surfactant and gadolinium ion as a co-luminescence reagent. The signal for Eu-MX-1,10-phenanthroline is monitored at λ(ex) = 360 nm and λ(em) = 620 nm. Optimum conditions for the formation of the complex in aqueous system were 0.01 M TRIS buffer, pH 8.0, 1,10-phenanthroline (6.0 × 10(-6) M), Gd(3+) (7.0 × 10(-6) M), Tween-80 (0.28%) and 1.75 mM of Eu(3+) which allows the determination of 20-800 ppb of MX with limit of detection (LOD) of 7 ppb. The relative standard deviations of the method range between 0.1 and 1.1% indicating excellent reproducibility of the method. The proposed method was successfully applied for the assay of MX in pharmaceutical formulations, plasma and in urine samples. Average recoveries of 99.8 ± 1.1%, 100.2 ± 0.9% and 100.9 ± 1.1% were obtained for MX in tablet, plasma and urine sample respectively.

  19. Separation and determination of trace metal ions using organic chelating reagents

    SciTech Connect

    Palmieri, M.D.

    1987-11-01

    The four reagents tested were N,N-dihexylacetamide (DHA), 2,6-diacetylpyridine bis(furoylhydrazone) (H/sub 2/dapf), 1,3-dimethyl-4-acetyl-2-pyrazolin-5-one (DMAP) and N-methylfurohydroxamic acid (NMFHA). DHA and H/sub 2/dapf were investigated for their complex formation with uranium, and DMAP and NMFHA were used as chelating agents in high performance liquid chromatography (HPLC). Uranium(VI) is preferentially extracted from nitric acid solutions using DHA in toluene. The extraction characteristics of the U-DHA complex are studied. A 119,000 ..mu..gL/sup -1/ U solution is analyzed for twenty-six elements. The U is extracted with DHA, and the trace metal ions are then determined by inductively coupled plasma-mass spectrometry. Uranium must be removed from the sample before analysis to prevent ionization suppression. H/sub 2/dapf is synthesized and characterized. Studies of the complexation of metal ions with H/sub 2/dapf is described. U(VI) forms a stable complex with H/sub 2/dapf, and a procedure for selectively determining trace U by spectrophotometry is presented. DMAP complexes of Cu(II), Fe(III), Ga(III), Th(IV), U(VI), V(V), and Zr(IV) are separated using reversed phase HPLC. NMFHA complex of Al(III), Fe(III), Hf(IV), Nb(V), Sb(III), and Zr(IV) are separated using reversed phase HPLC. NMFHA is also used to separate uranium(VI) from trace lanthanide ions. 266 refs., 46 figs., 24 tabs

  20. Uranium content of blood, urine and hair of exposed and non-exposed persons determined by radiochemical neutron activation analysis, with emphasis on quality control.

    PubMed

    Byrne, A R; Benedik, L

    1991-09-01

    Recent reviews have highlighted the diversity (and sparsity) of data for uranium concentrations in body fluids, bone and soft tissues, and it is unclear to what extent this reflects genuine geographical or biological variations. In the present work, a very sensitive radiochemical neutron activation analysis technique (detection limit, 1-2pg g-1) was applied to an exploratory study of uranium levels in hair, urine and blood of non-exposed and occupationally exposed persons. Since quality control in much previous work has been somewhat neglected, this aspect was emphasized by the use of a wide range of suitable reference materials, by standard addition experiments, and by care in sampling and sample handling. For controls, typical levels found in hair, urine and blood were 10 ng g-1, 10 and 5 ng l-1, respectively. The urine values correspond to the lower end of the literature data, while for blood our value is about two orders of magnitude lower than the presently quoted level. In the case of occupationally exposed persons, it was found that hair shows some promise as an indicator of exposure.

  1. A selective spectrophotometric method for determination of rosoxacin antibiotic using sodium nitroprusside as a chromogenic reagent.

    PubMed

    Askal, Hassan F; Refaat, Ibrahim H; Darwish, Ibrahim A; Marzouq, Mostafa A

    2008-04-01

    A selective spectrophotometric method for the determination of rosoxacin (ROS), a 4-quinolone antimicrobial agent, has been developed and validated. The method was based on the reaction of ROS with alkaline sodium nitroprusside (SNP) reagent at room temperature forming a red colored chromogen measured at 455 nm. The conditions affecting the reaction (SNP concentration, pH, color-developing time, temperature, diluting solvent and chromogen stability time) were optimized. Under the optimum conditions, good linear relationship (r=0.9987) was obtained between the absorbance and the concentration of ROS in the range of 20-50 microg ml(-1). The assay limits of detection and quantitation were 2.5 and 8.4 microg ml(-1), respectively. The method was successfully applied to the analysis of bulk drug and laboratory-prepared tablets; the mean percentage recoveries were 100.1+/-0.33 and 101.24+/-1.28%, respectively. The results were compared favourably with those obtained by the reported method; no significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. The robustness and ruggedness of the method was checked and satisfactory results were obtained. The proposed method was found to be highly selective for ROS among the fluoroquinolone antibiotics. The reaction mechanism was proposed and it proceeded in two steps; the formation of nitroferrocyanide by the action of sodium hydroxide alkalinity on SNP and the subsequent formation of the colored nitrosyl-ROS derivative by the attack at position 6 of ROS.

  2. A selective spectrophotometric method for determination of rosoxacin antibiotic using sodium nitroprusside as a chromogenic reagent

    NASA Astrophysics Data System (ADS)

    Askal, Hassan F.; Refaat, Ibrahim H.; Darwish, Ibrahim A.; Marzouq, Mostafa A.

    2008-04-01

    A selective spectrophotometric method for the determination of rosoxacin (ROS), a 4-quinolone antimicrobial agent, has been developed and validated. The method was based on the reaction of ROS with alkaline sodium nitroprusside (SNP) reagent at room temperature forming a red colored chromogen measured at 455 nm. The conditions affecting the reaction (SNP concentration, pH, color-developing time, temperature, diluting solvent and chromogen stability time) were optimized. Under the optimum conditions, good linear relationship ( r = 0.9987) was obtained between the absorbance and the concentration of ROS in the range of 20-50 μg ml -1. The assay limits of detection and quantitation were 2.5 and 8.4 μg ml -1, respectively. The method was successfully applied to the analysis of bulk drug and laboratory-prepared tablets; the mean percentage recoveries were 100.1 ± 0.33 and 101.24 ± 1.28%, respectively. The results were compared favourably with those obtained by the reported method; no significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. The robustness and ruggedness of the method was checked and satisfactory results were obtained. The proposed method was found to be highly selective for ROS among the fluoroquinolone antibiotics. The reaction mechanism was proposed and it proceeded in two steps; the formation of nitroferrocyanide by the action of sodium hydroxide alkalinity on SNP and the subsequent formation of the colored nitrosyl-ROS derivative by the attack at position 6 of ROS.

  3. The protonated 4,4'-diaminotriphenylmethyl cation as a reagent and cyclohexanone as an absorbant for sulphur dioxide determination.

    PubMed

    Lambert, J L; Chejlava, M J; Beyad, M H; Paukstelis, J V

    1982-01-01

    Protonated 4,4'-diaminotriphenylmethyl cation, DATM, has been investigated as a colorimetric reagent for the determination of sulphur dioxide. The bisulphite addition compound with formaldehyde alkylates a primary arylamine group in the protonated reagent to re-establish resonance, and hence produces a colour that is proportional in intensity to the concentration of either bisulphite or formaldehyde (the other being in excess). The large bathochromic spectral shift results in a negligible blank correction. Cyclohexanone in aqueous solution has been found to stabilize bisulphite solutions for up to 6 hr. The stabilization by cyclohexanone has been compared with stabilization by tetrachloromercurate(II). The Beer-Lambert law is obeyed with good precision for both sulphite and formaldehyde determination.

  4. Laboratory Reagents

    SciTech Connect

    CARLSON, D.D.

    1999-10-08

    Replaced by WMH-310, Section 4.17. This document outlined the basic methodology for preparing laboratory reagents used in the 222-S Standards Laboratory. Included were general guidelines for drying, weighing, transferring, dissolving, and diluting techniques common when preparing laboratory reagents and standards. Appendix A contained some of the reagents prepared by the laboratory.

  5. Volumetric Titrations Using Electrolytically Generated Reagents for the Determination of Ascorbic Acid and Iron in Dietary Supplement Tablets: An Undergraduate Laboratory Experiment

    ERIC Educational Resources Information Center

    Scanlon, Christopher; Gebeyehu, Zewdu; Griffin, Kameron; Dabke, Rajeev B.

    2014-01-01

    An undergraduate laboratory experiment for the volumetric quantitative analysis of ascorbic acid and iron in dietary supplement tablets is presented. Powdered samples of the dietary supplement tablets were volumetrically titrated against electrolytically generated reagents, and the mass of dietary reagent in the tablet was determined from the…

  6. INFLUENCE OF REAGENT PURITY ON THE ION CHROMATOGRAPHIC DETERMINATION OF BROMATE IN WATER USING 3,3'-DIMETHOXYBENZIDINE AS A PROCHROMOPHORE FOR PHOTOMETRIC DETECTION

    EPA Science Inventory

    Variable availability of the purified dihydrochloride salt of 3,3'-dimethoxybenzidine (DMB, ortho-dianisidine) led us to investigate the effects of reagent purity on the analytical results obtinaed when this reagent is used in the photometric determination of the disinfection byp...

  7. Volumetric Titrations Using Electrolytically Generated Reagents for the Determination of Ascorbic Acid and Iron in Dietary Supplement Tablets: An Undergraduate Laboratory Experiment

    ERIC Educational Resources Information Center

    Scanlon, Christopher; Gebeyehu, Zewdu; Griffin, Kameron; Dabke, Rajeev B.

    2014-01-01

    An undergraduate laboratory experiment for the volumetric quantitative analysis of ascorbic acid and iron in dietary supplement tablets is presented. Powdered samples of the dietary supplement tablets were volumetrically titrated against electrolytically generated reagents, and the mass of dietary reagent in the tablet was determined from the…

  8. INFLUENCE OF REAGENT PURITY ON THE ION CHROMATOGRAPHIC DETERMINATION OF BROMATE IN WATER USING 3,3'-DIMETHOXYBENZIDINE AS A PROCHROMOPHORE FOR PHOTOMETRIC DETECTION

    EPA Science Inventory

    Variable availability of the purified dihydrochloride salt of 3,3'-dimethoxybenzidine (DMB, ortho-dianisidine) led us to investigate the effects of reagent purity on the analytical results obtinaed when this reagent is used in the photometric determination of the disinfection byp...

  9. [Determination of blood constituents with dry reagent carriers. Comparison with wet chemical tests (author's transl)].

    PubMed

    Thomas, L; Appel, W; Storz, G; Plischke, W

    1981-08-28

    Quantitative measurement of blood constituents (glucose, uric acid, urea-N) on dry reagent carriers was compared with corresponding wet-chemical methods. There was a good correlation (r greater than 0.95) and excellent linear regression with small scatter between the two methods for the three constituents. The dry test has proved to be a precise, simple, rapid and economic method, especially suitable for the practitioner and emergency laboratory.

  10. Reverse flow injection spectrophotometric determination of ciprofloxacin in pharmaceuticals using iron from soil as a green reagent.

    PubMed

    Palamy, Sysay; Ruengsitagoon, Wirat

    2017-09-13

    A novel reverse flow injection spectrophotometric method for the determination of ciprofloxacin was successfully combined with the on-line introduction of an iron solution extracted from soil as green reagent. The assay was optimized by a univariate method to select the optimum conditions for the highest absorbance and highest stability of the complex. Beer-Lambert's law (λmax=440nm) is obeyed in the range 0.5-50μgmL(-1) with a correlation coefficient (r(2)) of 0.9976 and 0.9996 using soil as green reagent from Khon Kaen, Thailand and Vientiane, Laos, respectively. The average percentage recoveries were in the range of 98.55-102.14% and the precision was in the range of 0.80-1.73%. The limit of detection and the limit of quantitation were 0.20 and 0.69μgmL(-1), respectively, with a sampling rate of over 46samplesh(-1). The method was successfully applied to the determination of ciprofloxacin in commercial pharmaceutical formulations. The results were in good agreement with those obtained by the reference HPLC method using a t-test at 95% of confidence level for comparison. This method is suitable for laboratories looking for alternative analytical methods using green reagents. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Investigation of selected ferroin-type compounds as fluorometric reagents Determination of zinc with 2-(4-methyl-2-pyridyl)-5(6)-phenylbenzimidazole.

    PubMed

    Schilt, A A; Hillison, T E

    1980-11-01

    In a search for new fluorometric reagents for trace metal determinations, forty different ferroin-type compounds and their silver, lead and zinc chelates were tested for luminescence in aqueous-ethanol solutions at various pH values. Twelve formed fluorescent chelates of potential analytical utility, and the results revealed some correlation between ligand structure and fluorescence. After identification of the most sensitive fluorometric reagent for zinc among those tested, a spectrophotofluorometric method for the determination of zinc was developed. Proper control of pH and reagent concentration allows determination of nanogram amounts of zinc.

  12. An enzyme-chromogenic surface plasmon resonance biosensor probe for hydrogen peroxide determination using a modified Trinder's reagent.

    PubMed

    Nakamura, Hideaki; Mogi, Yotaro; Akimoto, Takuo; Naemura, Kiyoshi; Kato, Teru; Yano, Kazuyoshi; Karube, Isao

    2008-11-15

    An absorption-based surface plasmon resonance (SPR(Abs)) biosensor probe has been developed for simple and reproducible measurements of hydrogen peroxide using a modified Trinder's reagent (a chromogenic reagent). The reagent enabled the determination of the hydrogen peroxide concentration by the development of deep color dyes (lambda(max)=630 nm) through the oxidative coupling reaction with N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3,5-dimethylaniline sodium salt monohydrate (MAOS; C(13)H(20)NNaO(4)S.H(2)O) and 4-aminoantipyrine (4-AA) in the presence of hydrogen peroxide and horseradish peroxidase (HRP). In the present study, urea as an adduct of hydrogen peroxide for color development could be omitted from the measurement solution. The measurement solution containing 5mM hydrogen peroxide was deeply colored at a high absorbance value calculated as 46.7cm(-1) and was directly applied to the SPR(Abs) biosensing without dilution. The measurement was simply performed by dropping the measurement solution onto the surface of the SPR sensor probe, and the SPR(Abs) biosensor response to hydrogen peroxide was obtained as a reflectivity change in the SPR spectrum. After investigation of the pH profiles in the SPR(Abs) biosensor probe, a linear calibration curve was obtained between 1.0 and 50mM hydrogen peroxide (r=0.991, six points, average of relative standard deviation; 0.152%, n=3) with a detection limit of 0.5mM. To examine the applicability of this SPR(Abs) biosensor probe, 20mM glucose detection using glucose oxidase was also confirmed without influence of the refractive index in the measurement solution. Thus, the SPR(Abs) biosensor probe employing the modified Trinder's reagent demonstrated applicability to other analyte biosensing tools.

  13. Fluorimetric determination of copper(II) in aqueous solution using lucifer yellow CH as selective metal reagent.

    PubMed

    Mayr, T; Wencel, D; Werner, T

    2001-09-01

    Lucifer yellow CH is shown to be a highly selective fluorescent reagent for the determination of Cu(III) in the microg L(-1) concentration range. The fluorophore is statically quenched by Cu(II); the carbohydrazide group was assigned as the complexing part of the dye molecule. A total range of Cu(II) determination from 0.06 mg L(-1) (1 micromol L(-1)) to 6.3 mg L(-2) (100 micromol L(-1)) with a limit of detection of 0.019 mg L(-1) (0.3 micromol L(-1)) was obtained, along with surprisingly high selectivity. There was no interference from alkaline and earth alkaline metal ions. The cross sensitivity to heavy metal ions was evaluated by the separate solution method and by competitive binding experiments. Calibration plots are shown for Cu(II) determination at different pH and the dissociation constant was determined. The application of the reagent was demonstrated by the determination of the Cu(II) content of tap water samples.

  14. High-performance liquid chromatographic determination of uranium using solvent extraction and bis(salicylaldehyde) tetramethylethylenediimine as complexing reagent.

    PubMed

    Khuhawar, M Y; Lanjwani, S N

    1995-12-01

    The reagent bis(salicylaldehyde)tetramethylethylenediimine has been used for the determination of dioxouranium(VI), based on complexation in aqueous solution at pH 6, followed by extraction in chloroform and HPLC determination on a Hypersil ODS (3 mum) column. The complex was eluted with the ternary mixture methanol-acetonitrile-water (40:30:30, v/v/v), with UV detection at 260 nm. Oxovanadium(IV), iron(III), copper(II), cobalt(II), nickel(II) and palladium(II) were completely separated and did not interfere in the determination of uranium. The linear calibration range and detection limits have been obtained. The method has been applied to the determination of uranium together with copper, iron and nickel in mineral ore samples.

  15. New chelating reagents for preconcentration, separation, determination of metal complexes by high performance liquid chromatography and solid phase extraction

    SciTech Connect

    Qian, Yan wen.

    1991-12-03

    A general scheme is outlined for rapid determination of metal cations by complexation and subsequent HPLC separation. The synthesis and general properties are described for several new thiohydrazone chelating reagents. Solubility considerations suggest that the metal complexes have a positive charge. Excellent chromatographic separations are obtained for mixtures of up to seven metal complexes. Addition of a positively charged additive to the eluent is shown to have a significant effect on both the retention times and sharpness of the chromatographic peaks. Separation of the metal complexes on resins with a permanent charge is also shown to be feasible. Two new hydrazone reagents have been synthesized and characterized. Trace metal ions in aqueous solution are complexed by one of the hydrazones and the resulting metal complexes are solid phase extracted onto a mini cation-exchange or polymeric column. The uptake of metal complexes is complete and the elution step is fast and complete. The quantitative recoveries of metal ions determined by both spectrophotometric method and ICP-MS are very satisfactory and agree with each other.

  16. New chelating reagents for preconcentration, separation, determination of metal complexes by high performance liquid chromatography and solid phase extraction

    SciTech Connect

    Qian, Yan wen

    1991-12-03

    A general scheme is outlined for rapid determination of metal cations by complexation and subsequent HPLC separation. The synthesis and general properties are described for several new thiohydrazone chelating reagents. Solubility considerations suggest that the metal complexes have a positive charge. Excellent chromatographic separations are obtained for mixtures of up to seven metal complexes. Addition of a positively charged additive to the eluent is shown to have a significant effect on both the retention times and sharpness of the chromatographic peaks. Separation of the metal complexes on resins with a permanent charge is also shown to be feasible. Two new hydrazone reagents have been synthesized and characterized. Trace metal ions in aqueous solution are complexed by one of the hydrazones and the resulting metal complexes are solid phase extracted onto a mini cation-exchange or polymeric column. The uptake of metal complexes is complete and the elution step is fast and complete. The quantitative recoveries of metal ions determined by both spectrophotometric method and ICP-MS are very satisfactory and agree with each other.

  17. Camphor-3-thioxo-2-oxime as an analytical reagent for extractive spectrophotometric determination and separation of lead

    NASA Astrophysics Data System (ADS)

    Ninan, S.; Varadarajan, A.; Jadhav, S. B.; Kulkarni, A. J.; Malve, S. P.

    1999-04-01

    Camphor-3-thioxo-2-oxime (HCTO) is proposed as a new sensitive analytical reagent for the extractive spectrophotometric determination of trace amounts of lead. The method is based on the instantaneous formation of a stable yellow-orange colored 1:2 chelate with lead at room temperature in the pH range 9.3-9.6 selectively extracted in carbon tetrachloride. The extracted species exhibits an absorption maximum at 400 nm with a molar absorptivity of 4.14×10 4 mol -1 cm -1, complying with Beer's law over the concentration range 0.1-0.5 μg ml -1 of lead with an optimum concentration range 0.18-0.37 μg ml -1. The effects of pH, concentration of reagent and salting-out agents, time of equilibration, order of addition of diluents and the tolerance limit of the method towards various cations and anions usually associated with lead are reported. The developed method is successfully used for the determination of traces of lead in synthetic mixtures, alloys and ore samples.

  18. Spectrophotometric determination of trazodone, amineptine and amitriptyline hydrochlorides through ion-pair formation using methyl orange and bromocresol green reagents

    NASA Astrophysics Data System (ADS)

    Nour El-Dien, Faten A. F.; Mohamed, Gehad G.; Mohamed, Nehad A.

    2006-09-01

    A simple and rapid extraction spectrophotometric procedure has been developed for the determination of tricyclic anti-depressant drugs such as trazodone (TZH), amineptine (APH) and amitriptyline (ATPH) hydrochlorides in pure form and in different dosage forms. The method involves the formation of intense yellow ion-pairs between these drugs under investigation and methyl orange (MO) and bromocresol green (BCG) reagents followed by their extraction with 1,2-dichloroethane and quantitative microdetermination at 420 and 410 nm using MO or BCG, respectively. The optimum experimental conditions for the ion-pairs formation are established. The method permits the determination of TZH, APH and ATPH over a concentration range of 2-50, 2-50 and 1-25 μg ml -1 for TZH, APH and ATPH, using MO and 1-25 μg ml -1 for TZH, APH and ATPH, using BCG, respectively. The Sandell sensitivity ( S) is found to be 0.106, 0.1071 and 0.0907 g cm -2 for TZH, APH and ATPH, respectively, using MO reagent and 0.0788, 0.0661 and 0.0494 g cm -2 for TZH, APH and ATPH, respectively, using BCG. The method is applicable for the assay of the investigated drugs in different dosage forms and the results are in good agreement with those obtained by the official method.

  19. Direct determination of inorganic phosphorus in serum with a single reagent.

    PubMed

    Muñoz, M A; Balón, M; Fernandez, C

    1983-02-01

    Estimation of inorganic phosphate in serum based on the formation of "molybdenum blue" may be simplified by eliminating the reduction stage. The yellow complex formed by the reaction of phosphate with molybdate in an acid medium is measured at 390 nm. The yellow complex behaves in accordance with Beer's law over a wide concentration range (to at least 80 mg of P per liter in the initial sample); its molar absorptivity at 390 nm is 2.51 X 10(3) L mol-1 cm-1. Sensitivity is increased in the presence of a detergent (triethanolamine lauryl sulfate), which is also used to dissolve the proteins. Because only one reagent is used (a stable combination of, per liter, 20 mmol of sodium molybdate, 82 mmol of nitric acid, and 100 mg of the detergent), the method is simple and rapid. We describe a manual procedure and an automated one. Within-run precision was 1.9%, and day-to-day precision less than 7%. Results by the automated method compare favorably (r = 0.96) with those obtained by Drewes's method (Clin Chim Acta 39: 81-88, 1972).

  20. Spectrophotometric determination of trace amounts of fluoride using an Al-xylenol orange complex as a colored reagent.

    PubMed

    Zolgharnein, Javad; Shahrjerdi, Akram; Azimi, Gholamhassan; Ghasemi, Jahanbakhsh

    2009-10-01

    A new spectrophotometric reagent for the determination of trace amounts of fluoride has been introduced. This method is based on the decolorization of a complex of Al(III) with xylenol orange (XO) as an ultra-sensitive colored reagent. Since the Al-XO complex plays an important role in this method, the protonation and complexation of XO with Al(III) at an ionic strength of 0.1 mol L(-1) at 25 degrees C has been studied by a spectrophotometric global analysis method. The EQUISPEC program was used to evaluate the protonation constants of XO and the stability constants of the formed complexes with Al(III). The protonation and the stability constants of the major complex species such as ML, MLH and MLH2, were determined. Finally, a spectrophotometric method for the assay of fluoride based on a decrease of the color intensity of the Al-XO complex, in an aqueous solution has been designed. The effects of some important variables on the determination of fluoride based on the proposed method were investigated. The method was applied to the determination of fluoride under the optimum conditions (pH 5.2, ionic strength 0.1 mol L(-1), 25 degrees C). The determination of fluoride in the range of 0.08-1.4 microg mL(-1) (SD = 1.2%) was successfully performed. Interferences of Fe(III) were easily eliminated by using ascorbic acid. The proposed method was applied to the determination of trace amounts of fluoride content of some real water samples.

  1. Collected radiochemical and geochemical procedures

    SciTech Connect

    Kleinberg, J

    1990-05-01

    This revision of LA-1721, 4th Ed., Collected Radiochemical Procedures, reflects the activities of two groups in the Isotope and Nuclear Chemistry Division of the Los Alamos National Laboratory: INC-11, Nuclear and radiochemistry; and INC-7, Isotope Geochemistry. The procedures fall into five categories: I. Separation of Radionuclides from Uranium, Fission-Product Solutions, and Nuclear Debris; II. Separation of Products from Irradiated Targets; III. Preparation of Samples for Mass Spectrometric Analysis; IV. Dissolution Procedures; and V. Geochemical Procedures. With one exception, the first category of procedures is ordered by the positions of the elements in the Periodic Table, with separate parts on the Representative Elements (the A groups); the d-Transition Elements (the B groups and the Transition Triads); and the Lanthanides (Rare Earths) and Actinides (the 4f- and 5f-Transition Elements). The members of Group IIIB-- scandium, yttrium, and lanthanum--are included with the lanthanides, elements they resemble closely in chemistry and with which they occur in nature. The procedures dealing with the isolation of products from irradiated targets are arranged by target element.

  2. A novel flow injection spectrophotometric method using plant extracts as green reagent for the determination of doxycycline.

    PubMed

    Palamy, Sysay; Ruengsitagoon, Wirat

    2017-01-15

    A novel flow injection spectrophotometric method was developed for the determination of doxycycline in pharmaceutical preparations using iron(III) contained in extracts from plants. The assay was based on the complex formed between doxycycline and iron(III) characterized by an absorption maximum at 435nm. The calibration graphs obtained over the doxycycline concentration range 5-250μgmL(-1) gave correlation coefficients of 0.9979, 0.9987 and 0.9987 with the three green reagents prepared from Senna alata (L.) Roxb. (S. alata), Polygonum hydropiper L. (P. hydropiper) or Diplazium esculentum (Retz.) Sw. (D. esculentum), respectively. The relative standard deviations of the repeatability was <2.00%. The percentage recoveries were in the range of 98.27-101.03%. Doxycycline contents obtained by this new method and by the reference methods reported in literature were in agreement at 95% confidence level with the paired t-test. The sample throughput was 36h(-1) for each green reagent.

  3. A novel flow injection spectrophotometric method using plant extracts as green reagent for the determination of doxycycline

    NASA Astrophysics Data System (ADS)

    Palamy, Sysay; Ruengsitagoon, Wirat

    2017-01-01

    A novel flow injection spectrophotometric method was developed for the determination of doxycycline in pharmaceutical preparations using iron(III) contained in extracts from plants. The assay was based on the complex formed between doxycycline and iron(III) characterized by an absorption maximum at 435 nm. The calibration graphs obtained over the doxycycline concentration range 5-250 μg mL- 1 gave correlation coefficients of 0.9979, 0.9987 and 0.9987 with the three green reagents prepared from Senna alata (L.) Roxb. (S. alata), Polygonum hydropiper L. (P. hydropiper) or Diplazium esculentum (Retz.) Sw. (D. esculentum), respectively. The relative standard deviations of the repeatability was < 2.00%. The percentage recoveries were in the range of 98.27-101.03%. Doxycycline contents obtained by this new method and by the reference methods reported in literature were in agreement at 95% confidence level with the paired t-test. The sample throughput was 36 h- 1 for each green reagent.

  4. Soluble manganese(IV) as a chemiluminescence reagent for the determination of opiate alkaloids, indoles and analytes of forensic interest.

    PubMed

    Brown, Allyson J; Lenehan, Claire E; Francis, Paul S; Dunstan, David E; Barnett, Neil W

    2007-03-30

    We present the results of our investigations into the use of soluble manganese(IV) as a chemiluminescence reagent, which include a significantly faster method of preparation and a study on the effect of formaldehyde and orthophosphoric acid concentration on signal intensity. Chemiluminescence detection was applied to the determination of 16 analytes, including opiate alkaloids, indoles and analytes of forensic interest, using flow injection analysis methodology. The soluble manganese(IV) reagent was less selective than either acidic potassium permanganate or tris(2,2'-bipyridyl)ruthenium(III) and therefore provided a more universal chemiluminescence detection system for HPLC. A broad spectral distribution with a maximum at 730+/-5nm was observed for the reaction between the soluble manganese(IV) and a range of analytes, as well as the background emission from the reaction with the formaldehyde enhancer. This spectral distribution matches that reported for chemiluminescence reactions with acidic potassium permanganate, where a manganese(II) emitting species was elucidated. This provides further evidence that the emission evoked in reactions with soluble manganese(IV) also emanates from a manganese(II) species, and not bimolecular singlet oxygen as suggested by previous authors.

  5. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    PubMed

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation.

  6. Safety assessment for TA-48 radiochemical operations

    SciTech Connect

    1994-08-01

    The purpose of this report is to document an assessment performed to evaluate the safety of the radiochemical operations conducted at the Los Alamos National Laboratory operations area designated as TA-48. This Safety Assessment for the TA-48 radiochemical operations was prepared to fulfill the requirements of US Department of Energy (DOE) Order 5481.1B, ``Safety Analysis and Review System.`` The area designated as TA-48 is operated by the Chemical Science and Technology (CST) Division and is involved with radiochemical operations associated with nuclear weapons testing, evaluation of samples collected from a variety of environmental sources, and nuclear medicine activities. This report documents a systematic evaluation of the hazards associated with the radiochemical operations that are conducted at TA-48. The accident analyses are limited to evaluation of the expected consequences associated with a few bounding accident scenarios that are selected as part of the hazard analysis. Section 2 of this report presents an executive summary and conclusions, Section 3 presents pertinent information concerning the TA-48 site and surrounding area, Section 4 presents a description of the TA-48 radiochemical operations, and Section 5 presents a description of the individual facilities. Section 6 of the report presents an evaluation of the hazards that are associated with the TA-48 operations and Section 7 presents a detailed analysis of selected accident scenarios.

  7. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode.

    PubMed

    Veera Manohara Reddy, Y; Prabhakara Rao, V; Vijaya Bhaskar Reddy, A; Lavanya, M; Venu, M; Lavanya, M; Madhavi, G

    2015-12-01

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1M phosphate buffer solution (PBS) at pH7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples.

  8. Synthesis and application of a new thiazolylazo reagent for cloud point extraction and determination of cobalt in pharmaceutical preparations.

    PubMed

    Yamaki, Regina Terumi; Nunes, Luana Sena; de Oliveira, Hygor Rodrigues; Araújo, André S; Bezerra, Marcos Almeida; Lemos, Valfredo Azevedo

    2011-01-01

    The synthesis and characterization of the reagent 2-(5-bromothiazolylazo)-4-chlorophenol and its application in the development of a preconcentration procedure for cobalt determination using flame atomic absorption spectrometry after cloud point extraction is presented. This procedure is based on cobalt complexing and entrapment of the metal chelates into micelles of a surfactant-rich phase of Triton X-114. The preconcentration procedure was optimized by using a response surface methodology through the application of the Box-Behnken matrix. Under optimum conditions, the procedure determined the presence of cobalt with an LOD of 2.8 microg/L and LOQ of 9.3 microg/L. The enrichment factor obtained was 25. The precision was evaluated as the RSD, which was 5.5% for 10 microg/L cobalt and 6.9% for 30 microg/L. The accuracy of the procedure was assessed by comparing the results with those found using inductively coupled plasma-optical emission spectrometry. After validation, the procedure was applied to the determination of cobalt in pharmaceutical preparation samples containing cobalamin (vitamin B12).

  9. Flow injection spectrophotometric determination of anionic surfactants using methyl orange as chromogenic reagent.

    PubMed

    He, Q; Chen, H

    2000-06-01

    A flow injection(FI) spectrophotometric method for the determination of anionic surfactants was developed on the basis of the competition for the cationic surfactant cetyl pyridine (CP+) chloride between the acidic dye methyl orange (MO) and anionic surfactants. In a pH 5.0 medium the cation of cetyl pyridine (CP+) reacts with dissociated methyl orange (MO-) to form an ion-associate complex, causing a blue shift of lambda(max) from 465 nm for MO- to 358 nm for the CP+ x MO- associate. The MO- in the ion-associate complex can be quantitatively substituted by such anionic surfactants as sodium dodecyl benzene sulfonate (DBS) or sodium lauryl sulfate (LS), leading to an increase in the absorbance measured at 465 nm. This increased absorbance value is proportional to the concentration of anionic surfactants. Various chemical and physical parameters for the FI spectrophotometric method were optimized, and interference-free levels were examined. At the optimized conditions, Beer's law was obeyed in the range 1.4 approximately 25 mg/L sodium DBS for an injected sample volume of 180 microL, and a detection limit of 0.22 mg/L for sodium DBS was achieved at a sampling rate of 90 h(-1). Eleven determinations of a 16 mg/L sodium DBS solution gave a RSD of 0.4%. The proposed method has successfully been applied to the determination of anionic surfactant concentration in waste water and in detergents.

  10. A novel chemiluminescence method for the determination of ergometrine maleate in serum sample without chemiluminescence reagent.

    PubMed

    Hu, Yufei; Zhang, Zhujun; Li, Gongke

    2010-04-15

    In this paper, a novel flow injection-chemiluminescence (FI-CL) method was proposed for the determination of ergometrine maleate in serum. The new CL reaction was based on the direct oxidation of ergometrine maleate by the complex of metal chelate diperiodatocuprate(III) (K(5)[Cu(HIO(6))(2)]) in an alkaline medium. The CL intensity was enhanced in the presence of ascorbic acid. Hereby under the optimum conditions, ergometrine maleate was determined over the range of 4.0 x 10(-9) gm L(-1) to 4.0 x 10(-7) gm L(-1) with a limit of detection (3 sigma) of 1.1 x 10(-9) gm L(-1). The relative standard deviation (R.S.D.) was 2.1% for 8.0 x 10(-9) gm L(-1) ergometrine maleate (n=7). The sensitive method was successfully applied to the direct determination of ergometrine maleate (ng mL(-1)) in pharmaceutical injection and serum samples. The mechanism of the reactions was also discussed.

  11. Deferiprone, a non-toxic reagent for determination of iron in samples via sequential injection analysis.

    PubMed

    Pragourpun, Kraivinee; Sakee, Uthai; Fernandez, Carlos; Kruanetr, Senee

    2015-05-05

    We present for the first time the use of deferiprone as a non-toxic complexing agent for the determination of iron by sequential injection analysis in pharmaceuticals and food samples. The method was based on the reaction of Fe(III) and deferiprone in phosphate buffer at pH 7.5 to give a Fe(III)-deferiprone complex, which showed a maximum absorption at 460nm. Under the optimum conditions, the linearity range for iron determination was found over the range of 0.05-3.0μgmL(-1) with a correlation coefficient (r(2)) of 0.9993. The limit of detection and limit of quantitation were 0.032μgmL(-1) and 0.055μgmL(-1), respectively. The relative standard deviation (%RSD) of the method was less than 5.0% (n=11), and the percentage recovery was found in the range of 96.0-104.0%. The proposed method was satisfactorily applied for the determination of Fe(III) in pharmaceuticals, water and food samples with a sampling rate of 60h(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Deferiprone, a non-toxic reagent for determination of iron in samples via sequential injection analysis

    NASA Astrophysics Data System (ADS)

    Pragourpun, Kraivinee; Sakee, Uthai; Fernandez, Carlos; Kruanetr, Senee

    2015-05-01

    We present for the first time the use of deferiprone as a non-toxic complexing agent for the determination of iron by sequential injection analysis in pharmaceuticals and food samples. The method was based on the reaction of Fe(III) and deferiprone in phosphate buffer at pH 7.5 to give a Fe(III)-deferiprone complex, which showed a maximum absorption at 460 nm. Under the optimum conditions, the linearity range for iron determination was found over the range of 0.05-3.0 μg mL-1 with a correlation coefficient (r2) of 0.9993. The limit of detection and limit of quantitation were 0.032 μg mL-1 and 0.055 μg mL-1, respectively. The relative standard deviation (%RSD) of the method was less than 5.0% (n = 11), and the percentage recovery was found in the range of 96.0-104.0%. The proposed method was satisfactorily applied for the determination of Fe(III) in pharmaceuticals, water and food samples with a sampling rate of 60 h-1.

  13. Flow injection colorimetric method using acidic ceric nitrate as reagent for determination of ethanol.

    PubMed

    Pinyou, Piyanut; Youngvises, Napaporn; Jakmunee, Jaroon

    2011-05-15

    Ceric ammonium nitrate has been used for qualitative analysis of ethanol. It forms an intensely colored unstable complex with alcohol. In this work, a simple flow injection (FI) colorimetric method was developed for the determination of ethanol, based on the reaction of ethanol with ceric ion in acidic medium to produce a red colored product having maximum absorption at 415 nm. Absorbance of this complex could be precisely measured in the FI system. A standard or sample solution was injected into a deionized water donor stream and flowed to a gas diffusion unit, where the ethanol diffused through a gas permeable membrane made of plumbing PTFE tape into an acceptor stream to react with ceric ammonium nitrate in nitric acid. Color intensity of the reddish product was monitored by a laboratory made LED based colorimeter and the signal was recorded on a computer as a peak. Peak height obtained was linearly proportional to the concentration of ethanol originally presented in the injected solution in the range of 0.1-10.0% (v/v) (r(2)=0.9993), with detection limit of 0.03% (v/v). With the use of gas diffusion membrane, most of the interferences could be eliminated. The proposed method was successfully applied for determination of ethanol in some alcoholic beverages, validating by gas chromatographic method. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. A new spectrophotometric method for the determination of tianeptine in tablets using ion-pair reagents.

    PubMed

    Ulu, Sevgi Tatar; Aydogmus, Zeynep

    2008-12-01

    A new rapid and sensitive procedure assay is proposed for the spectrophotometric determination of tianeptine. The developed method involves formation of colored chloroform extractable ion-pair complexes of tianeptine with bromophenol blue (BPB), bromocresol green (BCG), bromothymol blue (BTB) and methyl orange (MO) in acidic medium. Beer's law is obeyed in the concentration ranges 3.0-12.0, 4.0-16.0, 4.0-14.0 and 2.0-10.0 microg ml(-1) with BPB, BCG, BTB and MO, respectively. The detection limit of tianeptine was found to be 1.8 microg ml(-1) for BPB, 2.0 for BCG, 2.0 microg ml(-1) for BTB and 1.0 microg ml(-1) for MO. Validation of the method was performed in terms of linearity, limit of detection (LOD), quantification (LOQ), accuracy and precision. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed method. The proposed method has been applied to determination of the examined drugs in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise, and reproducible as the official method. The t-test showed no significant difference at 95% confidence level.

  15. Use of cloud point extraction with derivatizing reagent for the extraction and determination of isoniazid.

    PubMed

    Zhao, Wei-jun; Liu, Wei; Chen, Jian-bo; Zhou, Zhi-ming; Yang, Ming-min

    2011-02-01

    A simple and sensitive cloud point extraction high-performance liquid chromatography method is proposed for the determination of isoniazid in blood. The procedure is based on the product of the reaction of isoniazid with benzaldehyde. It can be validated that there is a linear relationship between the signal of isonicotinyl hydrazone and the concentration of isoniazid. A cloud point extraction system of nonionic surfactant Triton X-100 is applied for preconcentration of isonicotinyl hydrazone. Then the analytes in surfactant-rich phase are detected with HPLC-UV system. calibration graph was obtained in the range of 2.0 × 10(-3)-0.5 mg/L, the detection limit was 5.0 × 10(-4) mg/L. Method validation is performed on serum samples spiked at two levels, the recoveries ranging from 82.17-83.81%, with relative standard deviations from 2.45% to 3.89%.

  16. A modified manual method for the determination of urea in seawater using diacetylmonoxime reagent

    NASA Astrophysics Data System (ADS)

    Mulvenna, Pamela F.; Savidge, Graham

    1992-05-01

    A manual method for the quantitative determination of urea in seawater was developed based on the reaction of urea with diacetylmonoxime. Critical factors include the treatment of collection bottles, sample storage, pre-filtration techniques, water purification, reaction temperature and reproducible cooling of samples during analysis. The limit of detection was 0·14 μg-at urea-N 1 -1 with Beer's Law being obeyed in the range tested of 0-15 μg-at urea-N 1 -1. The precision (±1 SD) of replicate samples of 1,2 and 15 μg-at urea-N 1 -1 was 0·024, 0·019 and 0·03 μg-at urea-N 1 -1 ( n = 10) respectively.

  17. Novel reagents for the sensitive spectrophotometric determination of flutamide, an anticancer drug in pharmaceutical preparations.

    PubMed

    Nagaraja, Padmarajaiah; Arun Kumar, Hassan R; Vasantha, Ramanathapura A; Yathirajan, Hemmige S

    2002-03-20

    Simple and sensitive spectrophotometric methods for the determination of flutamide (FLA) in either pure form or in its pharmaceutical preparations are described. The first method is based on the diazotisation of reduced FLA, followed by coupling with alcoholic iminodibenzyl (IDB) in acid medium to give a purple coloured product having a lambda(max) of 570 nm. In the second method, the diazotisation of reduced FLA followed by coupling with 4-amino-5-hydroxy-2,7-naphthalenedisulphonic acid monosodium salt (AHND) in a buffer medium of pH 12, gives a red coloured product having a lambda(max) of 520 nm. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed methods. Both the methods are highly reproducible and have been applied to a wide variety of pharmaceutical preparations and the results compare favourably with the reported method.

  18. The enzymatic determination of bicarbonate and CO2 in reagents and buffer solutions.

    PubMed

    Hall, N P; Cornelius, M J; Keys, A J

    1983-07-01

    A method for the determination of bicarbonate in buffer solutions between pH 7.5 and 8.75 and in stock solutions of NaHCO3 is described. The HCO-3 is reacted with phosphoenolpyruvate (PEP) in the presence of PEP carboxylase (EC 4.1.1.31) and the oxaloacetate formed reduced to malate by NADH in the reaction catalyzed by malate dehydrogenase (EC 1.1.1.37). The extent of oxidation of NADH is measured spectrophotometrically. Experiments using standard solutions show that 1 mol of NADH is oxidized per mol of HCO-3 added. The method was used to establish the precautions needed to prepare buffer solutions containing less than 1% of the bicarbonate which would be present in the same buffers in equilibrium with air.

  19. [Determination of pesticide residues from seed coating reagent in agricultural products using ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Chen, Yue; Wang, Jinhua; Lu, Xiaoyu; Wang, Wanchun; Huang, Mei; Xu, Chaoyi

    2008-11-01

    An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) has been developed for the simultaneous determination of eight pesticide residues from seed coating in fruits, vegetable and grain. The sample was extracted by methanol-water (1:1, v/v) and determined by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry in positive mode (ESI+) and multiple reaction monitoring (MRM) mode. The UPLC analyses were performed on an Acquity UPLC C18 column with gradient eluation. The utility of the method was demonstrated by the analysis of crude extracts, with no sample clean up, from soybean. The linear range was 1 - 200 microg/L. The correlation coefficients (r) were under 0.997. The average recoveries of eight pesticides in samples (from 0.006 to 1.2 mg/kg) ranged from 60% to 110%, and the relative standard deviations (RSDs) were less than 10%. The results indicate that the method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of pesticide residues from seed coating reagent in fruit, vegetable and grain samples.

  20. Waveband selection of reagent-free determination for thalassemia screening indicators using Fourier transform infrared spectroscopy with attenuated total reflection.

    PubMed

    Long, Xiaoli; Liu, Guisong; Pan, Tao; Chen, Jiemei

    2014-08-01

    A reagent-free determination method for the thalassemia screening indicators hemoglobin (Hb), mean corpuscular Hb (MCH), and mean corpuscular volume (MCV) was developed based on Fourier transform infrared spectrometers equipped with an attenuated total reflection accessory. A random and stability-dependent rigorous process of calibration, prediction, and validation was conducted. Appropriate wavebands were selected using the improved moving window partial least squares method with stability and equivalence. The obtained optimal wavebands were 1722 to 1504 cm⁻¹ for Hb, 1653 to 901 cm⁻¹ for MCH, and 1562 to 964 cm⁻¹ for MCV. A model set equivalent to the optimal model was proposed for each indicator; the public waveband of Hb equivalent wavebands was 1717 to 1510 cm⁻¹, and the public equivalent waveband for MCH and MCV was 1562 to 901 cm⁻¹. All selected wavebands were within the MIR fingerprint region and achieved high validation effects. The sensitivity and specificity were 100.0% and 96.9% for the optimal wavebands and 100.0% and 95.3% for the equivalent wavebands, respectively. Thus, the spectral prediction was highly accurate for determining negative and positive for thalassemia screening. This technique is rapid and simple in comparison with conventional methods and is a promising tool for thalassemia screening in large populations.

  1. Spectrofluorometric determination and chemical speciation of trace concentrations of tungsten species in water using the ion pairing reagent procaine hydrochloride.

    PubMed

    El-Shahawi, M S; Al Khateeb, L A

    2012-01-15

    A highly selective and low cost extractive spectrofluorimetric method was developed for determination of trace concentrations of tungsten (VI) in water. The method was based upon solvent extraction of the developed ion associate [(PQH(+))(2)·WO(4)(2-)] of the fluorescent ion-pairing reagent [2-(diethylamino)ethyl 4 aminobenzoate] hydrochloride namely procaine hydrochloride, PQH(+)·Cl(-) and tungstate (WO(4)(2-)) in aqueous solution of pH 6-7 followed by measuring the resulting fluorescence enhancement in n-hexane at λ(ex/em)=270/320nm. The fluorescence intensity of PQH(+)·Cl(-) increased linearly on increasing tungstate concentration in the range 25-250μgL(-1). The limits of detection (LOD) and quantification (LOQ) of tungsten (VI) were found 7.51 and 24.75μgL(-1), respectively. Chemical composition of the developed ion associate and the molar absorptivity at 270nm were found to be [(PQH(+))(2)·WO(4)(2-)] and 2.7×10(4)Lmol(-1)cm(-1), respectively. Other oxidation states (III, IV, V) of tungsten species could also be determined after oxidation with H(2)O(2) in aqueous solution to tungsten (VI). The method was applied for analysis of tungsten in certified reference material (IAEA Soil-7) and wastewater samples. The results were compared successfully (>95%) with the data of inductively coupled plasma-mass spectrometry (ICP-MS).

  2. Ethyl chloroformate as a derivatizing reagent for the gas chromatographic determination of isoniazid and hydrazine in pharmaceutical preparations.

    PubMed

    Khuhawar, Mohammad Yar; Zardari, Liaquat Ali

    2008-01-01

    Ethyl chloroformate was examined as a precolumn derivatizing reagent for the gas chromatographic (GC) determination of isoniazid (INH) and hydrazine (HZ). Phenylhydrazine (PHZ) was used as an internal standard. GC separation was carried out on an HP-5 column (30 m x 0.32 mm i.d.) with flame ionization detection. The elution was carried out at an initial column temperature of 150 degrees C for 1 min at a heating rate of 10 degrees C/min up to 250 degrees C, nitrogen flow rate of 4 ml/min and a split ratio of 10:1, v/v. The linear calibration ranges for INH and HZ were observed between 3.5-37.5 and 3.5-35 microg/ml with corresponding detection limits of 0.18 and 0.17 ng reaching the detector. The method was subsequently applied to the determination of INH and HZ in pharmaceutical preparations, achieving a relative standard deviation (RSD) of 3.8-5.8%. The recovery percentage of INH from isoniazid syrup was 98% with an RSD of 5.2%.

  3. Reagent-Less and Robust Biosensor for Direct Determination of Lactate in Food Samples.

    PubMed

    Bravo, Iria; Revenga-Parra, Mónica; Pariente, Félix; Lorenzo, Encarnación

    2017-01-13

    Lactic acid is a relevant analyte in the food industry, since it affects the flavor, freshness, and storage quality of several products, such as milk and dairy products, juices, or wines. It is the product of lactose or malo-lactic fermentation. In this work, we developed a lactate biosensor based on the immobilization of lactate oxidase (LOx) onto N,N'-Bis(3,4-dihydroxybenzylidene) -1,2-diaminobenzene Schiff base tetradentate ligand-modified gold nanoparticles (3,4DHS-AuNPs) deposited onto screen-printed carbon electrodes, which exhibit a potent electrocatalytic effect towards hydrogen peroxide oxidation/reduction. 3,4DHS-AuNPs were synthesized within a unique reaction step, in which 3,4DHS acts as reducing/capping/modifier agent for the generation of stable colloidal suspensions of Schiff base ligand-AuNPs assemblies of controlled size. The ligand-in addition to its reduction action-provides a robust coating to gold nanoparticles and a catalytic function. Lactate oxidase (LOx) catalyzes the conversion of l-lactate to pyruvate in the presence of oxygen, producing hydrogen peroxide, which is catalytically oxidized at 3,4DHS-AuNPs modified screen-printed carbon electrodes at +0.2 V. The measured electrocatalytic current is directly proportional to the concentration of peroxide, which is related to the amount of lactate present in the sample. The developed biosensor shows a detection limit of 2.6 μM lactate and a sensitivity of 5.1 ± 0.1 μA·mM(-1). The utility of the device has been demonstrated by the determination of the lactate content in different matrixes (white wine, beer, and yogurt). The obtained results compare well to those obtained using a standard enzymatic-spectrophotometric assay kit.

  4. Reagent-Less and Robust Biosensor for Direct Determination of Lactate in Food Samples

    PubMed Central

    Bravo, Iria; Revenga-Parra, Mónica; Pariente, Félix; Lorenzo, Encarnación

    2017-01-01

    Lactic acid is a relevant analyte in the food industry, since it affects the flavor, freshness, and storage quality of several products, such as milk and dairy products, juices, or wines. It is the product of lactose or malo-lactic fermentation. In this work, we developed a lactate biosensor based on the immobilization of lactate oxidase (LOx) onto N,N′-Bis(3,4-dihydroxybenzylidene) -1,2-diaminobenzene Schiff base tetradentate ligand-modified gold nanoparticles (3,4DHS–AuNPs) deposited onto screen-printed carbon electrodes, which exhibit a potent electrocatalytic effect towards hydrogen peroxide oxidation/reduction. 3,4DHS–AuNPs were synthesized within a unique reaction step, in which 3,4DHS acts as reducing/capping/modifier agent for the generation of stable colloidal suspensions of Schiff base ligand–AuNPs assemblies of controlled size. The ligand—in addition to its reduction action—provides a robust coating to gold nanoparticles and a catalytic function. Lactate oxidase (LOx) catalyzes the conversion of l-lactate to pyruvate in the presence of oxygen, producing hydrogen peroxide, which is catalytically oxidized at 3,4DHS–AuNPs modified screen-printed carbon electrodes at +0.2 V. The measured electrocatalytic current is directly proportional to the concentration of peroxide, which is related to the amount of lactate present in the sample. The developed biosensor shows a detection limit of 2.6 μM lactate and a sensitivity of 5.1 ± 0.1 μA·mM−1. The utility of the device has been demonstrated by the determination of the lactate content in different matrixes (white wine, beer, and yogurt). The obtained results compare well to those obtained using a standard enzymatic-spectrophotometric assay kit. PMID:28098753

  5. Determination of efficacy of fingermark enhancement reagents; the use of propyl chloroformate for the derivatization of fingerprint amino acids extracted from paper.

    PubMed

    Mink, Tineke; Voorhaar, Annelies; Stoel, Reinoud; de Puit, Marcel

    2013-09-01

    The analysis of the constituents of fingerprints has been described numerous times, mainly with the purpose of determining the aging effect on fingerprints or showing the differences between donors or groups of donors. In this paper we describe the use of derivatized amino acids to determine the efficacy of the visualization reagents 1,8-diazafluoren-9-one (DFO) and ninhydrin. At present certain conditions are used for the application of these reagents, as determined by trial-and-error investigations, to the effect on fingerprints. The recovery of amino acids from a porous surface can be used as a measure for the efficacy of a visualization agent. In this paper we describe a method for the determination of the amount of amino acid left after reaction with well known fingerprint visualization reagents. This will allow a more scientific approach to method development for fingermark enhancement techniques. Furthermore, investigations on the influence of the concentration of fingermark amino acids, the order of application of and exposure time to reagents and the influence of age of the amino acids were carried out. These studies have resulted in a broader understanding of the mechanism involved in visualization of fingermarks using DFO and ninhydrin.

  6. Extractive liquid-liquid spectrophotometric procedure for the determination of thiocyanate ions employing the ion pair reagent amiloride monohydrochloride.

    PubMed

    Bashammakh, A S; Bahaffi, S O; Al-Sibaai, A A; Al-Wael, H O; El-Shahawi, M S

    2007-05-29

    An accurate, inexpensive and less laborious liquid-liquid extractive spectrophotometric procedure for the determination of thiocyanate ions in aqueous media has been developed. The method has been based upon the formation of a yellow colored complex ion associate of the ion-pairing reagent 1-(3, 5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride hydrochloride, DPG+.Cl- and the thiocyanate ions in aqueous media containing HNO3 (0.5 mol L(-1)) and subsequent extraction with 4-methyl-2-pentanone. The absorption electronic spectrum of the ion associate showed one well-defined peak at lambda(max) 366 nm. The stoichiometric mole ratio of DPG+.Cl- to the thiocyanate ions is 1:1. The effective molar absorptivity (epsilon) of the ion associate at lambda(max) 366 nm is 1.1+/-0.1x10(4) L mol(-1) cm(-1). The extraction constants (K(d), K(ex), and beta) enabled a simple and convenient use of the developed binary ion associate for the extractive spectrophotometric determination of traces of thiocyanate ions in the aqueous media. Beer's law and Ringbom's plots are obeyed in the concentration range 0.05-10 and 0.1-7 microg mL(-1) of the thiocyanate ions, respectively with a relative standard deviation of +/-2.3%. The calculated lower limits of detection (LOD) and quantitation (LOQ) of the developed procedure for the thiocyanate ions were found equal to 0.02 and 0.066 microg mL(-1), respectively. The developed method has been applied for the determination of trace amounts of thiocyanate ions in tap-, waste- and natural water samples and compared successfully with the reported methods at the 95% confidence level. The proposed method was also applied successfully for the determination of thiocyanate ions in saliva samples.

  7. Radiochemical Solar Neutrino Experiments - Successful and Otherwise.

    SciTech Connect

    Hahn,R.L.

    2008-05-25

    Over the years, several different radiochemical systems have been proposed as solar neutrino detectors. Of these, two achieved operating status and obtained important results that helped to define the current field of neutrino physics: the first solar-neutrino experiment, the Chlorine Detector ({sup 37}Cl) that was developed by chemist Raymond Davis and colleagues at the Homestake Mine, and the subsequent Gallium ({sup 71}Ga) Detectors that were operated by (a) the SAGE collaboration at the Baksan Laboratory and (b) the GALLEX/GNO collaborations at the Gran Sasso National Laboratory. These experiments have been extensively discussed in the literature and in many previous International Neutrino Conferences. In this paper, I present important updates to the results from SAGE and GALLEX/GNO. I also review the principles of the radiochemical detectors and briefly describe several different detectors that have been proposed. In light of the well-known successes that have been subsequently obtained by real-time neutrino detectors such as Kamiokande, Super-Kamiokande, SNO, and KamLAND, I do not anticipate that any new radiochemical neutrino detectors will be built. At present, only SAGE is still operating; the Chlorine and GNO radiochemical detectors have been decommissioned and dismantled.

  8. Acetylacetone as chelating reagent, extracting solvent, and electrolysis medium: Polarographic determination of uranium(VI) and iron(III).

    PubMed

    Fujinaga, T; Lee, H L

    1977-06-01

    The chelating reagent acetylacetone has been examined as a polarographic medium; a method for its purification has been developed and it is found that the specific conductance is 4.2 x 10(-8) mho/cm, the accessible potential ranges are from -0.16 to -2.26 V vs. Ag/0.1M AgClO(4) for the pure solvent and from -0.35 to -2.20 V in the solvent after extraction. In pure solvent ferric acetylacetonate exhibits one wave and the uranyl complex gives two waves. After extraction from aqueous solution at pH 6.8-7.0, both metal acetylacetonates are reduced more reversibly and at more positive potential than in the pure solvent. Calibration curves are linear in the range 10(-5) -10(-3)M metal ion in the extract. The direct polarographic determination of uranium and iron in acetylacetone after extraction of the chelate from aqueous solution has been developed.

  9. Determination and control of TEMPO, a potentially genotoxic free radical reagent used in the synthesis of filibuvir.

    PubMed

    Strohmeyer, Holly E; Sluggett, Gregory W

    2012-03-25

    The synthesis of filibuvir, a hepatitis C virus polymerase inhibitor candidate, involves use of 2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO), a potentially genotoxic free radical reagent. A headspace gas chromatographic method utilizing selected-ion monitoring (SIM) mode mass spectrometric detection was developed, validated and applied to the determination of low levels of TEMPO in filibuvir. The GC-MS method was validated in terms of specificity, linearity, precision, accuracy/recovery, limit of quantitation (LOQ) and limit of detection (LOD). The method was shown to be specific for detection of TEMPO in the presence of filibuvir and exhibited acceptable linearity (r ≥ 0.997) over the range of 4-60 ppm vs. filibuvir (0.4-6.0 μg/mL). The system precision was 14% and 8% relative standard deviation (RSD) at the 4 ppm and 8 ppm levels, respectively. Method repeatability was 15% and 13% RSD at the 4 ppm and 8 ppm levels, respectively. Recovery was approximately 50-80% across the method range. Accuracy was 135% and 91% vs. nominal at the 4 and 8 ppm levels, respectively. The LOQ and LOD are 4 ppm and 2 ppm, respectively. Thirteen batches of filibuvir drug substance had no detectable TEMPO (≤ 2 ppm). Purge studies demonstrated that the synthetic process has an extremely high capability to remove TEMPO and consistently delivers filibuvir drug substance with TEMPO levels well below the staged threshold of toxicological concern.

  10. Evaluation of two derivatization reagents for the determination by LC-MS/MS of ammonia in cigarette mainstream smoke.

    PubMed

    Mottier, Nicolas; Jeanneret, Florent

    2011-01-12

    Ammonia in cigarette mainstream smoke was quantified by LC-MS/MS after derivatization. Two different reagents, fluorescamine and dansyl chloride, were investigated, but only the latter gave stable derivatives; therefore, it was considered the most appropriate choice. Smoke samples were collected on a Cambridge filter pad followed by an impinger containing a solution of hydrochloric acid. Ammonia was then derivatized with a 18.5 mM solution of dansyl chloride in acetonitrile at 70 °C for 30 min in a vial with the internal standard, (15)ND(4)Cl. The resulting derivative was analyzed by LC-MS/MS detection with an atmospheric pressure chemical ionization (APCI) interface in the positive ionization mode using multiple-reaction monitoring (MRM). Good linearity was obtained in the concentration range of 0.02-1.65 μg/mL (r(2) ≥ 0.999), and the limit of detection (LOD) was established at 0.006 μg/mL. This method has the advantage of being sensitive, efficient, and reliable and is not hindered by interferences from the sample matrix. It should thus be considered a reference method of choice for the determination of ammonia in smoke.

  11. Determination of malondialdehyde in biological fluids by high-performance liquid chromatography using rhodamine B hydrazide as the derivatization reagent.

    PubMed

    Li, Pingliang; Ding, Guanglong; Deng, Yufang; Punyapitak, Darunee; Li, Deguang; Cao, Yongsong

    2013-12-01

    Malondialdehyde (MDA) is a biomarker for lipid peroxidation, and studies of sensitive and selective analytical methods for it are very important for pathological research. The aim of this work was to develop and validate a novel HPLC method for the quantification of MDA in biological fluids using rhodamine B hydrazide (RBH) as the derivatization reagent. After pretreatment and derivatization in acid medium at 50 °C for 40 min, the RBH-derivatized MDA was separated on a Kromasil C18 column at 25 °C and detected by a fluorescence detector at excitation wavelength of 560 nm and emission wavelength of 580 nm. The results showed linearity in the range of 0.8-1500.0 nM with a detection limit of 0.25 nM (S/N = 3). The recovery of MDA from plasma and urine was 91.50 to 99.20%, with a relative standard deviation range of 1.45 to 3.26%. In comparison to other methods reported for the determination of MDA, the proposed method showed superiority in simplicity, more sensitivity, shorter derivatization time, and less interference. The developed method was applied to quantification of MDA in human biological fluids collected from five volunteers with a concentration range of 24.62-245.00 nM. Copyright © 2013. Published by Elsevier Inc.

  12. An improved reagent for determination of aliphatic amines with fluorescence and online atmospheric chemical ionization-mass spectrometry identification.

    PubMed

    You, Jinmao; Song, Cuihua; Yan, Tao; Sun, Zhiwei; Li, Yulin; Suo, Yourui

    2010-01-18

    An improved reagent named 2-[2-(dibenzocarbazole)-ethoxy] ethyl chloroformate (DBCEC-Cl) for the determination of aliphatic amines by high-performance liquid chromatography (HPLC) with fluorescence detection and post-column online atmospheric chemical ionization-mass spectrometry (APCI-MS) identification has been developed. DBCEC-Cl could easily and quickly label aliphatic amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+H](+) under APCI-MS in positive-ion mode. The ratios for fluorescence responses were I(DBCEC-amine)/I(BCEC-amine)=1.02-1.60; I(DBCEC-amine)/I(BCEOC-amine)=1.30-2.57; and I(DBCEC-amine)/I(FMOC-amine)=2.20-4.12 (here, I was relative fluorescence intensity). The ratios for MS responses were IC(DBCEC-amine)/IC(BCEC-amine)=4.16-29.31 and IC(DBCEC-amine)/IC(BCEOC-amine)=1.23-2.47 (Here, IC: APCI-MS ion current intensity). Detection limits calculated from 0.0244 pmol injection, at a signal-to-noise ratio of 3, were 0.3-3.0 fmol. The relative standard deviations for within-day determination (n=6) were 0.045-0.081% for retention time and 0.86-1.03% for peak area for the tested aliphatic amines. The mean intra- and inter-assay precision for all amine levels were <3.64% and 4.67%, respectively. The mean recoveries ranged from 96.9% to 104.7% with their standard deviations in the range of 1.80-2.70 (RSDs%). Excellent linear responses were observed with coefficients of >0.9991. Copyright 2009 Elsevier B.V. All rights reserved.

  13. Spectrophotometric determination of copper in alkaline solutions and evaluation of some hydroxy-substituted 1,10-phenanthrolines as chromogenic reagents.

    PubMed

    Dunbar, W E; Schilt, A A

    1972-09-01

    Seven new hydroxy-substituted 1,10-phenanthroline derivatives have been evaluated as chromogenic reagents for the determination of copper in strongly alkaline solution. The most sensitive of these, 2,9-dimethyl-4,7-dihydroxy-1,10-phenanthroline, has proven to be highly effective in a simple, rapid procedure for determining trace amounts of copper in sodium hydroxide, potassium carbonate, sodium phosphate or ammonium hydroxide.

  14. Evaluation of N-bromosuccinimide as a new analytical reagent for the spectrophotometric determination of fluoroquinolone antibiotics.

    PubMed

    Askal, Hassan; Refaat, Ibrahim; Darwish, Ibrahim; Marzouq, Mostafa

    2007-11-01

    Analytical studies were carried out, for the first time, to evaluate the use of N-bromosuccinimide (NBS) as an analytical reagent for the spectrophotometric determination of eleven therapeutically important fluoroquinolone antibiotics (FQA). The procedures involved the reaction of the FQA with NBS and subsequent measurement of the excess NBS by its reaction with p-phenylenediamine (PDA) to give a violet colored product that was measured at 530 nm. Different variables affecting the reaction (concentration of NBS, concentration of PDA, pH of reaction medium, reaction time, and the diluting solvents) were carefully studied and optimized. The molar ratio and mechanism of the reaction between each of the studied FQA with NBS were proposed using UV-vis, IR, and NMR techniques. Under the optimum reaction conditions, the analytical method was developed and validated. Beer's law was obeyed in the general concentration range of 3-25 microg/ml. The assay limits of detection and quantitation were 0.33-1.29 and 1.10-4.31 microg/ml, respectively. The precision of the method was satisfactory; the values of relative standard deviations did not exceed 2%. The proposed method was successfully applied to the analysis of the investigated FQA in their pure and pharmaceutical dosage forms without interference from the common excipients (label claim values were 99.85-100.17+/-0.13-0.59%). Interference from ascorbic acid, that is co-formulated as a stabilizer for the ampoule form, was avoided by its pre-oxidation with potassium bromate before applying the analytical procedure. The results obtained by the proposed method were comparable with those obtained by the official and reported methods.

  15. Chemiluminescence determination of antibacterial drug trimethoprim by automated sequential injection technique with permanganate and hexametaphosphate as reagents.

    PubMed

    Polásek, Miroslav; Jambor, Michal

    2002-12-06

    Antibacterial drug trimethoprim [2,4-diamino-5-(3,4,5-trimethoxybenzyl)-pyrimidine] (I) was determined in pharmaceutical formulations by using a lab-made PC-controlled SIA analyser linked to conventional HPLC fluorimetric detector equipped with a chemiluminescence module. The chemical principle is the oxidation of I by KMnO(4) in acid medium; the reaction is accompanied by the emission of chemiluminescence, which is enhanced in the presence of hexametaphosphate (HMP). The optimum sequence and the flow parameters and concentrations and volumes of reagents aspirated optimised by a computer-aided simplex method were, 100 mul of 5 mM HMP, 40 mul of a test solution of I, 2 mul of 0.5 M H(2)SO(4) and 20 mul of 1 mM KMnO(4); the luminescing zone was pushed into the detector at a flow rate of 49 mul s(-1). The calibration graph relating the intensity of luminescence to concentration of I was parabolic (r=0.9994) in the range 0.5-100 mug ml(-1) of I with rectilinear part (r=0.9999) in the range 20-100 mug ml(-1) of I; the limit of detection was 0.1 mug ml(-1) of I. The method was used for the assay of Triprim(R) tablets (with nominal content 100 or 200 mg of I) for the active substance as well as for content uniformity tests; the R.S.D. values did not exceed 1% (n=5). The SIA results did not show statistical difference from those obtained by pharmacopoeial acidimetric titration in non-aqueous medium; the excipients such as microcrystalline cellulose, maze starch, povidone, talc, magnesium stearate and gelatin did not interfere.

  16. Rapid, synergistic extractive spectrophotometric determination of copper(II) by using sensitive chromogenic reagent N″,N″‧-bis[(E)-(4-fluorophenyl) methylidene]thiocarbonohydrazide

    NASA Astrophysics Data System (ADS)

    Nalawade, Rekha A.; Nalawade, Avinash M.; Kamble, Ganesh S.; Anuse, Mansing A.

    2015-07-01

    A rapid and simple spectrophotometric method was developed for the determination of copper(II) by using newly synthesized chromogenic reagent, N″,N″‧-bis[(E)-(4-fluorophenyl)methylidene]thiocarbonohydrazide [bis(4-fluoroPM)TCH]. The reagent is highly sensitive and it forms yellow colored ternary complex with copper(II) in presence pyridine having composition 1:1:2 (M:L:Py) in the acidic pH range. Absorption of colored complex in amyl acetate is measured with reagent as a blank at λmax 375 nm. The synergistic effect is observed due to pyridine forming adduct with reagent in the organic phase. Beer's law was obeyed in the concentration range from 2.0 to 14 μg mL-1 for copper(II)-[bis(4-fluoroPM)TCH]-Py complex. Molar absorptivity and Sandell's sensitivity values for Cu(II)-bis(4-fluoroPM)TCH]-Py complex are 0.42545 × 105 and 0.0014 μg/cm2, respectively. The selectivity of the developed method was checked in the presence of various foreign ions. The developed method showed relative standard deviation (R.S.D.) of 0.13% for n = 10. The composition of Cu(II)-[bis(4-fluoroPM)TCH]-Py complex was determined by known methods such as Job's method of continuous variation, mole ratio method and slope ratio method. It is found that the ternary complex is stable for more than 24 h. Various factors influencing on the degree of complexation, such as, effect of pH, reagent concentration, synergent concentration, solvent etc. were studied. The accuracy and reliability of method was verified by AAS. This method is found to be simple, rapid and reproducible.

  17. Influence of reagent purity on the ion chromatographic determination of bromate in water using 3,3'-dimethoxybenzidine as a prochromophore for photometric detection.

    PubMed

    Urbansky, E T; Brown, S K

    2000-12-01

    Variable availability of the purified dihydrochloride salt of 3,3'-dimethoxybenzidine (DMB; ortho-dianisidine) led us to investigate the effects of reagent purity on the analytical results obtained when this reagent is used in the photometric determination of the disinfection byproduct bromate. After analyte ions are separated by ion chromatography, a solution of DMB (post-column reagent) is added to the eluate and the DMB is oxidized, thereby producing a chromophore detected by its absorbance. Although some commercial products of undefined grade performed well, others did not. Variability was also observed between lots of purified material. Sensitivity at low concentrations (< 5 micrograms L-1 BrO3-) varied by a factor of up to 10. In some cases, the lower limit of detection for photometric detection was greater than that obtained using conductivity detection, as high as 5-7 micrograms L-1 BrO3-. An impurity or several impurities are suspected to be responsible for deviations from linearity at low analyte concentrations. This investigation underscores the need for ensuring reagent purity in environmental analyses. Ideally, chemical manufacturers will meet the needs of analytical chemists who test potable water and begin producing a high grade material in sufficient quantities to meet monitoring requirements. The establishment of third-party standards for a spectrophotometric grade of DMB.2HCl would be helpful in ensuring that a variety of manufacturers could supply products of uniformly high quality that would be suitable for the measurement of bromate in public drinking water supplies.

  18. Spectrophotometric studies of 4-[N'-(4-imino-2-oxo-thiazolidin-5-ylidene)-hydrazino]-benzenesulfonic acid as a reagent for the determination of palladium.

    PubMed

    Lozynska, Lesya; Tymoshuk, Oleksandr; Chaban, Taras

    2015-01-01

    The spectrophotometric behavior of a new, first-time synthesized reagent - 4-[N'-(4-imino-2-oxo-thiazolidin-5-ylidene)hydrazino]-benzenesulfonic acid (ITHBA), has been investigated. A simple, rapid, accurate, selective and sensitive method for the spectrophotometric determination of Pd(II) ions using this reagent was developed. The optimal conditions for the formation of the complexes were found. The molar absorptivity at λ = 438 nm is 7.5 × 10(3) L mol(-1) cm(-1), and Beer's law is observed for the concentrations ranging from 0.2-2.2 µg mL-1Pd(II). The effects of extraneous ions were investigated. The method proved to be successful in determination of palladium in the intermetallides and resistor. The accuracy of spectrophotometric palladium assay in real objects with 4-[N'-(4-imino-2-oxo-thiazolidin-5-ylidene)-hydrazino]-benzenesulfonic acid has been confirmed by voltammetric or atomic absorption spectroscopy method.

  19. Aqueous-phase quantitative NMR determination of amino acid enantiomer ratio by 13C-NMR using chiral neodymium shift reagent.

    PubMed

    Florini, Nicola; Faglioni, Francesco; Zucchi, Claudia; Caglioti, Luciano; Pályi, Gyula

    2010-05-01

    A neodymium-(S)-PDTA (PDTA = N,N,N',N'-tetrakis[(hydroxycarbonyl)methyl]-1,2-diaminopropane) complex was found exceptionally useful in the quantitative determination of enantiomer ratios of water-soluble natural amino acids by (13)C-NMR. The method is demonstrated on mixtures of L- and D-enantiomers of various amino acids. The interactions of the chiral shift reagent with the amino acid molecules were rationalized by molecular orbital calculations.

  20. Application of a sensitive and specific reagent for the determination of serum iron to the Bayer DAX48.

    PubMed

    Artiss, J D; Yang, W C; Harake, B; Capellari, E; Kretch, C; Eisenbrey, A B; Zak, B

    1997-09-01

    We describe a modification of a previously described serum iron procedure applied to the Bayer DAX48 (Bayer Diagnostics, Tarrytown, NY) automated chemistry analyzer. The iron-ligand used in this assay, 2-(5-nitro-2-pyridylazo)-5-(N-propyl-N-sulfopropylamine) phenol (nitro-PAPS), has a molar absorptivity of 94,000 L mol(-1) cm(-1), which is three to four times more sensitive than the more commonly used ligands. The increased sensitivity of the iron-ligand complex facilitates modification of a Ferene S method that requires a smaller sample volume while it maintains the precision of the assay. Because the reagent does not contain ascorbate, the "onboard" stability has been increased to more than 4 weeks. The reagent seems to be quite insensitive to icterus and hemolysis. Furthermore, the interference of turbidity caused by triglycerides, abnormal proteins, or fibrinogen, present in samples from patients undergoing anticoagulant therapy, seems to have been eliminated.

  1. CF3(+) and CF2H(+): new reagents for n-alkane determination in chemical ionisation reaction mass spectrometry.

    PubMed

    Blake, Robert S; Ouheda, Saleh A; Evans, Corey J; Monks, Paul S

    2016-11-28

    Alkanes provide a particular analytical challenge to commonly used chemical ionisation methods such as proton-transfer from water owing to their basicity. It is demonstrated that the fluorocarbon ions CF3(+) and CF2H(+), generated from CF4, as reagents provide an effective means of detecting light n-alkanes in the range C2-C6 using direct chemical ionisation mass spectrometry. The present work assesses the applicability of the reagents in Chemical Ionisation Mass Spectrometric (CI-TOF-MS) environments with factors such as high moisture content, operating pressures of 1-10 Torr, accelerating electric fields (E/N) and long-lived intermediate complex formation. Of the commonly used chemical ionisation reagents, H3O(+) and NO(+) only react with hexane and higher while O2(+) reacts with all the target samples, but creates significant fragmentation. By contrast, CF3(+) and CF2H(+) acting together were found to produce little or no fragmentation. In dry conditions with E/N = 100 Td or higher the relative intensity of CF2H(+) to CF3(+) was mostly less than 1% but always less than 3%, making CF3(+) the main reagent ion. Using O2(+) in a parallel series of experiments, a substantially greater degree of fragmentation was observed. The detection sensitivities of the alkanes with CF3(+) and CF2H(+), while relatively low, were found to be better than those observed with O2(+). Experiments using alkane mixtures in the ppm range have shown the ionisation technique based on CF3(+) and CF2H(+) to be particularly useful for measurements of alkane/air mixtures found in polluted environments. As a demonstration of the technique's effectiveness in complex mixtures, the detection of n-alkanes in a smoker's breath is demonstrated.

  2. Lung cancer of radiochemical industry workers

    SciTech Connect

    Khokhryakov, V.F.; Romanov, S.A.

    1993-12-31

    The frequency of lung cancers among 2346 radiochemical industry workers exposed to combined external {beta}-{gamma} and internal incorporated plutonium irradiation has been investigated. The results of observation were analyzed assuming the linear relative risk model taking into account prolongation of exposure. On the basis of the obtained data it was shown that life span incidence, of radiation-induced lung cancer is several times greater than 8.5 x 10{sup -3}Sv{sup -1}, which is recommended by ICRP Publication 60 to estimate the carcinogenic risk of organ exposure.

  3. A sensitive fluorescence reagent for the determination of aldehydes from alcoholic beverage using high-performance liquid chromatography with fluorescence detection and mass spectrometric identification.

    PubMed

    You, Jinmao; Yan, Tao; Zhao, Huaixin; Sun, Zhiwei; Xia, Lian; Suo, Yourui; Li, Yulin

    2009-03-16

    A pre-column derivatization method for the sensitive determination of aldehydes using the tagging reagent 2-[2-(7H-dibenzo[a,g] carbazol-7-yl)-ethoxy] ethyl carbonylhydrazine (DBCEEC) followed by high-performance liquid chromatography with fluorescence detection and APCI-MS identification has been developed. The chromophore of fluoren-9-methoxy-carbonylhydrazine (Fmoc-hydrazine) reagent was replaced by 2-[2-(7H-dibenzo[a,g] carbazol-7-yl)-ethoxy] ethyl functional group, which resulted in a sensitive fluorescence tagging reagent DBCEEC. DBCEEC could easily and quickly labeled aldehydes. The maximum excitation (300nm) and emission (400nm) wavelengths did not essentially change for all the aldehyde derivatives. Derivatives were sufficiently stable to be efficiently analyzed by high-performance liquid chromatography. The derivatives showed an intense protonated molecular ion corresponding m/z [M+(CH(2))(n)](+) in positive-ion mode (M: molecular weight of DBCEEC, n: corresponding aldehyde carbon atom numbers). The collision-induced dissociation of protonated molecular ion formed fragment ions at m/z 294.6, m/z 338.6 and m/z 356.5. Studies on derivatization demonstrated excellent derivative yields in the presence of trichloroacetic acid (TCA) catalyst. Maximal yields close to 100% were observed with a 10 to 15-fold molar reagent excess. Separation of the derivatized aldehydes had been optimized on ZORBAX Eclipse XDB-C(8) column with aqueous acetonitrile as mobile phase in conjunction with a binary gradient elution. Excellent linear responses were observed at the concentration range of 0.01-10nmolmL(-1) with coefficients of >0.9991. Detection limits obtained by the analysis of a derivatized standard containing 0.01nmolmL(-1) of each aldehyde, were from 0.2 to 1.78nmolL(-1) (at a signal-to-noise ratio of 3).

  4. Radiochemical evaluation for debris-induced failures

    SciTech Connect

    Goncarovs, G. )

    1993-06-01

    Radiochemical trends and anomalies experienced during cycle 15 of the Haddam Neck nuclear power plant, as a result of > 450 debris-induced fuel rod failures, presented a situation previously unreported in the nuclear industry. These data, along with shutdown and depressurization spiking data, needed to be evaluated against ultrasonic fuel assembly examination results to derive a predictive model, called the xenon pin equivalent (XPE), to be used for cycle 16. During the development of the model, a fission product release mechanism for this particular type of failure needed to be postulated based on cycle 15 data. The predictive model was tested during cycle 16, which presented similar but more subtle radiochemical trends than cycle 15. Several operational events affected the XPE model, including use of degasification and down-power maneuvers. After the cycle 16 shutdown, the XPE model results were reviewed and evaluated against ultrasonic testing results. Although expected to be conservative, this evaluation proved encouraging in that the model performed more accurately than expected. Additionally, these data helped confirm the postulated release mechanism and its contribution to the XPE model.

  5. Isotope-coded, iodoacetamide-based reagent to determine individual cysteine pKa values by MALDI-TOF mass spectrometry

    PubMed Central

    Nelson, Kimberly J.; Day, Amanda E.; Zeng, Bubing B.; King, S. Bruce; Poole, Leslie B.

    2008-01-01

    Cysteine reactivity in enzymes is imparted to a large extent by the stabilization of the deprotonated form of the reduced cysteine (i.e. the thiolate) within the active site. While this is likely to be an important chemical attribute of many thiol-based enzymes including cysteine-dependent peroxidases (peroxiredoxins) and proteases, only relatively few pKa values have been determined experimentally. Presented here is a new technique for determining the pKa value of cysteine residues through quantitative mass spectrometry following chemical modification with an iodoacetamide-based reagent over a range of pH buffers. This isotope-coded reagent, N-phenyl iodoacetamide (iodoacetanilide), is readily prepared in deuterated (d5) and protiated (d0) versions and is more reactive toward free cysteine than is iodoacetamide. Using this approach, the pKa values for the two cysteine residues in Escherichia coli thioredoxin were determined to be 6.5 and > 10, in good agreement with previous reports using chemical modification approaches. This technique allows the pKa of specific cysteine residues to be determined in a clear, fast, and simple manner and, because cysteine residues on separate tryptic peptides are measured separately, is not complicated by the presence of multiple cysteines within the protein of interest. PMID:18162165

  6. Simultaneous photometric determination of albumin and total protein in animal blood plasma employing a multicommutated flow system to carried out on line dilution and reagents solutions handling

    NASA Astrophysics Data System (ADS)

    Luca, Gilmara C.; Reis, Boaventura F.

    2004-02-01

    An automatic flow procedure for the simultaneous determination of albumin and total protein in blood plasma samples is proposed. The flow network comprised a set of three-way solenoid valves assembled to implement the multicommutation. The flow set up was controlled by means of a computer equipped with an electronic interface card which running a software wrote in QUICKBASIC 4.5 performed on line programmed dilution to allow the determination of both albumin and total protein in blood plasma. The photometric methods based on Bromocresol Green and Biuret reagents were selected for determination of albumin and total protein, respectively. Two LEDs based photometers coupled together the flow cells were employed as detector. After the adjustment of the operational parameters the proposed system presented the following features: an analytical throughput of 45 sample processing per hour for two analytes; relative standard deviations of 1.5 and 0.8% ( n=10) for a typical sample presenting 34 g l -1 albumin and 90 g l -1 total protein, respectively; linear responses ranging from 0 to 15 g l -1 albumin ( r=0.998) and total protein ( r=0.999); sample and reagents consumption, 140 μl serum solution, 0.015 mg VBC and 0.432 mg CuSO 4 per determination, respectively. Applying the paired t-test between results obtained using the proposed system and reference methods no significant difference at 95 and 90% confidence level for albumin and total protein, respectively, were observed.

  7. Inter-laboratory comparison measurements of radiochemical laboratories in Slovakia.

    PubMed

    Meresová, J; Belanová, A; Vrsková, M

    2010-01-01

    The first inter-laboratory comparison organized by the radiochemistry laboratory of Water Research Institute (WRI) in Bratislava was carried out in 1993 and since then is it realized on an annual basis and about 10 radiochemical laboratories from all over Slovakia are participating. The gross alpha and gross beta activities, and the activity concentrations of (222)Rn, tritium, and (226)Ra, and U(nat) concentration in synthetic water samples are compared. The distributed samples are covering the concentration range prevailing in potable and surface waters and are prepared by dilution of certified reference materials. Over the course of the years 1993-2008, we observed the improvement in the quality of results for most of the laboratories. However, the success rate of the gross alpha determination activity is not improving as much as the other parameters.

  8. Development of robotic plasma radiochemical assays for positron emission tomography

    SciTech Connect

    Alexoff, D.L.; Shea, C.; Fowler, J.S.; Gatley, S.J.; Schlyer, D.J.

    1995-12-01

    A commercial laboratory robot system (Zymate PyTechnology II Laboratory Automation System; Zymark Corporation, Hopkinton, MA) was interfaced to standard and custom laboratory equipment and programmed to perform rapid radiochemical analyses for quantitative PET studies. A Zymark XP robot arm was used to carry out the determination of unchanged (parent) radiotracer in plasma using only solid phase extraction methods. Robotic throughput for the assay of parent radiotracer in plasma is 4--6 samples/hour depending on the radiotracer. Robotic assays of parent compound in plasma were validated for the radiotracers [{sup 11}C]Benztropine, [{sup 11}C]cocaine, [{sup 11}C]clorgyline, [{sup 11}C]deprenyl, [{sup 11}C]methadone, [{sup 11}C]methylphenidate, [{sup 11}C]raclorpride, and [{sup 11}C]SR46349B. A simple robot-assisted methods development strategy has been implemented to facilitate the automation of plasma assays of new radiotracers.

  9. Ethyl propiolate as a post-column derivatization reagent for thiols: development of a green liquid chromatographic method for the determination of glutathione in vegetables.

    PubMed

    Zacharis, Constantinos K; Tzanavaras, Paraskevas D; Zotou, Anastasia

    2011-03-25

    The present study reports the development, validation and application of a new green liquid chromatographic method for the determination of glutathione (GSH) in vegetable samples. In this work we introduce-for the first time-ethyl propiolate (EP) as an advantageous post-column derivatization reagent for thiolic compounds. GSH (t(R)=6.60 min) and N-acetylcysteine (NAC, internal standard) (t(R)=11.80 min) were separated efficiently from matrix endogenous compounds by using a 100% aqueous mobile phase (0.1%, v/v CH(3)COOH in 1 mmol L(-1) EDTA, Q(V)=0.5 mL min(-1)) and a Prevail(®) reversed phase column that offers the advantage of stable packing material in aqueous mobile phases. The parameters of the post-column reaction (pH, amount concentration of the reagent, flow rates, length of the reaction coil and temperature) were studied. The linear determination range for GSH was 1-200 μmol L(-1) and the LOD was 0.1 μmol L(-1) (S/N=3). Total endogenous GSH was determined in broccoli, potato, asparagus and Brussels sprouts using the standards addition approach. The accuracy was evaluated by both recovery experiments (R=91-110%) and comparison to an o-phthalaldehyde/glycine corroborative post-column derivatization fluorimetric method. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Radiochemical Analysis Methodology for uranium Depletion Measurements

    SciTech Connect

    Scatena-Wachel DE

    2007-01-09

    This report provides sufficient material for a test sponsor with little or no radiochemistry background to understand and follow physics irradiation test program execution. Most irradiation test programs employ similar techniques and the general details provided here can be applied to the analysis of other irradiated sample types. Aspects of program management directly affecting analysis quality are also provided. This report is not an in-depth treatise on the vast field of radiochemical analysis techniques and related topics such as quality control. Instrumental technology is a very fast growing field and dramatic improvements are made each year, thus the instrumentation described in this report is no longer cutting edge technology. Much of the background material is still applicable and useful for the analysis of older experiments and also for subcontractors who still retain the older instrumentation.

  11. Experimental and analysis methods in radiochemical experiments

    NASA Astrophysics Data System (ADS)

    Cattadori, C. M.; Pandola, L.

    2016-04-01

    Radiochemical experiments made the history of neutrino physics by achieving the first observation of solar neutrinos (Cl experiment) and the first detection of the fundamental pp solar neutrinos component (Ga experiments). They measured along decades the integral νe charged current interaction rate in the exposed target. The basic operation principle is the chemical separation of the few atoms of the new chemical species produced by the neutrino interactions from the rest of the target, and their individual counting in a low-background counter. The smallness of the expected interaction rate (1 event per day in a ˜ 100 ton target) poses severe experimental challenges on the chemical and on the counting procedures. The main aspects related to the analysis techniques employed in solar neutrino experiments are reviewed and described, with a special focus given to the event selection and the statistical data treatment.

  12. Derivatization following hollow-fiber microextraction with tetramethylammonium acetate as a dual-function reagent for the determination of benzoic acid and sorbic acid by GC.

    PubMed

    Sun, Yang; Wang, Xiaoqing; Huang, Yilei; Pan, Zaifa; Wang, Lili

    2013-07-01

    Derivatization at the injection port following hollow-fiber-based liquid-liquid-liquid microextraction with tetramethylammonium acetate as a dual-function reagent, i.e. an acceptor and derivatization reagent, for the determination of benzoic acid (BA) and sorbic acid (SA) in real samples by GC was developed. BA and SA were extracted from aqueous samples to an organic phase impregnated into the pores of the hollow fiber wall, and then back-extracted to the acceptor solution located inside the lumen of the hollow fiber. Upon injection, the extracted analytes were quantitatively derivatized to their methyl esters with tetramethylammonium acetate in the GC injection port. Several parameters related to the derivatization and extraction efficiency were optimized. The linearity was satisfactory over a concentration range of 0.1-50 mg/L with r > 0.993 for both analytes. The LODs were 2.0 μg/L for SA and 20 μg/L for BA. The recoveries (83-116%) and precisions (RSDs of 1.2-11.4% (n = 3)) were examined by analyzing real spiked samples. The enrichment factors of BA and SA were 300 and 425. The results demonstrated that this is a simple, rapid, accurate, and sensitive method for the determination of BA and SA in various samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Spectrophotometric studies of reactions between pseudo-ephedrine with different inorganic and organic reagents and its micro-determination in pure and in pharmaceutical preparations.

    PubMed

    Zayed, M A; El-Rasheedy, El-Gazy A

    2012-03-01

    Two simple, sensitive, cheep and reliable spectrophotometric methods are suggested for micro-determination of pseudoephedrine in its pure form and in pharmaceutical preparation (Sinofree Tablets). The first one depends on the drug reaction with inorganic sensitive reagent like molybdate anion in aqueous media via formation of ion-pair mechanism. The second one depends on the drug reaction with π-acceptor reagent like DDQ in non-aqueous media via formation of charge transfer complex. These reactions were studied under various conditions and the optimum parameters were selected. Under proper conditions the suggested procedures were successfully applied for micro-determination of pseudoephedrine in pure and in Sinofree Tablets without interference from excepients. The values of SD, RSD, recovery %, LOD, LOQ and Sandell sensitivity refer to the high accuracy and precession of the applied procedures. The results obtained were compared with the data obtained by an official method, referring to confidence and agreement with DDQ procedure results; but it referred to the more accuracy of the molybdate data. Therefore, the suggested procedures are now successfully being applied in routine analysis of this drug in its pharmaceutical formulation (Sinofree) in Saudi Arabian Pharmaceutical Company (SPIMACO) in Boridah El-Qaseem, Saudi Arabia instead of imported kits had been previously used.

  14. Spectrophotometric studies of reactions between pseudo-ephedrine with different inorganic and organic reagents and its micro-determination in pure and in pharmaceutical preparations

    NASA Astrophysics Data System (ADS)

    Zayed, M. A.; El-Rasheedy, El-Gazy A.

    2012-03-01

    Two simple, sensitive, cheep and reliable spectrophotometric methods are suggested for micro-determination of pseudoephedrine in its pure form and in pharmaceutical preparation (Sinofree Tablets). The first one depends on the drug reaction with inorganic sensitive reagent like molybdate anion in aqueous media via formation of ion-pair mechanism. The second one depends on the drug reaction with π-acceptor reagent like DDQ in non-aqueous media via formation of charge transfer complex. These reactions were studied under various conditions and the optimum parameters were selected. Under proper conditions the suggested procedures were successfully applied for micro-determination of pseudoephedrine in pure and in Sinofree Tablets without interference from excepients. The values of SD, RSD, recovery %, LOD, LOQ and Sandell sensitivity refer to the high accuracy and precession of the applied procedures. The results obtained were compared with the data obtained by an official method, referring to confidence and agreement with DDQ procedure results; but it referred to the more accuracy of the molybdate data. Therefore, the suggested procedures are now successfully being applied in routine analysis of this drug in its pharmaceutical formulation (Sinofree) in Saudi Arabian Pharmaceutical Company (SPIMACO) in Boridah El-Qaseem, Saudi Arabia instead of imported kits had been previously used.

  15. Spectrophotometric Determination of Distigmine Bromide, Cyclopentolate HCl, Diaveridine HCl and Tetrahydrozoline HCl via Charge Transfer Complex Formation with TCNQ and TCNE Reagents

    PubMed Central

    Mohamed, Gehad Genidy; Rizk, Mahmoud Sabry; Zaky Frag, Eman Yousry

    2015-01-01

    The purpose of this investigation was directed to propose sensitive, accurate and reproducible methods of analysis that can be applied to determine distigmine bromide (DTB), cyclopentolate hydrochloride (CPHC), diaveridine hydrochloride (DVHC) and tetrahydrozoline hydrochloride (THHC) drugs in pure form and pharmaceutical preparations via charge-transfer complex formation with 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE) reagents. Spectrophotometric method involve the addition a known excess of TCNQ or TCNE reagents to DTB, CPHC, DVHC and THHC drugs in acetonitrile, followed by the measurement of the absorbance of the CT complexes at the selected wavelength. The reaction stoichiometry is found to be 1:1 [drug]: [TCNQ or TCNE]. The absorbance is found to increase linearly with concentration of the drugs under investigation which is corroborated by the correlation coefficients of 0.9954-0.9981. The system obeys Beer’s law for 6-400, 20-500, 1-180 and 60-560 µg mL-1 and 80-600, 10-300, 1-60 and 80-640 µg mL-1 for DTB, CPHC, DVHC and THHC drugs using TCNQ and TCNE reagents, respectively. The apparent molar absorptivity, sandell sensitivity, the limits of detection and quantification are also reported for the spectrophotometric method. Intra- and inter-day precision and accuracy of the method were evaluated as per ICH guidelines. The method was successfully applied to the assay of DTB, CPHC, DVHC and THHC drugs in formulations and the results were compared with those of a reference method by applying Student’s t and F-tests. No interference was observed from common pharmaceutical excipients. PMID:26330858

  16. A quantitative method for determination of Co(II) based on the inner filter effect of reagents on the Raman scattering signals of water.

    PubMed

    Wang, Hui Ying; Huang, Cheng Zhi

    2007-03-21

    It is known that Raman scattering signals are one of main interference sources leading up to determination errors in spectrofluorometry, and thus the signals can be easily detected with a common spectrofluorometer. In this contribution, we propose a quantitative method based on the inner filter effect (IFE) of reagents on the Raman scattering signals of solvent by taking the complexation of divalent cobalt ion with 4-[(5-chloro-2-pyridyl)azo]-1,3-diaminobenzene (5-Cl-PADAB) as a model system. By adjusting the excitation wavelength of the spectrofluorometer, we could easily detect the Raman scattering signals of water at 424 nm where the maximum absorption of 5-Cl-PADAB reagent is located. In a solution of 5-Cl-PADAB, the Raman scattering signals of water are decreased owing to the IFE of 5-Cl-PADAB. If Co(II), which could form the binary complex of Co(II)/5-Cl-PADAB and consumes the 5-Cl-PADAB reagent, is present in such a case for a given amount of 5-Cl-PADAB solution, recovered Raman scattering signals could be observed and measured with a spectrofluorometer. It was found that the intensity of the enhanced Raman scattering signals is proportional to the Co(II) concentration over the range from 2.0 x 10(-7) mol L(-1) to 1.0 x 10(-5) mol L(-1), and the detection limit could reach 1.2 x 10(-7) mol L(-1). With that, Co(II) in samples could be detected with R.S.D. values lower than 2.6% and recoveries over the range of 97.2-104.7%.

  17. Flow-injection spectrophotometric determination of bromate in bottled drinking water samples using chlorpromazine reagent and a liquid waveguide capillary cell.

    PubMed

    Tóth, Ildikó V; Santos, Inês C; Azevedo, Cláudia F M; Fernandes, Jorge F S; Páscoa, Ricardo N M J; Mesquita, Raquel B R; Rangel, António O S S

    2013-01-01

    In this work, aiming to develop a simple, inexpensive method for the determination of low bromate levels in water samples, a liquid waveguide capillary cell (LWCC) was coupled to a FIA system. The long optical path (100 cm) of the LWCC was used to improve the sensitivity and the limit of detection without resorting to any off-line or in-line preconcentration processes. The spectrophotometric determination was based on the oxidation of chlorpromazine by bromate in an acidic medium, resulting in the formation of a colored radical product. Sulfamic acid was added to the reagent for minimizing the interference of nitrite, and a chelating ion exchange resin was used to remove major cationic interferences. The developed system allowed the determination of bromate within the range between 1 - 20 μg L(-1) with a detection limit of 0.2 μg L(-1).

  18. Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Al Okab, Riyad Ahmed

    2013-02-01

    Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml-1 and molar absorptivity 1.41 × 104 L mol-1 cm-1. All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

  19. Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods.

    PubMed

    Al Okab, Riyad Ahmed

    2013-02-15

    Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml(-1) and molar absorptivity 1.41 × 10(4) L mol(-1)cm(-1). All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

  20. A sensitive colorimetric method for the determination of nitrite in water supplies, meat and dairy products using ionic liquid-modified methyl red as a colour reagent.

    PubMed

    Zhang, Haijuan; Qi, Shengda; Dong, Yalei; Chen, Xiaojiao; Xu, Yinyin; Ma, Yanhua; Chen, Xingguo

    2014-05-15

    This paper describes a colorimetric approach to determine trace amounts of nitrite in water supplies, meat and dairy products using 1-butyl-3-methylimidazolium-modified methyl red ([BMIM]MR) as a colour reagent. The technique capitalises on the catalytic effect of nitrite on the oxidative degradation of [BMIM]MR by potassium bromate in acidic media. The absorbances were proportional to nitrite concentrations in the range of 8.70×10(-2) to 4.17 μM with a detection limit of 1.64×10(-2) μM. Compared with the method using methyl red as a colour reagent, 60 times improvement of sensitivity was obtained. Activation energy and the apparent rate constant for the catalytic reaction are 61.11 kJ mol(-1) and 1.18×10(4) s(-1), respectively. The proposed method was successfully applied for the analysis of nitrite in Yellow River water, chicken, and milk with recoveries ranging from 96% to 105%. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. High performance liquid chromatographic determination of copper(II) and nickel(II) by using solvent extraction and bis(acetylpivalylmethane)ethylenediimine as complexing reagent.

    PubMed

    Khuhawar, M Y; Soomro, A I

    1992-06-01

    The reagent bis(acetylpivalylmethane)ethylenediimine has been examined for the HPLC separation of copper(II), nickel(II), palladium(II) and oxovanadium(IV) chelates on reversed phase HPLC columns (250 x 4 mm) packed with Hypersil ODS, 5 mu and (150 x 3.9 mm) Nova Pak C(18) with guard column. The complexes are eluted with a binary mixture of methanol and water or methanol, acetonitrile and water. Detection is achieved with a UV detector. The solvent extraction procedure is used for the determination of copper and nickel simultaneously at microgram levels, corresponding to ng levels and pg levels respectively, per injection. The method has been applied to the determination of copper and nickel in a coin, nickel-aluminum alloy and water samples.

  2. Spectrophotometric determination of zirconium with 2-(1-hydroxy-4,6-dinitro-2-phenylazo)-1,8-dihydroxynaphthalene-3,6-disulphonate (picramine ca) as chromogenic reagent.

    PubMed

    Goyal, S S; Tandon, J P

    1968-09-01

    The title compound has been used as a selective reagent for the micro-determination of zirconium in acidic medium (0.5MHCl) and found to be better than Picramine R. Spectrophotometric studies show the formation of a 2:1 (ligand:Zr) water-soluble complex and the reaction is suitable for photometric determination of 0.4-2.8 ppm of zirconium. The colour takes about 90 min to develop fully and is stable for about 20 hr. The molar absorptivity of the complex is 2.4 x 10(4) and the equilibrium constant is of the order of 10(10). The interference due to a number of ions has been studied.

  3. Handling Pyrophoric Reagents

    SciTech Connect

    Alnajjar, Mikhail S.; Haynie, Todd O.

    2009-08-14

    Pyrophoric reagents are extremely hazardous. Special handling techniques are required to prevent contact with air and the resulting fire. This document provides several methods for working with pyrophoric reagents outside of an inert atmosphere.

  4. An improved radiochemical separation of uranium and thorium in environmental samples involving peroxide fusion.

    PubMed

    Galindo, C; Mougin, L; Nourreddine, A

    2007-01-01

    A radiochemical procedure for the accurate determination of uranium and thorium using peroxide fusion followed by ion exchange and extraction chromatography is described. The method of extraction of the element from solid samples is the most important factor in the investigation. It is demonstrated, by measuring a number of reference materials, that fusion with Na(2)O(2) ensures a complete destruction of the mineral lattice and greatly improves the determination of the true activity of actinides.

  5. Safety and Waste Management for SAM Radiochemical Methods

    EPA Pesticide Factsheets

    The General Safety and Waste Management page offers section-specific safety and waste management details for the radiochemical analytes included in EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM).

  6. Characterization of a titanium(IV)-porphyrin complex as a highly sensitive and selective reagent for the determination of hydrogen peroxide: a computational chemistry approach and a critical review.

    PubMed

    Takamura, Kiyoko; Matsumoto, Takatoshi

    2008-06-01

    The Ti-TPyP reagent, i.e. an acidic aqueous solution of the oxo[5,10,15,20-tetra(4-pyridyl)porphyrinato] titanium(IV) complex, TiO(tpyp), was developed as a highly sensitive and selective spectrophotometric reagent for determination of traces of hydrogen peroxide. Using this reagent, determination of hydrogen peroxide was performed by flow-injection analysis with a detection limit of 0.5 pmol per test. The method was actually applied to determination of several constituents of foods, human blood, and urine mediated by appropriate oxidase enzymes. The reaction specificity of the TiO(tpyp) complex for hydrogen peroxide was clarified from the viewpoint of the reaction mechanisms and molecular orbitals based on ab initio calculations. The results provided a well-grounded argument for determination of hydrogen peroxide using the Ti-TPyP reagent experimentally. This review deals with characterization of the high sensitivity and reaction specificity of the Ti-TPyP reagent for determination of hydrogen peroxide, to prove its reliability in analytical applications.

  7. 1,4-Anthraquinone: A new useful pre-column reagent for the determination of N-acetylcysteine and captopril in pharmaceuticals by high performance liquid chromatography.

    PubMed

    Gatti, Rita; Morigi, Rita

    2017-09-05

    1,4-Anthraquinone (ANQ) is proposed as a novel pre-column reagent for high performance liquid chromatography (HPLC) determination of N-acetylcysteine (NAC) and captopril (CAP) in pharmaceutical formulations. The derivatization reactions were carried out at room temperature: NAC at pH 8 for 1min, while CAP at pH 7.5 for 20min. Both reactions reached completeness at a reagent to thiol molar ratio of about 2.5. The synthesised derivatives were characterized by (1)H NMR and IR. The chromatographic separations were performed on a C18 Phenomenex Synergi Fusion 4μm (250mm×4.6mm I.D.) stainless steel column with detection at λ=300nm. The mobile phase consisted of methanol/triethylammonium (TEA) phosphate buffer (pH 3; 0.05mol/L) 75:25 (v/v) at a flow-rate of 0.4mL/min for NAC and 88:12 (v/v), at a flow-rate of 0.6mL/min for CAP. The validation parameters (linearity, sensitivity, accuracy, precision, specificity and stability) were highly satisfactory. Linear response was observed (determination coefficient ≥0.9996). Detection limits were about 8 and 18ng/mL for NAC and CAP, respectively. Intra-day precision (relative standard deviation, R.S.D.) was ≤1.58%, for thiol to internal standard (IS) peak area ratio and ≤0.33%, for thiol and IS retention times (tR), without significant differences between intra- and inter-day data. Thiol recovery studies were satisfactory (99.50%) with R.S.D. ≤0.56%. The results highlight the high sensitivity of the method and the remarkable reactivity and selectivity of the reagent towards the thiol function. The developed method is suitable for the quality control of both thiols in commercial products. The method can be applied in any analytical laboratory not requiring a sophisticated instrumentation. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Determination of nucleosides and nucleotides in baby foods by hydrophilic interaction chromatography coupled to tandem mass spectrometry in the presence of hydrophilic ion-pairing reagents.

    PubMed

    Mateos-Vivas, María; Rodríguez-Gonzalo, Encarnación; Domínguez-Álvarez, Javier; García-Gómez, Diego; Carabias-Martínez, Rita

    2016-11-15

    In this work we propose a rapid and efficient method for the joint determination of nucleosides and nucleotides in dairy and non-dairy baby foods based on hydrophilic interaction chromatography coupled to tandem mass spectrometry in the presence of diethylammonium (DEA) as a hydrophilic ion-pairing reagent (IP-HILIC-MS/MS). Sample treatment of the baby food included dilution with water and centrifugal ultrafiltration (CUF) with an additional washing step that notably improved the global performance of the process. Later dilution of the extract with acetonitrile allowed adequate separation in the HILIC system. With the proposed treatment, we obtained extraction recoveries higher than 80% and, additionally, no matrix effects were observed. The CUF-IP-HILIC-MS/MS method was validated according to the 2002/657/EC decision and was used for the quantification of nucleotides and nucleosides in sixteen samples of commercial baby foods.

  9. Determination of cysteine, homocysteine, cystine, and homocystine in biological fluids by HPLC using fluorosurfactant-capped gold nanoparticles as postcolumn colorimetric reagents.

    PubMed

    Zhang, Lijuan; Lu, Biqi; Lu, Chao; Lin, Jin-Ming

    2014-01-01

    We have demonstrated for the first time the suitability of fluorosurfactant-capped spherical gold nanoparticles as HPLC postcolumn colorimetric reagents for the direct assay of cysteine, homocysteine, cystine, and homocystine. The success of this work was based on the use of an on-line tris(2-carboxyethyl)phosphine reduction column for cystine and homocystine. Several parameters affecting the separation efficiency and the postcolumn colorimetric detection were thoroughly investigated. Under the optimized conditions, cysteine, homocysteine, cystine, and homocystine in human urine and plasma samples were determined. Detection limits for cysteine, homocysteine, cystine, and homocystine ranged from 0.16-0.49 μM. The accuracy in terms of recoveries ranged between 94.0-102.1%. This proposed method was rapid, inexpensive, and simple.

  10. Development of novel detection reagent for simple and sensitive determination of trace amounts of formaldehyde and its application to flow injection spectrophotometric analysis.

    PubMed

    Li, Qiong; Sritharathikhum, Piyanete; Oshima, Mitsuko; Motomizu, Shoji

    2008-04-07

    In this paper, a novel detection reagent for formaldehyde determination is proposed, and is applied to a simple and highly sensitive flow injection method for the spectrophotometric determination of formaldehyde. The method is based on the reaction of formaldehyde with methyl acetoacetate in the presence of ammonia. The increase in the absorbance of the reaction product was measured at 375 nm. An inexpensive light emitting diode (LED)-based UV detector (375 nm) was, for the first time, used. Under the optimized experimental conditions, formaldehyde in an aqueous solution was determined over the concentration range from 0.25 to 20.0 x 10(-6)M with a liner calibration graph; the limit of detection (LOD) of 5 x 10(-8)M (1.5 microgL(-1)) was possible. The relative standard deviation of 12 replicate measurements of 5 x 10(-6)M formaldehyde was 1.2%. Maximum sampling throughput was about 21 samples/h. The effect of potential interferences such as metals, organic compounds and other aldehyde was also examined. The analytical performance for formaldehyde determination was compared with those obtained by the conventional acetylacetone method, which uses visible absorption spectrophotometry. Finally, the proposed method was successfully applied to the determination of formaldehyde in natural water samples.

  11. Statistical analysis of radiochemical measurements of TRU radionuclides in REDC waste

    SciTech Connect

    Beauchamp, J.; Downing, D.; Chapman, J.; Fedorov, V.; Nguyen, L.; Parks, C.; Schultz, F.; Yong, L.

    1996-10-01

    This report summarizes results of the study on the isotopic ratios of transuranium elements in waste from the Radiochemical Engineering Development Center actinide-processing streams. The knowledge of the isotopic ratios when combined with results of nondestructive assays, in particular with results of Active-Passive Neutron Examination Assay and Gamma Active Segmented Passive Assay, may lead to significant increase in precision of the determination of TRU elements contained in ORNL generated waste streams.

  12. Simultaneous determination of amino acid and monoamine neurotransmitters in PC12 cells and rats models of Parkinson's disease using a sensitizing derivatization reagent by UHPLC-MS/MS.

    PubMed

    Zhao, Xian-En; Zhu, Shuyun; Yang, Hongmei; You, Jinmao; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

    2015-07-15

    Multi-analytes simultaneous monitoring of amino acid and monoamine neurotransmitters (NTs) has important scientific significance for their related pathology, physiology and drug screening. In this work, in virtue of a mass spectrometry sensitizing reagent 10-ethyl-acridone-3-sulfonyl chloride (EASC) as derivatization reagent, an Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS) method was developed and validated for simultaneous determination of six amino acid NTs, two monoamine ones and its one metabolite. The simple and rapid derivatization reaction was innovatively combined with plasma preparation by using EASC acetonitrile solution as protein precipitant. This interesting combination brought the advantages of speediness, simpleness and high-throughput in a cost-effective way. Under the optimized conditions, LODs (0.004-3.80nM) and LOQs (0.014-13.3nM) of EASC derivatized-NTs were calculated and found to be significantly lower than those of direct UHPLC-MS/MS detection about 11.5-275.0 and 14.4-371.4 times, respectively. Moreover, EASC derivatization significantly improved chromatographic resolution and matrix effect when compared with direct UPLC-MS/MS detection method without derivatization. Meanwhile, it also brought acceptable precision (3.0-13.0%, peak area CVs%), accuracy (86.4-112.9%), recovery (88.3-107.8%) and stability (3.8-8.5%, peak area CVs%) results. This method was successfully applied for the antiparkinsonian effect evaluation of levodopa and Ginsenoside Rg1 using PC12 cells and rats models by measuring multiple NTs. This provided a new method for the NTs related studies in the future.

  13. Development and validation of a simple and sensitive HPLC-UV method for the determination of captopril in human plasma using a new derivatizing reagent 2-naphthyl propiolate.

    PubMed

    Rastkari, Noushin; Khoobi, Mehdi; Shafiee, Abbas; Khoshayand, Mohammad Reza; Ahmadkhaniha, Reza

    2013-08-01

    In this study, a simple, sensitive and reliable HPLC-UV method applying rapid sample preparation technique for the determination of captopril in human plasma was developed and validated. The method is based on pre-column derivatization of captopril and 2-propene-1-thiol (internal standard) with a new reagent 2-naphthyl propiolate. Sample clean-up, derivatization and extraction were carried out in two steps, totally less than 30min. The extracts were chromatographed on a C18 column (5μm, 150mm×4.6mmi.d.). The mobile phase consisted of methanol (75%, v/v) and phosphate buffer (25%, pH=8, 0.01M). UV detection was performed at 290nm. To obtain the best reaction yield, the factors that could influence the derivatization process, including the concentration of derivatization reagent, pH of sample solution and temperature were investigated in detail and optimized using Box-Behnken response surface methodology. Under optimized conditions the average extraction recovery of captopril and internal standard were >86%. The achieved lower limit of quantification (LLOQ) was 3ng/mL; the assay exhibited a linear dynamic range of 3-2000ng/mL with correlation coefficient (r(2)) of ≥0.99. The precision was satisfactory in the whole calibration range with RSD of 5.9-12.4% (accuracy: from 97.5% to 93.6%) and of 6.4-12.8% (accuracy: from 97.3% to 95.2%) for intra- and inter-assay, respectively. The method stability was confirmed in a series of experiments including: freeze-thaw, short- and long-term stability testing. Lastly, the developed method was successfully applied to the bioequivalence study of captopril administrated as a single oral dose (50mg) to 12 healthy male volunteers. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Determination of epichlorohydrin and 1,3-dichloro-2-propanol in synthesis of cationic etherifying reagent by headspace gas chromatography.

    PubMed

    Tao, Zheng-Yi; Chai, Xin-Sheng; Wu, Shu-Bin

    2011-09-16

    This study demonstrates a headspace gas chromatographic(HS-GC) technique for the determination of residual epichlorohydrin (ECH) and generated 1,3-dichloro-2-propanol (DCP) in synthesis process of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHTAC). By a weight-based sampling method, coupled with significant dilution in 15.8% sodium sulfate and 0.1% silver nitrate mixed solution rapidly, the sample for HS-GC analysis is prepared. Based on the reaction stoichiometry, the conversion (R) of CHTAC during the synthesis process can be calculated from sampling weight and GC peak area. The results showed that the method has a good measurement precision (RSD<2.5%) and accuracy (recovery=101-104%) for the quantification of both ECH and DCP in the process samples. The present method is simple and accurate, which can be used for the efficient determination of the CHTAC conversion in the synthesis research.

  15. One-Shot, reagent-free determination of the alcoholic content of distilled beverages by thermal infrared enthalpimetry.

    PubMed

    Oliveira, Alessandra S; Nora, Flávia M Dalla; Mello, Renius O; Mello, Paola A; Tischer, Bruna; Costa, Adilson B; Barin, Juliano S

    2017-08-15

    A simple and fast method is proposed for determining the alcoholic content of distilled beverages by thermal infrared enthalpimetry (TIE), in which purified water is added directly and the temperature rise caused by the heat of dilution is monitored using an infrared camera. A calibration curve was constructed with hydroalcoholic reference solutions to determine the alcoholic content of vodka, whisky, and cachaça. The influence of the total volume of solutions in the reactor, the stirring speed, the dispensing rate, and the ratio between hydroalcoholic samples and water were evaluated to reach an optimum mixture and provide low variation among measurements. Optimized conditions for those respective parameters were 2.4mL, 200rpm, 0.57mLs(-1), and 1:1. To evaluate the accuracy, alcoholic content was also determined by a conventional method (AOAC method 942.06, pycnometry), with agreement ranging from 99.4% to 100.9%. No sample preparation (e.g., dilution or distillation) was required with the proposed method, decreasing the time required for analysis by at least one order of magnitude. The proposed method required less energy consumption by a factor of about three thousand in comparison with the conventional method. The proposed TIE method was robust, able to determine the alcoholic content of diverse distilled beverages. Due to these features and the high sample throughput (up to 480 samples per hour), the proposed method could be considered suitable for routine analysis and agrees with the principles of green analytical chemistry. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Determination of ultra-trace formaldehyde in air using ammonium sulfate as derivatization reagent and capillary electrophoresis coupled with on-line electrochemiluminescence detection.

    PubMed

    Deng, Biyang; Liu, Yang; Yin, Huihui; Ning, Xi; Lu, Hua; Ye, Li; Xu, Quanxiu

    2012-03-15

    The reaction between formaldehyde and ammonium ion to produce hexamethylenetetramine is well known. The reaction conditions are very easily controlled in situ and the experiment operation is very simple. However, such derivatization reaction for trace formaldehyde determination using capillary electrophoresis (CE) electrochemiluminescence (ECL) has not been reported before. In this study, the application of ammoniun sulfate as derivatization reagent to in-situ determination of formaldehyde in air was reported. Based on ECL enhancement of tris(2,2'-bipyridyl)ruthenium(II) with hexamethylenetetramine, a novel approach for the determination of ultra-trace formaldehyde in air using CE coupled with on-line ECL of tris(2,2'-bipyridyl)ruthenium(II) has been developed. The parameters affecting separation and detection such as detection potential, concentration and pH of phosphate buffer, and electrokinetic voltage, were investigated. Under the optimal conditions, the linear concentration range of formaldehyde in air was from 0.48 μg/m(3) to 96 mg/m(3) (linear range covering 5 orders of magnitude). The limit of detection (3σ) was 0.15 μg/m(3). The relative standard deviations of peak height and migration time for six consecutive injection of 1 ng/mL formaldehyde derivative were 0.9% and 0.8%, respectively. The recoveries of formaldehyde in air were between 99.3% and 101%. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Separation and quantitative determination of cinacalcet metabolites in urine sample using RP-HPLC after derivation with a fluorescent labeling reagent.

    PubMed

    Farnoudian-Habibi, Amir; Jaymand, Mehdi

    2016-08-01

    In this investigation, a novel strategy for separation and quantitative determination of four metabolites of cinacalcet (M2a-Glu, M2b-Glu, M7-Gly, and M8-Gly) in human urine is suggested. The analytical assay is based on a pre-column derivation procedure of cinacalcet metabolites with 1-pyrenyldiazomethane (PDAM) as a fluorescent labeling reagent, and subsequently separation and quantitative determination with reverse-phase high-performance liquid chromatography (RP-HPLC) coupled with a fluorescence detector. Metabolites were separated on a Microsorb-MV 100-5 C18 chromatography column (250×4.6mm, 5μm) using acetate buffer (pH 3.5):methanol (30:70 v/v) as mobile phase at a flow rate of 1.0mLmin(-1). The method was fully validated in terms of linearity (r(2)>0.996; 1-10ngmL(-1)), precision (both intra-day and inter-day; RSD<6.2%), accuracy (92-110%), specificity, robustness (0.15%determination of cinacalcet metabolites in urine samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Spectrophotometric determination of dapsone in pharmaceutical products using sodium 1,2-naphthoquinone-4-sulfonic as the chromogenic reagent

    NASA Astrophysics Data System (ADS)

    Wang, Huai You; Xu, Li Xiao; Xiao, Yan; Han, Juan

    2004-10-01

    Spectrophotometric determination of dapsone is described. The dapsone reacts with sodium 1,2-naphthoquinone-4-sulfonic in pH 6.98 buffer solution to form a salmon pink compound, and its maximum absorption wavelength is at 525 nm, ɛ525=3.68×10 4 l mol -1 cm -1. The absorbance of dapsone from 0.40 to 10 μg ml -1 obeys Beer's law. The linear regression equation of the calibration graph is C=0.2334 A+0.01288, with a linear regression correlation coefficient of 0.9998, the detection limit is 0.24 μg ml -1, and recovery is from 99.2 to 102.4%. Effects of pH, surfactant, organic solvents, foreign ions, and standing time on the determination of dapsone have been examined. This method is simple and can be used for the determination of dapsone in injection solution of dapsone. The results obtained by this method agreed with those by the official method (dead-stop titration method [The Chinese Pharmacopoeia, Pharmacopoeia Commission, Ministry of Health, vol. 2, fifth ed., PRC Chemical Industry Press, Beijing, 2000, p.720]).

  19. Spectrophotometric determination of procaine hydrochloride in pharmaceutical products using 1,2-naphthoquinone-4-sulfonic acid as the chromogenic reagent

    NASA Astrophysics Data System (ADS)

    Xu, Li Xiao; Shen, Yun Xiu; Wang, Huai You; Jiang, Ji Gang; Xiao, Yan

    2003-11-01

    Spectrophotometric determination of procaine hydrochloride is described. The procaine hydrochloride reacts with 1,2-naphthoquinone-4-sulfonic acid in pH 3.60 buffer solution to form a salmon pink compound, and its maximum absorption wavelength is at 484 nm, ɛ 484=5.22×10 3.The absorbance for procaine hydrochloride from 0.30 to 100 μg ml -1 obeys Beer's law. The linear regression equation of the calibration graph is C=19.23A-0.03, with a linear regression correlative coefficient is 0.9996, the detection limit is 0.28 μg ml -1; recovery is from 98.0 to 105.2%. Effects of pH, surfactant, organic solvent, foreign ions, and standing time on the determination of procaine hydrochloride have been examined. This method is rapid and simple, and can be used for the determination of procaine hydrochloride in injection solution of procaine hydrochloride. The results obtained by this method agreed with those by the official method (dead-stop titration).

  20. Spectrophotometric determination of ampicillin sodium in pharmaceutical products using sodium 1,2-naphthoquinone-4-sulfonic as the chromogentic reagent

    NASA Astrophysics Data System (ADS)

    Xu, Lixiao; Wang, Huaiyou; Xiao, Yan

    2004-11-01

    Spectrophotometric determination of ampicillin sodium is described. The ampicillin sodium reacts with sodium 1,2-naphthoquinone-4-sulfonic in pH 9.00 buffer solution to form a salmon pink compound, and its maximum absorption wavelength is at 463 nm, ɛ463=1.14×10 4. The absorbance of ampicillin sodium from 2.0-80 μg ml -1 obeys Beer's law. The linear regression equation of the calibration graph is C=40.24 A-2.603, with a linear regression correlation coefficient is 0.9997, the detection limit is 1.5 μg ml -1, recovery is from 97.23 to 104.5%. Effects of pH, surfactant, organic solvents, and foreign ions on the determination of ampicillin sodium have been examined. This method is rapid and simple, and can be used for the determination of ampicillin sodium in the injection solution of ampicillin sodium. The results obtained by this method agreed with those by the official method (HPLC).

  1. Spectrophotometric determination of dapsone in pharmaceutical products using sodium 1,2-naphthoquinone-4-sulfonic as the chromogenic reagent.

    PubMed

    Wang, Huai You; Xu, Li Xiao; Xiao, Yan; Han, Juan

    2004-10-01

    Spectrophotometric determination of dapsone is described. The dapsone reacts with sodium 1,2-naphthoquinone-4-sulfonic in pH 6.98 buffer solution to form a salmon pink compound, and its maximum absorption wavelength is at 525 nm, epsilon525=3.68 x 10(4) l mol(-1) cm(-1). The absorbance of dapsone from 0.40 to 10 microg ml(-1) obeys Beer's law. The linear regression equation of the calibration graph is C=0.2334 A + 0.01288, with a linear regression correlation coefficient of 0.9998, the detection limit is 0.24 microg ml(-1), and recovery is from 99.2 to 102.4%. Effects of pH, surfactant, organic solvents, foreign ions, and standing time on the determination of dapsone have been examined. This method is simple and can be used for the determination of dapsone in injection solution of dapsone. The results obtained by this method agreed with those by the official method (dead-stop titration method [The Chinese Pharmacopoeia, Pharmacopoeia Commission, Ministry of Health, vol. 2, fifth ed., PRC Chemical Industry Press, Beijing, 2000, p.720]).

  2. Spectrophotometric determination of ampicillin sodium in pharmaceutical products using sodium 1,2-naphthoquinone-4-sulfonic as the chromogentic reagent.

    PubMed

    Xu, Lixiao; Wang, Huaiyou; Xiao, Yan

    2004-11-01

    Spectrophotometric determination of ampicillin sodium is described. The ampicillin sodium reacts with sodium 1,2-naphthoquinone-4-sulfonic in pH 9.00 buffer solution to form a salmon pink compound, and its maximum absorption wavelength is at 463 nm, epsilon463 = 1.14 x 10(4). The absorbance of ampicillin sodium from 2.0-80 microg ml(-1) obeys Beer's law. The linear regression equation of the calibration graph is C = 40.24A - 2.603, with a linear regression correlation coefficient is 0.9997, the detection limit is 1.5 microg ml(-1), recovery is from 97.23 to 104.5%. Effects of pH, surfactant, organic solvents, and foreign ions on the determination of ampicillin sodium have been examined. This method is rapid and simple, and can be used for the determination of ampicillin sodium in the injection solution of ampicillin sodium. The results obtained by this method agreed with those by the official method (HPLC).

  3. Miniaturization of spectrophotometry based on micro flow analysis using norfloxacin as less-toxic reagent for iron determination.

    PubMed

    Prasertboonyai, Kanyarak; Arqueropanyo, Orn-Anong; Liawraungrath, Boonsom; Liawraungrath, Saisunee; Pojanakaroon, Teraboon

    2015-01-01

    A micro flow analysis (μFA) system has been designed and fabricated for determination of total iron. The system consists of a microchannels fabricated by etching the polymethyl methacrylate (PMMA) by using laser ablation techniques and a sealed polydimethylsiloxane (PDMS) as top plate. The PMMA micro-flow was topped with a home-made polydimethylsiloxane (PDMS) micro-flow through cell, which was integrated with light emitting diode (LED) as light source and a USB 2000 spectrometer as detector. The proposed μFA system was applied to determination of Fe(III) using norfloxacin as a less-toxic complexing agent in an acetate buffer solution pH 4.0, resulting in a yellow colored complex which gave the maximum absorption at 430nm. Under the optimum conditions, a linear calibration graph was obtained in the concentration range of 0.20-5.00mgL(-1). The limit of detection (LOD, defined as 3σ) and limit of quantification (LOQ, defined as 10σ) were 0.12 and 0.45mgL(-1), respectively. The relative standard deviation (R.S.D.) for repeatability and reproducibility were less than 1.50% and 1.24% (n=11) for 0.2mgL(-1) and 1.0mgL(-1) Fe(III), respectively. The proposed method was successfully applied to the determination of total iron in water samples, validated by the FAAS standard method after digestion by HNO3 and H2O2.

  4. Trivalent manganese as an environmentally friendly oxidizing reagent for microwave- and ultrasound-assisted chemical oxygen demand determination.

    PubMed

    Domini, Claudia E; Vidal, Lorena; Canals, Antonio

    2009-06-01

    In the present work manganese(III) has been used as oxidant and microwave radiation and ultrasound energy have been assessed to speed up and to improve the efficiency of digestion step for the determination of chemical oxygen demand (COD). Microwave (MW) and ultrasound-assisted COD determination methods have been optimized by means of experimental design and the optimum conditions are: 40psi pressure, 855W power and 1min irradiation time; and 90% of maximum nominal power (180W), 0.9s (s(-1)) cycles and 1min irradiation time for microwaves and ultrasound, respectively. Chloride ion interference is removed as hydrochloric acid gas from acidified sample solutions at 150 degrees C in a closed reaction tube and captured by bismuth-based adsorbent suspended above the heated solution. Under optimum conditions, the evaluated assisted digestion methods have been successfully applied, with the exception of pyridine, to several pure organic compounds and two reference materials. COD recoveries obtained with MW and ultrasound-assisted digestion for five real wastewater samples were ranged between 86-97% and 68-91%, respectively, of the values obtained with the classical method (open reflux) used as reference, with relative standard deviation lower than 4% in most cases. Thus, the Mn(III) microwave-assisted digestion method seems to be an interesting and promising alternative to conventional COD digestion methods since it is faster and more environmentally friendly than the ones used for the same purpose.

  5. Chemiluminescence flow sensor with immobilized reagent for the determination of pyrogallol based on potassium hexacyanoferrate(III) oxidation

    NASA Astrophysics Data System (ADS)

    Chen, Jianchun; Bai, Jun

    2008-12-01

    A novel chemiluminescence (CL) flow-through sensor for the determination of pyrogallol has been developed. The method is based on the reaction between pyrogallol and potassium hexacyanoferrate(III) in sodium hydroxide solution. Potassium hexacyanoferrate(III) involved in the CL reaction was electrostatically immobilized on anion-exchange resin packed in a column. Pyrogallol was sensed by the CL reaction between pyrogallol and potassium hexacyanoferrate(III) which was eluted from the ion-exchange column through sodium phosphate injection. The CL emission allows quantitation of pyrogallol concentration in the range 0.01-3.8 μg/mL with a detection limit (3 σ) of 0.003 μg/mL and a sample throughput of 118 h -1. The relative standard deviation ( n = 7) was 2.2% for 0.2 μg/mL of pyrogallol. The influence of foreign compounds was tested.

  6. In-line electrochemical reagent generation coupled to a flow injection biamperometric system for the determination of sulfite in beverage samples.

    PubMed

    de Paula, Nattany T G; Barbosa, Elaine M O; da Silva, Paulo A B; de Souza, Gustavo C S; Nascimento, Valberes B; Lavorante, André F

    2016-07-15

    This work reports an in-line electrochemical reagent generation coupled to a flow injection biamperometric procedure for the determination of SO3(2-). The method was based on a redox reaction between the I3(-) and SO3(2-) ions, after the diffusion of SO2 through a gas diffusion chamber. Under optimum experimental conditions, a linear response ranging from 1.0 to 12.0 mg L(-1) (R=0.9999 and n=7), a detection and quantification limit estimated at 0.26 and 0.86 mg L(-1), respectively, a standard deviation relative of 0.4% (n=10) for a reference solution of 4.0 mg L(-1) SO3(2-) and sampling throughput for 40 determinations per hour were achieved. Addition and recovery tests with juice and wine samples were performed resulting in a range between 92% and 110%. There were no significant differences at a 95% confidence level in the analysis of eight samples when comparing the new method with a reference procedure.

  7. Spectrofluorometric determination and chemical speciation of trace concentrations of chromium (III & VI) species in water using the ion pairing reagent tetraphenyl-phosphonium bromide.

    PubMed

    El-Shahawi, M S; Al-Saidi, H M; Bashammakh, A S; Al-Sibaai, A A; Abdelfadeel, M A

    2011-03-15

    A highly selective, and low cost extractive spectrofluorometric method has been developed for determination of trace concentrations of chromium (III & VI) in water samples using the fluorescent reagent tetraphenylphosphonium bromide (TPP(+) · Br(-)). The method was based upon solvent extraction of the produced ion associate [TPP(+) · CrO(3)Cl(-)] of TPP(+) · Br(-) and halochromate in aqueous HCl and measuring the fluorescence quenching of TPP(+) · Br(-) in chloroform at λ(ex/em)=242/305 nm. The fluorescence intensity of TPP(+)Br(-) decreased linearly on increasing the chromium (VI) concentration in the range of 1-114 μg L(-1). The limits of detection (LOD) and quantification (LOQ) of chromium (VI) were 0.43 and 1.42 μg L(-1), respectively. Chromium (III) species after oxidation to chromium (VI) with H(2)O(2) in alkaline solution were also determined. Chemical speciation of chromium (III & VI) species at trace levels was achieved. The method was applied for analysis of chromium in certified reference material (IAEA Soil-7) and in tap- and wastewater samples and compared successfully (>95%) with the inductively coupled plasma-mass spectrometry (ICP-MS) results.

  8. Flow and sequential injection methods for the spectrofluorimetric determination of aluminium in pharmaceutical products using chromotropic acid as chromogenic reagent.

    PubMed

    Themelis, Demetrius G; Kika, Fotini S

    2006-06-16

    This work reports rapid and sensitive FI and SI spectrofluorimetric methods for the determination of aluminium in pharmaceutical formulations. The methods are based on the reaction of aluminium with chromotropic acid (CA) in acidic medium to form a water-soluble complex (lambdaex.=360 nm, lambdaem.=385 nm). The proposed methods were validated in terms of linearity, repeatability, detection limit, accuracy and selectivity. The calibration curves were linear over the range of 0.03-2.0 and 0.1-4.0mg/l of aluminium using the FI and SI assays, respectively. The repeatabilities (sr=0.8% and 1.1% at 1mg/l aluminium using the FI and the SI assay, respectively, n=12) were satisfactory. The FI and SI methods proved to be adequately selective and sensitive with respective 3sigma limits of detection equal to cL=0.01 and 0.03 mg/l Al(III). The sampling rates were 120 and 72 h(-1) with the FI and SI assay. The methods were applied successfully to the analysis of pharmaceutical formulations (tablets and suspensions). The results were in good agreement with those by an official reference method and the nominal values of the pharmaceutical products.

  9. Rapid and highly sensitive determination of trace proteins using dibromomethyl carboxyazo-Pb(II) complex as a spectroscopic reagent.

    PubMed

    Wei, Qin; Li, Yuan-Yuan; Li, Yan; Du, Bin; Duan, Cai-Hong

    2005-12-01

    The concentration of protein in body fluids is an important measure in disease diagnosis and in analytical biochemistry. Searching for a sensitive and rapid method for proteins is an ongoing subject of investigation. We describe the reaction of dibromomethyl carboxyazo-Pb(II) with proteins found in urine. In a buffer containing of HCl and KCl at pH 1.80, dibromomethyl carboxyazo-Pb(II) complex combined with proteins to form a colored compound. The reaction was completed in 2 min and remained stable for 80 min. Under optimum conditions, the product of reaction between protein and dibromomethyl carboxyazo-Pb(II) absorbed at 530 nm and was linear in the range of 0-50 microg/ml of BSA. Moreover, the maximum binding number was defined to express the binding ability of dibromomethyl carboxyazo-Pb(II) to protein under a given set of conditions. The method was applied to the determination of urine proteins. The recovery of protein from human urine was 97.6-103% and the precision was <4.8%. Results compared favorably to the Biuret and Bradford protein methods on 50 urine samples. This method had high sensitivity and specificity and may be applicable to clinical analysis.

  10. Determination of thiophenols with a novel fluorescence labelling reagent: analysis of industrial wastewater samples with SPE extraction coupled with HPLC.

    PubMed

    Sun, Yanan; Lv, Zhengxian; Sun, Zhiwei; Wu, Chuanxiang; Ji, Zhongyin; You, Jinmao

    2016-05-01

    A simple, sensitive, and selective high-performance liquid chromatography (HPLC) method using 9-(2-iodoethyl)acridone (IEA) as a novel fluorescence derivatizing agent for the simultaneous determination of six thiophenols has been developed. An efficient Pb(2+)-modified OASIS-MCX cartridge was used and could get good recoveries. IEA was successfully used to label thiophenols with high sensitivity and excellent selectivity. The effects of different solvents, pH, and surfactants on fluorescence properties of derivatives were investigated. To obtain the best labeling efficiency, derivatizing parameters including pH value, temperature, and concentration of IEA, as well as types of catalysts were also evaluated in detail. Under the optimal conditions, the separation could be achieved within 12 min with limits of detection (LODs) in the range of 0.6-5.8 μg L(-1) and relative standard deviations (RSDs) < 3.9%. This is the first time that IEA was applied to the analysis of thiophenols, and the established method has been successfully applied to the trace level detection of thiophenols in industrial wastewater samples.

  11. 3-((3-/sup 125/I)Iodo-4-hydroxyphenyl)propionyl Carbohydrazide, a new radioiodination reagent for ultrasensitive detection and determination of periodate-oxidized nucleoside derivatives

    SciTech Connect

    Randerath, K.

    1981-08-01

    A new radioiodination reagent for the identification and quantitation of periodate-oxidized ribonucleosides was developed. The reagent, 3-((3-/sup 125/I)iodo-4-hydroxyphenyl)propionyl carbohydrazide, was prepared by radioiodination of 3-(4-hydroxyphenyl)propionic acid N-hydroxysuccinimide ester in the presence of chloramine T, followed by reduction of the latter with sodium arsenite and treatment of the radioiodinated ester with an excess of carbohydrazide. The reagent reacted quantitatively with periodate-oxidized nucleosides to form /sup 125/I-labeled morpholine derivatives which were separated by thin-layer chromatography and quantitated by liquid scintillation counting. The reagent was found to react also with other carbonyl compounds and thus may find more general application in the qualitative and quantitative ultramicroanalysis of aldehydes and ketones.

  12. Perchlorate in water via US Environmental Protection Agency Method 331 Determination of method uncertainties, lowest concentration minimum reporting levels, and Hubaux-Vos detection limits in reagent water and simulated drinking water.

    PubMed

    Wendelken, S C; Vanatta, L E; Coleman, D E; Munch, D J

    2006-06-16

    US Environmental Protection Agency (EPA) Method 331 determines perchlorate in drinking water using non-suppressed ion chromatography with tandem mass spectrometry. This study reports the results of calibration and recovery studies in reagent water, as well as of a recovery study in simulated drinking water (i.e., total dissolved solids are 500 mg/mL each of chloride, sulfate, and bicarbonate). The perchlorate concentrations in the study ranged from 0.05 to 64 ng/mL. At 95% confidence, the Hubaux-Vos detection limit (H-V DL) was 0.04 ng/mL for the calibration study and the simulated-drinking-water recovery study, and 0.03 ng/mL for the reagent-water recovery study. The lowest concentration minimum reporting level was 0.03 ng/mL for reagent water and 0.0 7 ng/mL for simulated drinking water, again at 95% confidence.

  13. RESEARCH NOTE: INTERFERENCES DUE TO OZONE-SCAVENGING REAGENTS IN THE GC-ECD DETERMINATION OF ALDEHYDES AND KETONS AS THE O-(2,3,4,5,6-PENTAFLUOROBENZYL)OXIMES

    EPA Science Inventory

    Six potential ozone-scavenging reagents were tested for possible interference in the GC-ECD determination of aldehydes and ketones after derivatization with O-(2,3,4,5,6-pentafluorobenzyl)oxylamine (PFBOA). All six-nitrite, cynaide, methanoate (formate), indigo-55'-disulfonate d...

  14. Exploitation of phosphorescent labelling reagent of fullerol-fluorescein isothiocyanate and new method for the determination of trace alkaline phosphatase as well as forecast of human diseases.

    PubMed

    Liu, Jia-Ming; Huang, Xiao-Mei; Liu, Zhen-Bo; Lin, Shao-Qin; Li, Fei-Ming; Gao, Fei; Li, Zhi-Ming; Zeng, Li-Qing; Li, Lian-Ying; Ouyang, Ying

    2009-08-26

    A new phosphorescent labelling reagent consisting of fullerol, fluorescein isothiocyanate and N,N-dimethylaniline (F-ol-(FITC)(n)-DMA) was developed. The mode of action is based on the reactivity of the active -OH group in F-ol with the -COOH group of FITC to form an F-ol-(FITC)(n)-DMA complex containing several FITC molecules. F-ol-(FITC)(n)-DMA increased the number of luminescent molecules in the biological target of WGA-AP-WGA-F-ol-(FITC)(n)-DMA (WGA and AP are wheat germ agglutinin and alkaline phosphatase, respectively) which improved the sensitivity using solid substrate room temperature phosphorimetry (SSRTP) detection. The proposed method provided high sensitivity and strong specificity for WGA-AP. The limit of detection (LD) was 0.15 ag AP spot(-1) for F-ol and 0.097 ag AP spot(-1) for FITC in F-ol-(FITC)(n)-DMA, which was lower than the method using single luminescent molecules of F-ol-DMA and FITC-DMA to label WGA (0.20 ag AP spot(-1) for F-ol-DMA and 0.22 ag AP spot(-1) for FITC-DMA). Results for the determination of AP in human serum were in good agreement with those obtained by enzyme-linked immunosorbent assay. The mechanism of F-ol-(FITC)(n)-DMA labelling of WGA was discussed.

  15. Potentiometric flow injection system for determination of reductants using a polymeric membrane permanganate ion-selective electrode based on current-controlled reagent delivery.

    PubMed

    Song, Wenjing; Ding, Jiawang; Liang, Rongning; Qin, Wei

    2011-10-17

    A polymeric membrane permanganate-selective electrode has been developed as a current-controlled reagent release system for potentiometric detection of reductants in flow injection analysis. By applying an external current, diffusion of permanganate ions across the polymeric membrane can be controlled precisely. The permanganate ions released at the sample-membrane interface from the inner filling solution of the electrode are consumed by reaction with a reductant in the sample solution thus changing the measured membrane potential, by which the reductant can be sensed potentiometrically. Ascorbate, dopamine and norepinephrine have been employed as the model reductants. Under the optimized conditions, the potential peak heights are proportional to the reductant concentrations in the ranges of 1.0×10(-5) to 2.5×10(-7)M for ascorbate, of 1.0×10(-5) to 5.0×10(-7)M for dopamine, and of 1.0×10(-5) to 5.0×10(-7)M for norepinephrine, respectively with the corresponding detection limits of 7.8×10(-8), 1.0×10(-7) and 1.0×10(-7)M. The proposed system has been successfully applied to the determination of reductants in pharmaceutical preparations and vegetables, and the results agree well with those of iodimetric analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Determination of uranium, iron, copper, and nickel from ore samples by MEKC using N,N'-ethylene bis(salicylaldimine) as complexing reagent.

    PubMed

    Mirza, Muhammed Aslam; Khuhawar, Muhammad Yar; Arain, Rafee

    2008-02-01

    An analytical procedure has been developed for the separation of dioxouranium(VI), iron(III), copper(II), nickel(II), cobalt(II), cobalt(III), palladium(II), and thorium(IV) by MEKC using N,N'-ethylene bis(salicylaldimine) (H(2)SA(2)en) as a complexing reagent with total runtime <4.5 min. SDS was used as micellar medium at pH 8 with sodium tetraborate buffer (0.1 M). An uncoated fused-silica capillary with an effective length of 50 cm x 75 microm id was used with an applied voltage of 30 kV with photodiode array detection at 231 nm. Linear calibrations were obtained within 0.111-1000 microg/mL of each element with LODs within 37-325 ng/mL. The developed method was tested for analysis of uranium ore samples indicating its presence within 103-1789 microg/g with RSD within 0.79-1.87%. Likewise copper, nickel, and iron in their combined matrix were also simultaneously determined with RSD 0.4-1.6% (n = 6).

  17. Determination of amlodipine using terbium-sensitized luminescence in the presence of europium(III) as a co-luminescence reagent.

    PubMed

    Al-Kindy, Salma M Z; Al-Snedi, Abdalla; Suliman, Fakhr Eldin O; Al-Lawati, Haidar A J

    2014-09-01

    A sensitive time-resolved luminescence method for the determination of amlodipine (AM) in methanol and in aqueous solution is described. The method is based on the luminescence sensitization of terbium (Tb(3+) ) by formation of a ternary complex with AM in the presence of tri-n-octylphosphine oxide (TOPO) as co-ligand, dodecylbenzenesulfate as surfactant and europium ion as a co-luminescence reagent. The signal for Tb-AM-TOPO is monitored at λex  = 242 nm and λem  = 550 nm. Optimum conditions for the formation of the complex in aqueous system were 0.015 m Tris (hydroxylmethyl) amino methane buffer, pH 9.0, TOPO (1.0 × 10(-4) m), Eu(3+) (2.0 × 10(-7) m), dodecylbenzenesulfate (0.14%) and 6.0 × 10(-5) m of Tb(3+) , which allows the determination of 10-50 ppb of AM with a limit of detection of 1.2 ppb. The relative standard deviations of the method range between 0.1 and 0.2% indicated excellent reproducibility of the method. The proposed method was successfully applied for the assay of AM in pharmaceutical formulations and in plasma samples. Average recoveries of 98.5 ± 0.2% and 95.2 ± 0.2% were obtained for AM in tablet and plasma samples respectively. Copyright © 2013 John Wiley & Sons, Ltd.

  18. Sequential injection analysis (SIA)-chemiluminescence determination of indomethacin using tris[(2,2'-bipyridyl)]ruthenium(III) as reagent and its application to semisolid pharmaceutical dosage forms.

    PubMed

    Mervartová, Katerina; Polásek, Miroslav; Calatayud, José Martínez

    2007-09-26

    Automated sequential injection (SIA) method for chemiluminescence (CL) determination of nonsteroidal anti-inflammatory drug indomethacin (I) was devised. The CL radiation was emitted in the reaction of I (dissolved in aqueous 50% v/v ethanol) with intermediate reagent tris(2,2'-bipyridyl)ruthenium(III) (Ru(bipy)(3)(3+)) in the presence of acetate. The Ru(bipy)(3)(3+) was generated on-line in the SIA system by the oxidation of 0.5mM tris(2,2'-bipyridyl)ruthenium(II) (Ru(bipy)(3)(2+)) with Ce(IV) ammonium sulphate in diluted sulphuric acid. The optimum sequence, concentrations, and aspirated volumes of reactant zones were: 15 mM Ce(IV) in 50mM sulphuric acid 41 microL, 0.5 mM Ru(bipy)(3)(2+) 30 microL, 0.4M Na acetate 16 microL and I sample 15 microL; the flow rates were 60 microLs(-1) for the aspiration into the holding coil and 100 microLs(-1) for detection. Calibration curve relating the intensity of CL (peak height of the transient CL signal) to concentration of I was curvilinear (second order polynomial) for 0.1-50 microM I (r=0.9997; n=9) with rectilinear section in the range 0.1-10 microM I (r=0.9995; n=5). The limit of detection (3sigma) was 0.05 microM I. Repeatability of peak heights (R.S.D., n=10) ranged between 2.4% (0.5 microM I) and 2.0% (7 microM I). Sample throughput was 180 h(-1). The method was applied to determination of 1 to 5% of I in semisolid dosage forms (gels and ointments). The results compared well with those of UV spectrophotometric method.

  19. Determination of histamine in microdialysis samples from rat brain by microbore column liquid chromatography following intramolecular excimer-forming derivatization with pyrene-labeling reagent.

    PubMed

    Yoshitake, Takashi; Yamaguchi, Masatoshi; Nohta, Hitoshi; Ichinose, Fumio; Yoshida, Hideyuki; Yoshitake, Shimako; Fuxe, Kjell; Kehr, Jan

    2003-07-15

    This paper describes a sensitive and selective liquid chromatographic method with fluorescence detection for determination of histamine in brain microdialysis samples from awake rats. Samples containing histamine (10 microl) were derivatized with 20 microl of the reagent consisting of 3 mM 4-(1-pyrene)butyric acid N-hydroxysuccinimide ester (PSE), 3 mM potassium carbonate and acetonitrile (1:1:18, v/v), thereafter 20 microl volume was injected onto the microbore column packed with C18 silica gel. The histamine derivative contained two pyrene moieties, which generated intramolecular excimer fluorescence (450-540 nm) and allowed clear discrimination from the monomer fluorescence (360-420 nm) emitted by PSE itself. The separation of histamine-pyrene derivative was achieved within 25 min, the detection limit (S/N=3) was 0.3 fmol histamine in 20 microl injected. The basal extracellular levels of histamine collected in 10-min fractions (fmol per 10 microl, mean+/-S.D., not corrected for recovery, n=10 rats) were 35.45+/-4.56 (hypothalamus), 9.05+/-1.56 (prefrontal cortex), 7.83+/-0.86 (hippocampus) and 6.54+/-0.66 (striatum). The voltage-sensitive release of histamine was evaluated by perfusing the probes with high (100 mM) concentration of potassium ions or with sodium channel blocker tetrodotoxin (1 microM), and the calcium-dependent release was tested by perfusion with calcium-free Ringer solution. These data, together with physiologically induced increase of extracellular histamine in four examined brain regions during forced swimming demonstrate that this method is suitable for high-sensitive determination of neuronally released histamine under various pharmacological and physiological conditions.

  20. Use of fluorescein hydrazide and fluorescein thiosemicarbazide reagents for the fluorometric determination of protein carbonyl groups and for the detection of oxidized protein on polyacrylamide gels.

    PubMed

    Ahn, B; Rhee, S G; Stadtman, E R

    1987-03-01

    Highly fluorescent thiosemicarbazide and hydrazide prepared by reaction of fluorescein isothiocyanate with hydrazine or adipic acid dihydrazide have been used to monitor the presence of carbonyl groups in oxidatively modified proteins. After oxidation, proteins react with these reagents under anaerobic conditions in the dark to yield fluorescent protein conjugates (presumably thiosemicarbazones or hydrazones) which can be visualized as fluorescent bands following electrophoresis (0-4 degrees C) on lithium dodecyl sulfate-polyacrylamide gels. These reagents do not react with unoxidized proteins. The conjugates formed dissociate readily at room temperature but are fairly stable at pH 6-9, 0 degrees C. Current data suggest that these reagents will be useful in the detection and quantitation of oxidatively modified proteins in biological systems.

  1. Purity control of uranium by neutron activation assay--II. Determination of manganese, nickel and copper.

    PubMed

    Abdel-Rassoul, A A; Wahba, S S

    1967-09-01

    Activation analysis is applied for the simultaneous determination of manganese, nickel and copper in different uranium samples, including metallic uranium, uranium concentrates, oxide, acetate, nitrate and sodium uranate. The analytical scheme developed is based on separation of the uranium by paper chromatography and subsequent determination of these elements in the pile-irradiated residues by simple radiochemical operations. The reliability of the scheme proposed is tested, and the limits of sensitivity of the methods worked out are ascertained. Accordingly, microgram concentrations of the elements studied could be assayed in limited quantities of the samples analysed with a precision of +/- 15%. Reagent-blank determinations are also considered.

  2. Simplified NaCl based (68)Ga concentration and labeling procedure for rapid synthesis of (68)Ga radiopharmaceuticals in high radiochemical purity.

    PubMed

    Mueller, Dirk; Klette, Ingo; Baum, Richard P; Gottschaldt, M; Schultz, Michael K; Breeman, Wouter A P

    2012-08-15

    A simple sodium chloride (NaCl) based (68)Ga eluate concentration and labeling method that enables rapid, high-efficiency labeling of DOTA conjugated peptides in high radiochemical purity is described. The method utilizes relatively few reagents and comprises minimal procedural steps. It is particularly well-suited for routine automated synthesis of clinical radiopharmaceuticals. For the (68)Ga generator eluate concentration step, commercially available cation-exchange cartridges and (68)Ga generators were used. The (68)Ga generator eluate was collected by use of a strong cation exchange cartridge. 98% of the total activity of (68)Ga was then eluted from the cation exchange cartridge with 0.5 mL of 5 M NaCl solution containing a small amount of 5.5 M HCl. After buffering with ammonium acetate, the eluate was used directly for radiolabeling of DOTATOC and DOTATATE. The (68)Ga-labeled peptides were obtained in higher radiochemical purity compared to other commonly used procedures, with radiochemical yields greater than 80%. The presence of (68)Ge could not be detected in the final product. The new method obviates the need for organic solvents, which eliminates the required quality control of the final product by gas chromatography, thereby reducing postsynthesis analytical effort significantly. The (68)Ga-labeled products were used directly, with no subsequent purification steps, such as solid-phase extraction. The NaCl method was further evaluated using an automated fluid handling system and it routinely facilitates radiochemical yields in excess of 65% in less than 15 min, with radiochemical purity consistently greater than 99% for the preparation of (68)Ga-DOTATOC.

  3. Determination of citrus limonoid glucosides by high performance liquid chromatography coupled to post-column reaction with Ehrlich’s Reagent

    USDA-ARS?s Scientific Manuscript database

    A method for the identification and quantification of citrus limonoid glucosides in juices based upon high performance liquid chromatography (HPLC) separation coupled to post-column reaction with Ehrlichs’s reagent has been developed. This method utilizes a phenyl stationary phase and an isocratic ...

  4. Highly sensitive derivatization reagents possessing positively charged structures for the determination of oligosaccharides in glycoproteins by high-performance liquid chromatography electrospray ionization tandem mass spectrometry.

    PubMed

    Min, Jun Zhe; Nagai, Keisuke; Shi, Qing; Zhou, Wenjun; Todoroki, Kenichiro; Inoue, Koichi; Lee, Yong-Ill; Toyo'oka, Toshimasa

    2016-09-23

    We have developed three kinds of novel derivatization reagents (4-CEBTPP, 4-CBBTPP, 5-COTPP) with triphenylphosphine (TPP) as a basic structure carrying a permanent positive charge for resolution of the oligosaccharides in glycoprotein using high-performance liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). The synthesized reagents reacted with the sialylglycosylamine of the sialylglycopeptide after treatment by PNGase F. The final derivatives were analyzed by ESI-MS and sensitively detected in the selected reaction monitoring (SRM) mode. Furthermore, the limits of detection (S/N=3) on the SRM chromatograms were at the fmol level (30fmol). Therefore, we used the limit of detection of the reagent products detected by the SRM and evaluated the utility of each reagent. Among the reagents, the positively charged 4-CEBTPP derivative's peak area was the highest; 4-CEBTPP with a positively charged structure showed about a 20 times greater sensitivity for the glycosylamine of the SGP product compared to the conventional fluorescence reagent, Fmoc-Cl. In addition, various fragment ions based on the carbohydrate units also appeared in the MS/MS spectra. Among the fragment ions, m/z 627.37 (CE=40eV) corresponding to 4-CEBTPP-GlcNAc and m/z 120.09 (CE=100eV) corresponding to 4-CEBTPP are the most important ones for identifying the oligosaccharide. 4-CEBTPP-SGA was easily identified by the selected-ion chromatogram in the product ion scan (m/z 120.09) and in the precursor ion scan (m/z 627.37) by MS/MS detection. The derivatized analytes have a high ionization efficiency and they are detected with a high sensitivity in the electrospray ionization. The novel derivatization reagent with a multi-function provided a higher sensitivity for the oligosaccharide analysis, as well as a better specificity and feasibility. Furthermore, several oligosaccharides in fetuin and ribonuclease B were successfully identified by the proposed procedure

  5. A novel approach for HPLC determination of 2-cynaoacetamide using derivatization procedure with 2-hydroxyacetophenone as a new useful derivatization reagent.

    PubMed

    Douša, Michal; Břicháč, Jiří; Tkadlecová, Marcela; Man, Stanislav; Zezula, Josef; Hájíček, Josef; Pekárek, Tomáš

    2016-09-05

    A novel and sensitive derivatization procedure for the determination of 2-cynaoacetamide in pharmaceutical samples using liquid chromatography with the fluorescence detection was discovered. The method is based on derivatization of 2-cynaoacetamide using 2-hydroxyacetophenone as a new derivatization reagent. The product of derivatization reaction was isolated and characterized using spectroscopic techniques namely LC-MS, NMR and IR. The structure of 2-cyanoacetamide derivative was unambiguously assigned as a 2-amino-4-phenylfuran-3-carboxamide. Two derivatization systems were optimized in terms of reaction temperature, reaction time, pH and concentration of 2-hydroxyacetophenone, and a new pre- and post-derivatization HPLC methods were developed. The separations on HPLC with pre-column derivatization were accomplished using stationary phase based on a XBridge C18 column (100×4.6, 3.5μm) and isocratic elution using the mobile phase acetonitrile - 0.1% formic acid (30:70, v/v). The separations on the HPLC with post-column derivatization were performed on stationary phase on a TSKgel Amide-80 column (150×4.6mm, 3μm). The mobile phase was a mixture of acetonitrile, methanol and 10mM sodium formate buffer at pH=4.5 in ratio 3:2:95 (v/v). Both HPLC methods were fully validated in terms of linearity, sensitivity (limit of detection and limit of quantification), accuracy and precision according to ICH guidelines. The pre-column derivatization method was linear in the range 1.1-2000μg/l with method accuracy≥98.2% and method precision RSD≤4.8%. The post-column derivatization method was linear in the range 12-2000μg/l. Method accuracy≥96.3% and method precision RSD≤3.5%. Proposed new methods were proved to be highly sensitive, simple and rapid, and were successfully applied to the determinations of 2-cynaoacetamide in pregabalin.

  6. Antiproton nucleus potentials from global fits to antiprotonic X-rays and radiochemical data

    NASA Astrophysics Data System (ADS)

    Friedman, E.; Gal, A.; Mareš, J.

    2005-11-01

    We report on global fits of optical-model parameters to 90 data points for p¯ X-rays and 17 data points of radiochemical data put together. By doing separate fits to the two kinds of data it is possible to determine phenomenologically the radial region where the absorption of antiprotons takes place and to obtain neutron densities which represent the average behaviour over the periodic table. A finite-range attractive and absorptive p¯-nuclear isoscalar potential fits the data well. Self-consistent dynamical calculations within the RMF model demonstrate that the polarization of the nucleus by the atomic antiproton is negligible.

  7. Radiochemical Determination of Polonium in Liquid Metal Spallation Targets

    NASA Astrophysics Data System (ADS)

    Hammer, B.; Schumann, D.; Neuhausen, J.; Wohlmuther, M.; Türler, A.

    2014-05-01

    The MEGAPIE target, consisting of 82 litres of lead-bismuth eutectic (LBE), was irradiated close to the megawatt range (0.8 MW) from August to December 2006 in the SINQ facility at PSI. After a cooling period of 5 years, a post-irradiation examination (PIE) program was started and samples were taken from different positions in the target. In this paper we focus on the measurement of α-emitting 208-210Po in the MEGAPIE target. The experimental results are compared with theoretical predictions obtained by FLUKA and MCNPX calculations.

  8. An enzymic radiochemical method for determining phosphatidylglycerol in amniotic fluid

    SciTech Connect

    Siegel, L.; Walker, S.I.; Robin, N.I.

    1983-05-01

    We describe an enzymic quantification of phosphatidylglycerol in amniotic fluid. Phosphatidylglycerol is hydrolyzed in alkali and the resulting glycerol is then enzymatically phosphorylated with adenosine 5'-(gamma-/sup 32/P)triphosphate to yield glycero(/sup 32/P)phosphate. After removal of excess (gamma-/sup 32/P)ATP by charcoal, the radioactivity of the glycerophosphate is measured in a liquid scintillation counter. Triglyceride in the amniotic fluid is hydrolyzed by lipase before extraction and thus does not interfere with the analysis. This method is specific for phosphatidylglycerol. Preliminary studies suggest that a phosphatidylglycerol value greater than or equal to 10 nmol/mL correlates with fetal lung maturity.

  9. Radiochemical Sensor for Continuous and Remote Liquid Effluents Monitoring

    SciTech Connect

    Tarancon, A.; Garcia, J.F.; Rauret, G.; Padro, A.

    2008-07-01

    On-line radioactivity monitoring in liquid effluents is an increasing need according to the international regulations at present. Classical activity determination procedures include the sequence of sampling, chemical treatment, measurement and data treatment. These steps are man-power consuming, generate a great amount of waste and introduce an important delay between the potential pollution event and its detection and quantification. To overcome these limitations, we have developed a radiochemical sensor for liquid effluents capable of sending information about the specific activity and volume of a contamination episode to a remote position, on line and continuously. The capabilities of the sensor developed here allow detecting and quantifying contamination pulses of alpha, beta and gamma emitters of different volumes and activity levels included in a continuous stream. Sensor receptor includes two detection systems, one addressed to determine alpha, beta and gamma events and the other to detect sample gamma emissions. Detailed sensor structure will be shown at the conference because patent is in process at this moment. Detection efficiencies (%) obtained in the alpha-beta-gamma system for the range of contamination volumes considered (2- 300 ml) are: 1.6 - 3.2%, for Pu-240; 22.2 - 58.4%, for Sr-90/Y-90 and 8.8 -17.7%, for Cs-134. In the gamma system, values for Cs-134 detection range from 0.6% to 1.3%. Prediction errors obtained show that sensor is capable to detect Sr-90/Y-90 contamination pulses of at least 2 ml and 3 Bq/ml with a relative error lower of 10% in activity and 60% in volume. When contamination pulse increases up to 7 ml, relative errors decrease to 5% for both magnitudes. For Pu-240 and Cs-134, when contamination pulses are of at least 7 ml and 300 Bq/ml, the relative errors obtained in determinations performed in the alpha-beta-gamma system are lower than 10% in activity and 20 % in volume. The same errors are obtained in the gamma system for Cs

  10. Radiochemical Mix Diagnostic in the Presence of Burn

    SciTech Connect

    Hayes, Anna C.

    2014-01-28

    There is a general interest in radiochemical probes of hydrodamicalmix in burning regions of NIF capsule. Here we provide estimates for the production of 13N from mixing of 10B ablator burning hotspot of a capsule. By comparing the 13N signal with x-ray measurements of the ablator mix into the hotspot it should be possible to estimate the chunkiness of this mix.

  11. Radiochemical separation of gallium by amalgam exchange

    USGS Publications Warehouse

    Ruch, R.R.

    1969-01-01

    An amalgam-exchange separation of radioactive gallium from a number of interfering radioisotopes has been developed. A dilute (ca. 0.3%) gallium amalgam is agitated with a slightly acidic solution of 72Ga3+ containing concentrations of sodium thiocyanate and either perchlorate or chloride. The amalgam is then removed and the radioactive gallium stripped by agitation with dilute nitric acid. The combined exchange yield of the perchlorate-thiocyanate system is 90??4% and that of the chloride-thiocyanate system is 75??4%. Decontamination yields of most of the 11 interfering isotopes studied were less than 0.02%. The technique is applicable for use with activation analysis for the determination of trace amounts of gallium. ?? 1969.

  12. Automatic measurements and computations for radiochemical analyses

    USGS Publications Warehouse

    Rosholt, J.N.; Dooley, J.R.

    1960-01-01

    In natural radioactive sources the most important radioactive daughter products useful for geochemical studies are protactinium-231, the alpha-emitting thorium isotopes, and the radium isotopes. To resolve the abundances of these thorium and radium isotopes by their characteristic decay and growth patterns, a large number of repeated alpha activity measurements on the two chemically separated elements were made over extended periods of time. Alpha scintillation counting with automatic measurements and sample changing is used to obtain the basic count data. Generation of the required theoretical decay and growth functions, varying with time, and the least squares solution of the overdetermined simultaneous count rate equations are done with a digital computer. Examples of the complex count rate equations which may be solved and results of a natural sample containing four ??-emitting isotopes of thorium are illustrated. These methods facilitate the determination of the radioactive sources on the large scale required for many geochemical investigations.

  13. Novel chiral derivatization reagents possessing a pyridylthiourea structure for enantiospecific determination of amines and carboxylic acids in high-throughput liquid chromatography and electrospray-ionization mass spectrometry for chiral metabolomics identification.

    PubMed

    Nagao, Ryuji; Tsutsui, Haruhito; Mochizuki, Toshiki; Takayama, Takahiro; Kuwabara, Tomohiro; Min, Jun Zhe; Inoue, Koichi; Todoroki, Kenichiro; Toyo'oka, Toshimasa

    2013-06-28

    This paper reports the synthesis and the application of novel derivatization reagents possessing a pyridylthiourea structure for the enantiospecific determination of chiral amines and carboxylic acids in high-throughput LC-ESI-MS/MS. The novel reagents, i.e., (R)-N-(3-pyridylthiocarbamoyl)pyrrolidine-2-carboxylic acid (PyT-C) and (S)-3-amino-1-(3-pyridylthiocarbamoyl)pyrrolidine (PyT-N), were evaluated as chiral derivatization reagents for the enantiomeric determination of chiral amines and carboxylic acids, respectively, in terms of separation efficiency by reversed-phase chromatography and detection sensitivity by ESI-MS/MS. The chiral amines and carboxylic acids were easily labeled with PyT-C and PyT-N, respectively, at 60°C in 60min in the presence of 2,2'-dipyridyl disulfide (DPDS) and triphenylphosphine (TPP) as the activation reagents. The resulting diastereomers were completely separated by reversed-phase chromatography using a small particle (1.7μm) ODS column (Rs=3.54-6.00 for carboxylic acids and Rs=3.07-4.75 for amines). A highly sensitive detection at the sub-fmol level was also obtained from the SRM chromatograms at a single monitoring ion, m/z 137.0 (0.72-1.46fmol for carboxylic acids and 0.55-1.89fmol for amines). The proposed procedure using PyT-C and PyT-N was applied to the determination of chiral amines and carboxylic acids spiked into human saliva, as a model study of chiral metabonomics identification. dl-Amino acid methyl esters and N-acetyl dl-amino acids, which are the representatives as the chiral amines and carboxylic acids, in the saliva were clearly identified by the present method. Because the same product ion at m/z 137.0 was obtained from collision-induced dissociation (CID) of protonated molecular ions of all the derivatives, the proposed procedure using both reagents (i.e., PyT-C and PyT-N) seems to be useful for chiral metabolomics identification having selected functional groups (i.e., amines and carboxylic acids).

  14. Radiochemical purity of Mo and Tc solution obtained after irradiation and dissolution of Mo-100-enriched and ultra-high-purity natural Mo disks

    SciTech Connect

    Tkac, Peter; Gromov, Roman; Chemerisov, Sergey D.; Rotsch, David A.; Vandegrift, George F.

    2016-09-01

    Four irradiations of ultra-high-purity natural Mo targets and one irradiation using 97.4% Mo-100-enriched material were performed. The purpose of these irradiations was to determine whether the presence of Sn stabilizer in the H2O2 used for the dissolution of sintered Mo disks can affect the radiochemical purity of the final K2MoO4 in 5M KOH solution. Results from radiochemical purity tests performed using thin-layer paper chromatography show that even 2– 3× excess of Sn-stabilized H2O2 typically used for dissolution of sintered Mo disks did not affect the radiochemical purity of the final product.

  15. Simultaneous determination of glucose, triglycerides, urea, cholesterol, albumin and total protein in human plasma by Fourier transform infrared spectroscopy: direct clinical biochemistry without reagents.

    PubMed

    Jessen, Torben E; Höskuldsson, Agnar T; Bjerrum, Poul J; Verder, Henrik; Sørensen, Lars; Bratholm, Palle S; Christensen, Bo; Jensen, Lene S; Jensen, Maria A B

    2014-09-01

    Direct measurement of chemical constituents in complex biologic matrices without the use of analyte specific reagents could be a step forward toward the simplification of clinical biochemistry. Problems related to reagents such as production errors, improper handling, and lot-to-lot variations would be eliminated as well as errors occurring during assay execution. We describe and validate a reagent free method for direct measurement of six analytes in human plasma based on Fourier-transform infrared spectroscopy (FTIR). Blood plasma is analyzed without any sample preparation. FTIR spectrum of the raw plasma is recorded in a sampling cuvette specially designed for measurement of aqueous solutions. For each analyte, a mathematical calibration process is performed by a stepwise selection of wavelengths giving the optimal least-squares correlation between the measured FTIR signal and the analyte concentration measured by conventional clinical reference methods. The developed calibration algorithms are subsequently evaluated for their capability to predict the concentration of the six analytes in blinded patient samples. The correlation between the six FTIR methods and corresponding reference methods were 0.87

  16. Fluorinated Diluents - New Possibilities For Radiochemical Technology

    SciTech Connect

    Babain, V.A.

    2007-07-01

    increases solubility of metal solvates, but, as a rule, the hazard of forming the third phase or precipitate remains even on complete saturation. Introduction of modifier into the system results in additional formation of new plausible radiolysis products, the effect of which on extraction and especially on stripping process calls for further investigation. An alternative approach to improving the solubility of extractants consists in the use of well-solvating polar solvents. Diluents modify the extraction ability of extractant over a wide range. The polar diluents enhance the extraction process of metals and the solubility of complexes in many cases, especially as applied to polydentate compounds. The use of fluorinated polar diluents for many extractants allows to offer much more effective extraction flowsheets of radionuclide recovery. The operating experience on meta-nitro-benzo-trifluoride (MNBTF, F-3, fluoro-pole-732) has shown that it is more readily regenerated than saturated hydrocarbons. Its radiolysis products are washed-out into aqueous phase and are not accumulated in organic phase. Some doubts on high corrosion hazard are overestimated, as is obvious from practical implementation. Based upon the principle of optimizing not an individual operation, but the process as a whole the fluorinated diluents may be considerably more efficient than the traditional hydrocarbon ones. Unfortunately, up till now there has been no way to determine the effect of diluent structure on the extraction properties of system. Nevertheless, the empirical regularities generalizing the large volume of experimental data have made it possible to define several classes of compounds showing promise as potential commercial diluents. (author)

  17. Hydrologic conditions and distribution of selected radiochemical and chemical constituents in water, Snake River Plain aquifer, Idaho National Engineering Laboratory, Idaho, 1992 through 1995

    SciTech Connect

    Bartholomay, R.C.; Tucker, B.J.; Ackerman, D.J.; Liszewski, M.J.

    1997-04-01

    Radiochemical and chemical wastewater discharged since 1952 to infiltration ponds and disposal wells at the Idaho National Engineering Laboratory (INEL) has affected water quality in the Snake River Plain aquifer. The US Geological Survey, in cooperation with the US Department of Energy, maintains a monitoring network at the INEL to determine hydrologic trends and to delineate the movement of radiochemical and chemical wastes in the aquifer. This report presents an analysis of water-level and water-quality data collected from the Snake River Plain aquifer during 1992--95.

  18. Determination of amines using 2-(11H-benzo[a]carbazol-11-yl) ethyl chloroformate (BCEC-Cl) as labeling reagent by HPLC with fluorescence detection and identification with APCI/MS.

    PubMed

    You, Jinmao; Zhao, Wenchen; Liu, Lingjun; Zhao, Xianen; Suo, Yourui; Wang, Honglun; Li, Yulin; Ding, Chenxu

    2007-05-15

    A pre-column derivatization method for the sensitive determination of amines using a labeling reagent 2-(11H-benzo[a]-carbazol-11-yl) ethyl chloroformate (BCEC-Cl) followed by high-performance liquid chromatography with fluorescence detection has been developed. Identification of derivatives was carried out by LC/APCI/MS in positive-ion mode. The chromophore of 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) reagent was replaced by 2-(11H-benzo[a]-carbazol-11-yl) ethyl functional group, which resulted in a sensitive fluorescence derivatizing reagent BCEC-Cl. BCEC-Cl could easily and quickly label amines. Derivatives were stable enough to be efficiently analyzed by HPLC and showed an intense protonated molecular ion corresponding m/z [M+H](+) under APCI/MS in positive-ion mode. The collision-induced dissociation of the protonated molecular ion formed characteristic fragment ions at m/z 261.8 and m/z 243.8 corresponding to the cleavages of CH(2)O-CO and CH(2)-OCO bonds. Studies on derivatization demonstrated excellent derivative yields over the pH 9.0-10.0. Maximal yields close to 100% were observed with three- to four-fold molar reagent excess. In addition, the detection responses for BCEC-derivatives were compared to those obtained using 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC-Cl) and 9-fluorenyl methylchloroformate (FMOC-Cl) as labeling reagents. The ratios I(BCEC)/I(BCEOC)=1.94-2.17 and I(BCEC)/I(FMOC)=1.04-2.19 for fluorescent (FL) responses (here, I was relative fluorescence intensity). Separation of the derivatized amines had been optimized on reversed-phase Eclipse XDB-C(8) column. Detection limits calculated from 0.50pmol injection, at a signal-to-noise ratio of 3, were 1.77-14.4fmol. The relative standard deviations for within-day determination (n=11) were 1.84-2.89% for the tested amines. The mean intra- and inter-assay precision for all amines levels were <3.64% and 2.52%, respectively. The mean recoveries ranged from

  19. Use of Protein Folding Reagents.

    PubMed

    2016-04-01

    The reagents and methods for purification and use of the most commonly used denaturants, guanidine hydrochloride (guanidine-HCl) and urea, are described. Other protein denaturants and reagents used to fold proteins are briefly mentioned. Sulfhydryl reagents (reducing agents) and "oxido-shuffling" (or oxidative regeneration) systems are also described.

  20. Guiding Principles for Sustainable Existing Buildings: Radiochemical Processing Laboratory

    SciTech Connect

    Pope, Jason E.

    2013-11-11

    In 2006, the United States (U.S.) Department of Energy (DOE) signed the Federal Leadership in High Performance and Sustainable Buildings Memorandum of Understanding (MOU), along with 21 other agencies. Pacific Northwest National Laboratory (PNNL) is exceeding this requirement and, currently, about 25 percent of its buildings are High Performance and Sustainable Buildings. The pages that follow document the Guiding Principles conformance effort for the Radiochemical Processing Laboratory (RPL) at PNNL. The RPL effort is part of continued progress toward a building inventory that is 100 percent compliant with the Guiding Principles.

  1. Radiochemical separation methods for preparation of biomedical cyclotron radionuclides

    NASA Astrophysics Data System (ADS)

    Zaitseva, N. G.; Dmitriev, S. N.

    1999-01-01

    A short review of the radiochemical methods for preparation of widely used or promising cyclotronproduced radionuclides for nuclear medicine and biomedical or environmental studies is given. The presented data include the current status of the production of some gamma-emitters (97Ru, 111In, 123I, 201Tl), generator-pairs (68Ge/68Ga, 82Sr/82Rb, 128Ba/128Cs, 178W/178Ta), radioisotopes for metabolism studies (26Al, 67Cu, 237Pu) and actinides tracers for environmental researches (235Np, 236Np, 236Pu). The conditions for preparation of high-purity isotopes have been investigated and procedures including target chemistry design were developed.

  2. Low temperature radio-chemical energy conversion processes

    SciTech Connect

    Gomberg, H.J.

    1986-11-04

    This patent describes a radio-chemical method of converting radiated energy into chemical energy form comprising the steps of: (a) establishing a starting chemical compound in the liquid phase that chemically reacts endothermically to radiation and heat energy to produce a gaseous and a solid constituent of the compound, (b) irradiating the compound in its liquid phase free of solvents to chemically release therefrom in response to the radiation the gaseous and solid constituents, (c) physically separating the solid and gaseous phase constituents from the liquid, and (d) chemically processing the constituents to recover therefrom energy stored therein by the irradiation step (b).

  3. Facility Effluent Monitoring Plan for the 325 Radiochemical Processing Laboratory

    SciTech Connect

    Shields, K.D.; Ballinger, M.Y.

    1999-04-02

    This Facility Effluent Monitoring Plan (FEMP) has been prepared for the 325 Building Radiochemical Processing Laboratory (RPL) at the Pacific Northwest National Laboratory (PNNL) to meet the requirements in DOE Order 5400.1, ''General Environmental Protection Programs.'' This FEMP has been prepared for the RPL primarily because it has a ''major'' (potential to emit >0.1 mrem/yr) emission point for radionuclide air emissions according to the annual National Emission Standards for Hazardous Air Pollutants (NESHAP) assessment performed. This section summarizes the airborne and liquid effluents and the inventory based NESHAP assessment for the facility. The complete monitoring plan includes characterization of effluent streams, monitoring/sampling design criteria, a description of the monitoring systems and sample analysis, and quality assurance requirements. The RPL at PNNL houses radiochemistry research, radioanalytical service, radiochemical process development, and hazardous and radioactive mixed waste treatment activities. The laboratories and specialized facilities enable work ranging from that with nonradioactive materials to work with picogram to kilogram quantities of fissionable materials and up to megacurie quantities of other radionuclides. The special facilities within the building include two shielded hot-cell areas that provide for process development or analytical chemistry work with highly radioactive materials and a waste treatment facility for processing hazardous, mixed radioactive, low-level radioactive, and transuranic wastes generated by PNNL activities.

  4. Radiochemical analysis of 41Ca and 45Ca.

    PubMed

    Suárez, J A; Rodríguez, M; Espartero, A G; Piña, G

    2000-03-01

    The radioactive isotopes of calcium, 41Ca (t1/2 = 1.03 x 10(5) yr) and 45Ca (t1/2 = 163 d), are produced by neutron capture in the stable isotopes 40Ca and 44Ca, respectively. These radionuclides are present in the environment due to the reactions between the galactic cosmic rays and the earth's surface, and in nuclear power plants by the activation of the structural components of nuclear reactor vessels. The aim of this paper is to propose a radiochemical separation method of 41Ca and 45Ca from the other beta gamma emitters present in radioactive materials, based on selective precipitation reactions. The activities were measured by liquid scintillation counting (LSC). The obtained decontamination factors are satisfactory for each radioactive component of the initial sample in that their activities in the final product were lower than the minimum detectable activity (MDA) due to the effectiveness of the radiochemical procedure. The sensitivity of the method allows the radiological characterization of 41Ca and 45Ca content in radioactive materials.

  5. Radiochemical ageing of EPDM elastomers. 3. Mechanism of radiooxidation

    NASA Astrophysics Data System (ADS)

    Rivaton, A.; Cambon, S.; Gardette, J.-L.

    2005-01-01

    The preceding paper of this series was devoted to the identification and quantification of the main chemical changes resulting from the radiochemical ageing of EPDM (77.9% ethylene, 21.4% propylene, 0.7% diene) and EPR (76.6% ethylene, 23.4% propylene) films irradiated under oxygen atmosphere using 60Co gamma rays. The double bond of the diene was observed to be consumed with a high radiochemical yield. The oxidation and reticulation rates were observed to be higher in the case of EPDM than in EPR. Accumulation of the major oxidation products in both polymers was shown to occur in the order of decreasing concentrations: hydroperoxides, ketones, carboxylic acids and alcohols, peroxides. On the basis of the analysis of the oxidation products formed in EPDM and EPR, and taking into account their relative concentrations, the mechanisms accounting for the EPDM γ-degradation under oxygen atmosphere are proposed in the present paper. Two main processes are involved in the EPDM radiooxidation. The random γ-radiolysis of the polymer provides a constant source of macroalkyl radicals mainly formed on ethylene units. The secondary radicals so formed are likely to initiate a selective oxidation of the polymer through free-radicals reactions involving the abstraction of labile hydrogen atoms. In particular, the hydroperoxides decomposition and the consumption of the ENB moieties, this latter being the most oxidisable site and the source of crosslinking, may result from hydrogen abstraction by radical species.

  6. Analysis of low levels of rare earths by radiochemical neutron activation analysis

    USGS Publications Warehouse

    Wandless, G.A.; Morgan, J.W.

    1985-01-01

    A procedure for the radiochemical neutron-activation analysis for the rare earth elements (REE) involves the separation of the REE as a group by rapid ion-exchange methods and determination of yields by reactivation or by energy dispersive X-ray fluorescence (EDXRF) spectrometry. The U. S. Geological Survey (USGS) standard rocks, BCR-1 and AGV-1, were analyzed to determine the precision and accuracy of the method. We found that the precision was ??5-10% on the basis of replicate analysis and that, in general the accuracy was within ??5% of accepted values for most REE. Data for USGS standard rocks BIR-1 (Icelandic basalt) and DNC-1 (North Carolina diabase) are also presented. ?? 1985 Akade??miai Kiado??.

  7. Solid debris collection for radiochemical diagnostics at the National Ignition Facilitya)

    NASA Astrophysics Data System (ADS)

    Gostic, J. M.; Shaughnessy, D. A.; Moore, K. T.; Hutcheon, I. D.; Grant, P. M.; Moody, K. J.

    2012-10-01

    Radiochemical analysis of post-ignition debris inside the National Ignition Facility (NIF) target chamber can help determine various diagnostic parameters associated with the implosion efficiency of the fusion capsule. This technique is limited by the ability to distinguish ablator material from other debris and by the collection efficiency of the capsule debris after implosion. Prior to designing an on-line collection system, the chemical nature and distribution of the debris inside the chamber must be determined. The focus of our current work has been on evaluating capture of activated Au hohlraum debris on passive foils (5 cm diameter, 50 cm from target center) post-shot. Preliminary data suggest that debris distribution is locally heterogeneous along the equatorial and polar line-of-sights.

  8. Analysis of 161Tb by radiochemical separation and liquid scintillation counting

    SciTech Connect

    Jiang, J.; Davies, A.; Arrigo, L.; Friese, J.; Seiner, B. N.; Greenwood, L.; Finch, Z.

    2015-12-05

    The determination of 161Tb activity is problematic due to its very low fission yield, short half-life, and the complication of its gamma spectrum. At AWE, radiochemically purified 161Tb solution was measured on a PerkinElmer 1220 QuantulusTM Liquid Scintillation Spectrometer. Since there was no 161Tb certified standard solution available commercially, the counting efficiency was determined by the CIEMAT/NIST Efficiency Tracing method. The method was validated during a recent inter-laboratory comparison exercise involving the analysis of a uranium sample irradiated with thermal neutrons. Lastly, the measured 161Tb result was in excellent agreement with the result using gamma spectrometry and the result obtained by Pacific Northwest National Laboratory.

  9. Analysis of 161Tb by radiochemical separation and liquid scintillation counting

    DOE PAGES

    Jiang, J.; Davies, A.; Arrigo, L.; ...

    2015-12-05

    The determination of 161Tb activity is problematic due to its very low fission yield, short half-life, and the complication of its gamma spectrum. At AWE, radiochemically purified 161Tb solution was measured on a PerkinElmer 1220 QuantulusTM Liquid Scintillation Spectrometer. Since there was no 161Tb certified standard solution available commercially, the counting efficiency was determined by the CIEMAT/NIST Efficiency Tracing method. The method was validated during a recent inter-laboratory comparison exercise involving the analysis of a uranium sample irradiated with thermal neutrons. Lastly, the measured 161Tb result was in excellent agreement with the result using gamma spectrometry and the result obtainedmore » by Pacific Northwest National Laboratory.« less

  10. Determination of Diacetyl in Beer by a Precolumn Derivatization-HPLC-UV Method Using 4-(2,3-Dimethyl-6-quinoxalinyl)-1,2-benzenediamine as a Derivatizing Reagent.

    PubMed

    Wang, Ji-Yu; Wang, Xin-Jie; Hui, Xian; Hua, Shui-Hong; Li, Heng; Gao, Wen-Yun

    2017-03-29

    Diacetyl is an important flavoring compound in many foods, especially in beer. In the present study, we developed and validated a new precolumn derivatization HPLC-UV method for the determination of diacetyl using 4-(2,3-dimethyl-6-quinoxalinyl)-1,2-benzenediamine as a novel derivatizing reagent. After derivatization with the reagent at a pH value 4.0 at ambient temperature for 10 min, diacetyl was analyzed on an ODS column and detected at 254 nm. The results show that the correlation coefficient of the method is 0.9991 in the range of 0.10 to 100.0 μM diacetyl, and the limit of detection is 0.02 μM. The method was further evaluated in the analysis of beer samples with the recoveries ranging from 94.4 to 102.6% and RSDs from 1.36 to 3.33%. The concentrations of diacetyl in 8 beer samples were determined in the range of 0.19 to 0.42 μM. The method established in this study may be well suitable for the determination of diacetyl in beer.

  11. Unnatural Isotopic Composition of Lithium Reagents

    USGS Publications Warehouse

    Qi, H.P.; Coplen, T.B.; Wang, Q. Zh; Wang, Y.-H.

    1997-01-01

    Isotopic analysis of 39 lithium reagents from several manufacturers indicates that seven were artificially depleted in 6Li significantly in excess of the variation found in terrestrial materials. The atomic weight of lithium in analyzed reagents ranged from 6.939 to 6.996, and ??7-Li, reported relative to L-SVEC lithium carbonate, ranged from -11 to +3013???. This investigation indicates that 6Li-depleted reagents are now found on chemists' shelves, and the labels of these 6Li-depleted reagents do not accurately reflect the atomic and (or) molecular weights of these reagents. In 1993, IUPAC issued the following statement: "Commercially available Li materials have atomic weights that range between 6.94 and 6.99; if a more accurate value is required, it must be determined for the specific material." This statement has been found to be incorrect In two of the 39 samples analyzed, the atomic weight of Li was in excess of 6.99.

  12. Validation of affinity reagents using antigen microarrays.

    PubMed

    Sjöberg, Ronald; Sundberg, Mårten; Gundberg, Anna; Sivertsson, Asa; Schwenk, Jochen M; Uhlén, Mathias; Nilsson, Peter

    2012-06-15

    There is a need for standardised validation of affinity reagents to determine their binding selectivity and specificity. This is of particular importance for systematic efforts that aim to cover the human proteome with different types of binding reagents. One such international program is the SH2-consortium, which was formed to generate a complete set of renewable affinity reagents to the SH2-domain containing human proteins. Here, we describe a microarray strategy to validate various affinity reagents, such as recombinant single-chain antibodies, mouse monoclonal antibodies and antigen-purified polyclonal antibodies using a highly multiplexed approach. An SH2-specific antigen microarray was designed and generated, containing more than 6000 spots displayed by 14 identical subarrays each with 406 antigens, where 105 of them represented SH2-domain containing proteins. Approximately 400 different affinity reagents of various types were analysed on these antigen microarrays carrying antigens of different types. The microarrays revealed not only very detailed specificity profiles for all the binders, but also showed that overlapping target sequences of spotted antigens were detected by off-target interactions. The presented study illustrates the feasibility of using antigen microarrays for integrative, high-throughput validation of various types of binders and antigens.

  13. Use of alumosilicic reagent for water purification

    NASA Astrophysics Data System (ADS)

    Tikhonov, S. N.; Kurchatov, I. M.; Byrkin, V. A.; Feklistov, D. Y.; Laguntsov, N. I.

    2016-09-01

    Workability of the hybrid reagent based on aluminium salts and the use of active silicic acid for the purposes of water treatment was investigated in this paper. The research of the residual aluminium concentration in the water was conducted after the introduction of the reagent into the model solution. The optimum concentration ASFC and the pH value was determined at which the coagulation process is intensified. The approaches of the interaction of the dispersed particles, specified method for calculating the interaction potential of the dispersed particles in the circumstance were described.

  14. Development of C60-based labeling reagents for the determination of low-molecular-weight compounds by matrix assisted laser desorption ionization mass (I): Determination of amino acids in microliter biofluids.

    PubMed

    Wu, Pin; Xiao, Hua-Ming; Ding, Jun; Deng, Qian-Yun; Zheng, Fang; Feng, Yu-Qi

    2017-04-01

    Quantification of low molecular weight compounds (<800 Da) using matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI MS) is challenging due to the matrix signal interference at low m/z region and poor reproducibility of MS responses. In this study, a C60 labeling-MALDI MS strategy was proposed for the fast, sensitive and reliable determination of amino acids (AAs) in biofluids. An N-hydroxysuccinimide functionalized C60 was synthesized as the labeling reagent and added as an 880 Da tag to AAs; a carboxyl acid containing C60 was employed as the internal standards to normalize MS variations. This solved the inherent problems of MALDI MS for small molecule analysis. The entire analytical procedure-which consisted of simple protein precipitation and 10 min of derivatization in a microwave prior to the MALDI MS analysis-could be accomplished within 20 min with high throughput and great sample matrix tolerance. AA quantification showed good linearity from 0.7 to 70.0 μM with correlation coefficients (R) larger than 0.9954. The limits of detection were 70.0-300.0 fmol. Good reproducibility and reliability of the method were demonstrated by intra-day and inter-day precision with relative standard deviations less than 13.8%, and the recovery in biofluid ranged from 80.4% to 106.8%. This approach could be used in 1 μL of urine, serum, plasma, whole blood, and cerebrospinal fluid. Most importantly, the C60 labeling strategy is a universal approach for MALDI MS analysis of various LMW compounds because functionalized C60 is now available on demand.

  15. Sensitive and simple determination of bromate in foods disinfected with hypochlorite reagents using high performance liquid chromatography with post-column derivatization.

    PubMed

    Yokota, Azusa; Kubota, Hiroki; Komiya, Satomi; Sato, Kyoko; Akiyama, Hiroshi; Koshiishi, Ichiro

    2012-11-02

    A novel analytical method for the quantification of bromate in fresh foods using high performance liquid chromatography (HPLC) with a post-column reaction has been developed. The fresh food sample solutions were pretreated with homogenization, centrifugal ultrafiltration and subsequent solid phase extraction using a strong anion-exchange resin. After separation on a strong anion-exchange chromatography column using a highly concentrated NaCl solution (0.3M) as the eluent, the bromate was quantified by detection using a post-column reaction with a non-carcinogenic reagent (tetramethylbenzidine). The developed HPLC technique made it possible to quantify bromate in salt-rich fresh foods. The recoveries from fresh foods spiked with bromate at low levels (2 or 10 ng/g) satisfactorily ranged from 75.3 to 90.7%. The lowest quantification limit in fresh foods was estimated to be 0.6 ng/g as bromic acid. The method should be helpful for the quantification of bromate in fresh foods disinfected with hypochlorite solutions. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. EFFECT OF FENTON'S REAGENT ON SUBSURFACE MICROBIOLOGY AND BIODEGRADATION CAPACITY

    EPA Science Inventory

    Microcosm studies were conducted to determine the effect of Fenton's reagent on subsurface microbiology and biodegradation capacity in a DNAPL (PCE/TCE) contaminated aquifer previously treated with the reagent. Groundwater pH declined from 5 to 2.4 immediately after the treatmen...

  17. EFFECT OF FENTON'S REAGENT ON SUBSURFACE MICROBIOLOGY AND BIODEGRADATION CAPACITY

    EPA Science Inventory

    Microcosm studies were conducted to determine the effect of Fenton's reagent on subsurface microbiology and biodegradation capacity in a DNAPL (PCE/TCE) contaminated aquifer previously treated with the reagent. Groundwater pH declined from 5 to 2.4 immediately after the treatmen...

  18. Radiolabelling, quality control and radiochemical purity assessment of the Octreotide analogue 68Ga DOTA NOC.

    PubMed

    Di Pierro, D; Rizzello, A; Cicoria, G; Lodi, F; Marengo, M; Pancaldi, D; Trespidi, S; Boschi, S

    2008-08-01

    Somatostatin receptors 1-5 are over expressed in neuroendocrine tumours (NETs). 68Ga-labelled [1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid]-1-Nal3-Octreotide (DOTA NOC), a recent synthesized somatostatin analogue, shows high affinity for those receptors. Herein, modifications of a commercial module for the labelling of DOTA NOC with 68Ga, as well as the assessment of time course of the radiochemical purity variation are described. The evaluation of radiochemical stability was done by two different chromatographic methods: reversed-phase radio HPLC and fast TLC analysis. Labelled compound has been found radiochemically stable within 3h from the end of labelling (EOL) and radiochemical purity was always higher than 99%. After 73 labelling sessions the system showed great reproducibility and high radiochemical yield.

  19. Volatile chemical reagent detector

    DOEpatents

    Chen, Liaohai; McBranch, Duncan; Wang, Rong; Whitten, David

    2004-08-24

    A device for detecting volatile chemical reagents based on fluorescence quenching analysis that is capable of detecting neutral electron acceptor molecules. The device includes a fluorescent material, a contact region, a light source, and an optical detector. The fluorescent material includes at least one polymer-surfactant complex. The polymer-surfactant complex is formed by combining a fluorescent ionic conjugated polymer with an oppositely charged surfactant. The polymer-surfactant complex may be formed in a polar solvent and included in the fluorescent material as a solution. Alternatively, the complex may be included in the fluorescent material as a thin film. The use of a polymer-surfactant complex in the fluorescent material allows the device to detect both neutral and ionic acceptor molecules. The use of a polymer-surfactant complex film allows the device and the fluorescent material to be reusable after exposing the fluorescent material to a vacuum for limited time.

  20. Improvement in the degradation resistance of LDPE for radiochemical processing

    NASA Astrophysics Data System (ADS)

    Zaharescu, Traian; Pleşa, Ilona; Jipa, Silviu

    2014-01-01

    The effect of rosemary extract on radiochemical stability of low density polyethylene was studied by chemiluminescence, FT-IR spectroscopy and differential scanning calorimetry after γ(137Cs)-irradiation at processing low doses (10 and 20 kGy) in respect of pristine material. The additive concentrations (1, 2 and 5 wt%) induced a significant improvement in radiation stability, especially at high temperatures, for example 200 °C, which is proved chiefly by lower values of chemiluminescence intensities. The comparison of neat and rosemary-modified LDPE samples has revealed the protection action of this natural extract, which delays efficiently the propagation of oxidative degradation in γ-exposed polyethylene. The most evident proof for antioxidative protection efficiency promoted by rosemary is the smooth changes in hydroxyl and carbonyl indexes calculated on LDPE/5 wt% rosemary samples at all exposure doses.

  1. Radiochemical Reactions Between Tritium Molecule and Carbon Dioxide

    SciTech Connect

    Shu, W.M.; O'Hira, S.; Suzuki, T.; Nishi, M. F.

    2005-07-15

    To have better understanding of radiochemical reactions among oxygen baking products in a fusion reactor, reactions in equimolar tritium molecule (T{sub 2}) and carbon dioxide (CO{sub 2}) were examined by laser Raman spectroscopy and mass spectrometry. After mixing them at room temperature, T{sub 2} and CO{sub 2} decreased rapidly in the first 30 minutes and then the reactions between them became much slower. As the predominant products of the reactions, carbon monoxide (CO) and tritiated water (T{sub 2}O) were found in gaseous phase and condensed phase, respectively. However, there likely existed also some solid products that were thermally decomposed into CO, CO{sub 2}, T{sub 2}, T{sub 2}O, etc. during baking up to 523 K.

  2. Handling of Ammonium Nitrate Mother-Liquid Radiochemical Production - 13089

    SciTech Connect

    Zherebtsov, Alexander; Dvoeglazov, Konstantine; Volk, Vladimir; Zagumenov, Vladimir; Zverev, Dmitriy; Tinin, Vasiliy; Kozyrev, Anatoly; Shamin, Dladimir; Tvilenev, Konstantin

    2013-07-01

    The aim of the work is to develop a basic technology of decomposition of ammonium nitrate stock solutions produced in radiochemical enterprises engaged in the reprocessing of irradiated nuclear fuel and fabrication of fresh fuel. It was necessary to work out how to conduct a one-step thermal decomposition of ammonium nitrate, select and test the catalysts for this process and to prepare proposals for recycling condensation. Necessary accessories were added to a laboratory equipment installation decomposition of ammonium nitrate. It is tested several types of reducing agents and two types of catalyst to neutralize the nitrogen oxides. It is conducted testing of modes of the process to produce condensation, suitable for use in the conversion of a new technological scheme of production. It is studied the structure of the catalysts before and after their use in a laboratory setting. It is tested the selected catalyst in the optimal range for 48 hours of continuous operation. (authors)

  3. Radiochemical analyses of several spent fuel Approved Testing Materials

    SciTech Connect

    Guenther, R.J.; Blahnik, D.E.; Wildung, N.J.

    1994-09-01

    Radiochemical characterization data are described for UO{sub 2} and UO{sub 2} plus 3 wt% Gd{sub 2}O{sub 3} commercial spent nuclear fuel taken from a series of Approved Testing Materials (ATMs). These full-length nuclear fuel rods include MLA091 of ATM-103, MKP070 of ATM-104, NBD095 and NBD131 of ATM-106, and ADN0206 of ATM-108. ATMs 103, 104, and 106 were all irradiated in the Calvert Cliffs Nuclear Power Plant (Reactor No.1), a pressurized-water reactor that used fuel fabricated by Combustion Engineering. ATM-108 was part of the same fuel bundle designed as ATM-105 and came from boiling-water reactor fuel fabricated by General Electric and irradiated in the Cooper Nuclear Power Plant. Rod average burnups and expected fission gas releases ranged from 2,400 to 3,700 GJ/kgM. (25 to 40 Mwd/kgM) and from less than 1% to greater than 10%, respectively, depending on the specific ATM. The radiochemical analyses included uranium and plutonium isotopes in the fuel, selected fission products in the fuel, fuel burnup, cesium and iodine on the inner surfaces of the cladding, {sup 14}C in the fuel and cladding, and analyses of the gases released to the rod plenum. Supporting examinations such as fuel rod design and material descriptions, power histories, and gamma scans used for sectioning diagrams are also included. These ATMs were examined as part of the Materials Characterization Center Program conducted at Pacific Northwest Laboratory provide a source of well-characterized spent fuel for testing in support of the US Department of Energy Office of Civilian Radioactive Waste Management Program.

  4. Determination of alternative and conventional chelating agents as copper(II) complexes by capillary zone electrophoresis--the first use of didecyldimethylammonium bromide as a flow reversal reagent.

    PubMed

    Laamanen, Pirkko-Leena; Matilainen, Rose

    2007-02-12

    A capillary zone electrophoresis (CZE) method for analyzing 11 chelating agents [beta-alaninediacetic acid (beta-ADA), trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid (HEDTA), N-(2-hydroxyethyl)iminodiacetic acid (HEIDA), iminodiacetic acid (IDA), methylglycinediacetic acid (MGDA), nitrilotriacetic acid (NTA), 1,3-diaminopropane-N,N,N',N'-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)] as negatively charged copper(II) complexes has been established. Both conventional and alternative chelating agents were included in this study, because they are used side by side in industrial applications. In this study, didecyldimethylammonium bromide (DMDDAB) was successfully used as a flow reversal reagent for the first time in an aqueous CZE method based on phosphate BGE with UV spectrophotometric detection. In addition this new flow modifier was compared to common TTAB. Method development was done using a fused silica capillary (61 cm x 50 microm i.d.). The optimized BGE was a 105 mmol L(-1) phosphate buffer with TTAB or DMDDAB in the concentration 0.5 mmol L(-1) at pH 7.1. The measurements were done with -20 kV voltage using direct UV detection at 254 nm. In both CZE methods all 11 analyte zones were properly separated (resolutions > or =2.4), and the calibrations gave excellent correlation coefficients (> or =0.998; linear range tested 0.5-2.0 mmol L(-1)). The limits of detection were < or =34 and < or =49 micromol L(-1) with the method of DMDDAB and TTAB, respectively. A clear benefit of both methods was the short analysis time; all 11 complexes were detected in less than 6 and 5.5 min with the methods of TTAB and DMDDAB, respectively. The two methods were tested with dishwashing detergents and paper mill wastewater samples and proved to be suitable for practical use.

  5. A stabilizing reagent prevents cell-free DNA contamination by cellular DNA in plasma during blood sample storage and shipping as determined by digital PCR.

    PubMed

    Norton, S E; Lechner, J M; Williams, T; Fernando, M R

    2013-10-01

    To study the ability of a stabilizing reagent to prevent cellular DNA contamination of cell-free DNA (cfDNA) in plasma during whole blood sample storage and shipping. Samples were drawn from healthy donors into K₃EDTA and Cell-Free DNA BCTs (BCT) and stored at room temperature (RT). Aliquots were removed at specified time points and cfDNA was purified from the plasma. A Droplet Digital PCR (ddPCR) assay that amplifies a short β-actin gene fragment (136 bp) was used to measure the total plasma cfDNA (pDNA) concentration while a longer β-actin fragment (420 bp) was used to quantify genomic DNA (gDNA). In a follow-up experiment, blood samples drawn into the same types of tubes were shipped round trip by overnight air before cfDNA was isolated and analyzed. Blood stored in K₃EDTA tubes at RT showed increases in pDNA and gDNA concentrations over time. However, both pDNA and gDNA levels remained stable in BCT for at least seven days. On day 14, there was a 4.5-fold increase in pDNA in BCT as compared to >200-fold increase in K₃EDTA tubes. Likewise, gDNA increased <2-fold on day 14 in BCT as opposed to a 456-fold increase in K₃EDTA tubes. Similar results were observed after samples were shipped. Cell-Free DNA BCTs prevent gDNA contamination that may occur due to nucleated cell disruption during sample storage and shipping. This novel blood collection tube provides a method for obtaining stable cfDNA samples for rare target detection and accurate analysis while mitigating the threat of gDNA contamination. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

  6. Complex amine-based reagents

    NASA Astrophysics Data System (ADS)

    Suslov, S. Yu.; Kirilina, A. V.; Sergeev, I. A.; Zezyulya, T. V.; Sokolova, E. A.; Eremina, E. V.; Timofeev, N. V.

    2017-03-01

    Amines for a long time have been applied to maintaining water chemistry conditions (WCC) at power plants. However, making use of complex reagents that are the mixture of neutralizing and the filmforming amines, which may also contain other organic components, causes many disputes. This is mainly due to lack of reliable information about these components. The protective properties of any amine with regard to metal surfaces depend on several factors, which are considered in this article. The results of applying complex reagents to the protection of heating surfaces in industrial conditions and estimated behavior forecasts for various reagents under maintaining WCC on heat-recovery boilers with different thermal circuits are presented. The case of a two-drum heat-recovery boiler with in-line drums was used as an example, for which we present the calculated pH values for various brands of reagents under the same conditions. Work with different reagent brands and its analysis enabled us to derive a composition best suitable for the conditions of their practical applications in heat-recovery boilers at different pressures. Testing the new amine reagent performed at a CCPP power unit shows that this reagent is an adequate base for further development of reagents based on amine compounds. An example of testing a complex reagent is shown created with the participation of the authors within the framework the program of import substitution and its possible use is demonstrated for maintaining WCC of power-generating units of combined-cycle power plants (CCPP) and TPP. The compliance of the employed reagents with the standards of water chemistry conditions and protection of heating surfaces were assessed. The application of amine-containing reagents at power-generating units of TPP makes it possible to solve complex problems aimed at ensuring the sparing cleaning of heating surfaces from deposits and the implementation of conservation and management of water chemistry condition

  7. Fluxes of metals to a manganese nodule: Radiochemical, chemical, structural, and mineralogical studies

    USGS Publications Warehouse

    Moore, W.S.; Ku, T.-L.; Macdougall, J.D.; Burns, V.M.; Burns, R.; Dymond, J.; Lyle, M.W.; Piper, D.Z.

    1981-01-01

    Fluxes of metals to the top and bottom surfaces of a manganese nodule were determined by combining radiochemical (230Th, 231Pa, 232Th, 238U, 234U) and detailed chemical data. The top of the nodule had been growing in its collected orientation at 4.7 mm Myr-1 for at least 0.5 Myr and accreting Mn at 200 ??g cm-2 kyr-1. The bottom of the nodule had been growing in its collected orientation at about 12 mm Myr-1 for at least 0.3 Myr and accreting Mn at about 700 ??g cm-2 yr-1. Although the top of the nodule was enriched in iron relative to the bottom, the nodule had been accreting Fe 50% faster on the bottom. 232Th was also accumulating more rapidly in the bottom despite a 20-fold enrichment of 230Th on the top. The distribution of alpha-emitting nuclides calculated from detailed radiochemical measurements matched closely the pattern revealed by 109-day exposures of alpha-sensitive film to the nodule. However, the shape and slope of the total alpha profile with depth into the nodule was affected strongly by 226Ra and 222Rn migrations making the alpha-track technique alone an inadequate method of measuring nodule growth rates. Diffusion of radium in the nodule may have been affected by diagenetic reactions which produce barite, phillipsite and todorokite within 1 mm of the nodule surface; however, our sampling interval was too broad to document the effect. We have not been able to resolve the importance of nodule diagenesis on the gross chemistry of the nodule. ?? 1981.

  8. RAPID RADIOCHEMICAL ANALYSES IN SUPPORT OF FUKUSHIMA NUCLEAR ACCIDENT

    SciTech Connect

    Maxwell, S.

    2012-11-07

    There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and data assessment teams were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90} Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed

  9. Rapid Radiochemical Analyses in Support of Fukushima Nuclear Accident - 13196

    SciTech Connect

    Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

    2013-07-01

    There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples [1, 2]. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and data assessment teams were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90}Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation [3, 4]. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride

  10. Radiochemical synthesis of a carbon-supported Pt-SnO2 bicomponent nanostructure exhibiting enhanced catalysis of ethanol oxidation

    NASA Astrophysics Data System (ADS)

    Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi; Kugai, Junichiro; Ohkubo, Yuji; Akita, Tomoki; Nitani, Hiroaki; Yamamoto, Takao A.

    2015-03-01

    Carbon-supported Pt-SnO2 electrocatalysts with various Sn/Pt molar ratios were prepared by an electron beam irradiation method. These catalysts were composed of metallic Pt particles approximately 5 nm in diameter together with low crystalline SnO2. The contact between the Pt and SnO2 in these materials varied with the amount of dissolved oxygen in the precursor solutions and it was determined that intimate contact between the Pt and SnO2 significantly enhanced the catalytic activity of these materials during the ethanol oxidation reaction. The mechanism by which the contact varies is discussed based on the radiochemical reduction process.

  11. Chemical speciation and recovery of gold(I, III) from wastewater and silver by liquid-liquid extraction with the ion-pair reagent amiloride mono hydrochloride and AAS determination.

    PubMed

    El-Shahawi, M S; Bashammakh, A S; Bahaffi, S O

    2007-06-15

    A novel and low cost liquid-liquid extraction procedure for the separation of gold(III) at trace level from aqueous medium of pH 5-9 has been developed. The method has been based upon the formation of a yellow colored ternary complex ion associate of tetrachloro gold(III) complex anion, AuCl(4)(-) with the ion-pair reagent 1-(3,5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride, DPG(+).Cl(-). The effect of various parameters, e.g. pH, organic solvent, shaking time, etc. on the preconcentration of gold(III) from the aqueous media by the DPG(+).Cl(-) reagent has been investigated. The colored gold species was quantitatively extracted into 4-methyl pentan-2-one. The chemical composition of the ion associate of DPG(+).Cl(-) with AuCl(4)(-) in the organic solvent has been determined by the Job's method. The molar absorptivity (2.19x10(4)Lmol(-1)cm(-1)) of the associate DPG(+).AuCl(4)(-) at 362nm enabled a convenient application of the developed extraction procedure for the separation and AAS determination of traces of aurate ions. Mono-valence gold ions after oxidation to gold(III) with bromine water in HCl (1.0molL(-1)) media have been also extracted quantitatively from the aqueous media by the developed procedure. The chemical speciation of mono- and/or tri-valence gold species spiked to fresh and industrial wastewater samples has been achieved. The method has been also applied successfully from the separation of gold(I) and gold(III) species from metallic ions and silver. The developed method has also the advantage of freedom from most diverse ions.

  12. Recyclable Trifluoromethylation Reagents from Fluoroform.

    PubMed

    Geri, Jacob B; Szymczak, Nathaniel K

    2017-07-26

    We present a strategy to rationally prepare CF3(-) transfer reagents at ambient temperature from HCF3. We demonstrate that a highly reactive CF3(-) adduct can be synthesized from alkali metal hydride, HCF3, and borazine Lewis acids in quantitative yield at room temperature. These nucleophilic reagents transfer CF3(-) to substrates without additional chemical activation, and after CF3 transfer, the free borazine is quantitatively regenerated. These features enable syntheses of popular nucleophilic, radical, and electrophilic trifluoromethylation reagents with complete recycling of the borazine Lewis acid.

  13. Reaction rates between water and some modified rapidly-reacting Karl Fischer reagents.

    PubMed

    Cedergren, A

    1978-04-01

    Rate constants were determined for the reaction between water and various modified Karl Fischer reagents containing formamide, dimethylformamide or N-methylformamide. It was shown that the reaction rate can be increased by a factor of 100 by using a reagent containing 40% v/v formamide in pyridine compared to that obtained by use of the conventional methanolic reagent.

  14. Waste treatment at the Radiochemical Engineering Development Center

    SciTech Connect

    Brunson, R.R.; Bond, W.D.; Chattin, F.R.; Collins, R.T.; Sullivan, G.R.; Wiles, R.H.

    1997-12-31

    At the Radiochemical Engineering Development Center (REDC) irradiated targets are processed for the recovery of valuable radioisotopes, principally transuranium nuclides. A system was recently installed for treating the various liquid alkaline waste streams for removal of excess radioactive contaminants at the REDC. Radionuclides that are removed will be stored as solids and thus the future discharge of radionuclides to liquid low level waste tank storage will be greatly reduced. The treatment system is of modular design and is installed in a hot cell (Cubicle 7) in Building 7920 at the REDC where preliminary testing is in progress. The module incorporates the following: (1) a resorcinol-formaldehyde resin column for Cs removal, (2) a cross flow filtration unit for removal of rare earths and actinides as hydroxide, and (3) a waste solidification unit. Process flowsheets for operation of the module, key features of the module design, and its computer-assisted control system are presented. Good operability of the cross flow filter system is mandatory to the successful treatment of REDC wastes. Results of tests to date on the operation of the filter in its slurry collection mode and its slurry washing mode are presented. These tests include the effects of entrained organic solvent in the waste stream feed to the filter.

  15. In-situ ionic liquid dispersive liquid-liquid microextraction using a new anion-exchange reagent combined Fe3O4 magnetic nanoparticles for determination of pyrethroid pesticides in water samples.

    PubMed

    Fan, Chen; Liang, You; Dong, Hongqiang; Ding, Guanglong; Zhang, Wenbing; Tang, Gang; Yang, Jiale; Kong, Dandan; Wang, Deng; Cao, Yongsong

    2017-07-04

    In this work, in-situ ionic liquid dispersive liquid-liquid microextraction combined ultrasmall Fe3O4 magnetic nanoparticles was developed as a kind of pretreatment method to detect pyrethroid pesticides in water samples. New anion-exchange reagents including Na[DDTC] and Na[N(CN)2] were optimized for in-situ extraction pyrethroids, which showed enhanced microextraction performance. Pyrethroids were enriched by hydrophilic ionic liquid [P4448][Br] (aqueous solution, 200 μL, 0.2 mmol mL(-1)) reaction in-situ with anion-exchange reagent Na[N(CN)2] (aqueous solution, 300 μL, 0.2 mmol mL(-1)) forming hydrophobic ionic liquid as extraction agent in water sample (10 mL). Ultrasmall superparamagnetic iron oxide nanoparticles (30 mg) were used to collect the mixture of ionic liquid and pyrethroids followed by elution with acetonitrile. The extraction of ionic liquid strategies was unique and efficiently fulfilled with high enrichment factors (176-213) and good recoveries (80.20-117.31%). The method was successively applied to the determination of pyrethroid pesticides in different kinds of water samples with the limits of detection ranged from 0.16 to 0.21 μg L(-1). The proposed method is actually nanometer-level microextraction (average size 80 nm) with the advantages of simplicity, rapidity, and sensitivity. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Inorganic and Radiochemical Analysis of AW-101 and AN-107 ''Diluted Feed'' Materials

    SciTech Connect

    MW Urie; JJ Wagner; LR Greenwood; OT Farmer; SK Fiskum; RT Ratner; CZ Soderquist

    1999-11-11

    This report presents the inorganic and radiochemical analytical results for AW-101 and AN-107 diluted feed materials. The analyses were conducted in support of the BNFL Proposal No. 29952/29953 Task 2.1. The inorganic and radiochemical analysis results obtained from the diluted feed materials are used to provide initial characterization information for subsequent processing testing. Quality Assurance (QA) Plan MCS-033 provides the operational and quality control protocols for the analytical activities.

  17. Summary Report of two-Dimensional Analysis of Radiochemical Assay Samples

    SciTech Connect

    C. Connell; J.M. Scaglione

    2001-12-03

    The ''Summary Report of Two-Dimensional Analysis of Radiochemical Assay Samples'' report provides a summary of the analyses comparing calculated isotopics generated by a point-depletion code that uses one-dimensional (1-D) neutron transport theory weighted cross-sections (SAS2H Control Module of the SCALE Modular Code System) and a two-dimensional (2-D) depletion code (GRCASMO3) with that of radiochemical assay (RCA) results.

  18. A radiochemical analysis developed by using sorption isolation of microcomponents to meet radioecological monitoring problems

    SciTech Connect

    Betenekov, N.D.; Denisov, E.I.; Egorov, Yu.V.

    1993-12-31

    The present report considers the main stages involved in the development of radiochemical analysis methods for natural waters, making use of the sorption isolation of uranium, plutonium, cesium, strontium, and rare earth elements radionuclides by thin-layer inorganic sorbents from samples of large volume in field conditions. The techniques developed are original, rapid, and simple to perform. A model of device designed to realize the radiochemical analysis is suggested.

  19. Flow injection spectrophotometric determination of sub-mg dm(-3) silver(I) in a strongly acidic solution containing concentrated copper(II) using a pyridylazo reagent.

    PubMed

    Fujimura, Kazuyoshi; Odake, Tamao; Takiguchi, Hiromi; Watanabe, Noriyuki; Sawada, Tsuguo

    2011-01-01

    A novel spectrophotometric flow injection method for determination of silver(I) in a strongly acidic solution containing concentrated copper(II) was developed using a coloring ligand, 4-(3,5-dibromo-2-pyridylazo)-N-ethyl-N-(3-sulfopropyl)aniline (3,5-diBr-PAESA). The method was first investigated by batch method. The interference from copper(II) chelate could be eliminated by the masking effect of EDTA. By utilizing the large formation constant (K = 12.3) of AgBr, one could determine silver(I) as a decrease of absorption by silver(I) chelate due to formation of AgBr by addition of KBr. Based on the results of batch experiments, two types of flow injection analysis (FIA) systems were constructed. Sub-mg dm(-3) determination of silver(I) was attained without interference from excess copper(II). The proposed method was successfully applied to determination of silver in a copper plating solution used in a plant to manufacture copper printed circuit boards, where the concentration of silver was critically important in the process control.

  20. Radiochemical ageing of EPDM elastomers.. 2. Identification and quantification of chemical changes in EPDM and EPR films γ-irradiated under oxygen atmosphere

    NASA Astrophysics Data System (ADS)

    Rivaton, A.; Cambon, S.; Gardette, J.-L.

    2005-01-01

    This paper is devoted to the identification and quantification of the main chemical changes resulting from the radiochemical ageing under oxygen atmosphere of ethylene-propylene-diene monomer (EPDM) and ethylene-propylene rubber (EPR) films containing the same molar ratio of ethylene/propylene. IR and UV-Vis analysis showed that radiooxidation produces a complex mixture of different products and provokes the consumption of the diene double bond. The radiochemical yields of formation of ketones, carboxylic acids, hydroperoxides and alcohols were determined by combining IR analysis with derivatisation reactions and chemical titration. The contributions of secondary and tertiary structures of these two types of -OH groups were separated. Esters and γ-lactones were formed in low concentration. The oxidation products distribution in irradiated films was determined by micro-FTIR spectroscopy. Crosslinking was evaluated by gel fraction methods. In complement, the gas phase composition was analysed by mass spectrometry.

  1. Comparison of the sensitivity of commercial APTT reagents in the detection of mild coagulopathies.

    PubMed

    Marlar, R A; Bauer, P J; Endres-Brooks, J L; Montgomery, R R; Miller, C M; Schanen, M M

    1984-10-01

    This study was undertaken to evaluate the precision and sensitivity of three different commercial APTT reagents containing the activators kaolin, micronized silica, or ellagic acid. These reagents varied greatly in their ability to detect mild coagulopathies. The ellagic acid reagent was able to detect the mildest deficiencies for the most common coagulopathies. This reagent was sensitive to 50% levels of Factor VIIIC, whereas the APTT with the kaolin reagent was not prolonged until levels of 35% or less were attained. The micronized silica reagent was the least sensitive to Factor IX deficiency, detecting levels of 12% or less. Precision was similar for all reagents when tested with normal and slightly abnormal plasmas. Since methods and instrumentation vary, each laboratory should evaluate their APTT reagent to determine its precision and sensitivity.

  2. DABTZ as a new reagent for solid phase extraction and spectrophotometric determination of trace amount of Hg(II) in water sample.

    PubMed

    Soleimani, Majid; Morsali, Ali; Khani, Azam

    2007-01-01

    A novel sensitive and simple method for rapid and selective extraction, preconcentration and determination of mercury as its 2,2' diamino-4,4' bithiazole (DABTZ) complex by using octadecylsilica cartridges and spectrophotometry is presented. Extraction efficiency and the influence of flow rates of sample solution and eluent, pH, amount of DABTZ, type and least amount of eluent for elution of mercury complex from cartridges, break through volume and limit of detection were evaluated. Also the effects of various cationic and anionic interferences on percent recovery of mercury were studied. Average extraction efficiency > 90% was obtained by elution of the cartridge with minimal amount of solvent in the presence of interferences. A preconcentration factor of 152 and a detection limit of 10.92 ng mL(-1) were obtained. The method was applied to the recovery and determination of mercury in different water samples.

  3. Determination of Ammonium in Aqueous Samples by Gas Phase Light Scattering Using Hydrogen Chloride Gas as a Derivatizing Reagent Followed by Nondispersive Atomic Fluorescence Spectrometry.

    PubMed

    Duan, Xuchuan; Fang, Jinliang; Sun, Rui

    2017-01-01

    A sensitive method was developed for the determination of ammonium in an aqueous solution based on gas phase light scattering. In a stream of carrier gas, the gaseous ammonia from the alkalized solution formed a volatile ammonium chloride derivative by reacting with gaseous hydrogen chloride; the gaseous ammonium chloride was analyzed by nondispersive atomic fluorescence spectrometry. The mechanisms of the method are elucidated based on evaporative light scattering detection. Parameters such as temperature, amount of sodium hydroxide, and carrier gas flow rate were studied. Under optimal conditions, the detection limit of ammonium-nitrogen was 0.045 μg. The method was successfully applied to the determination of ammonium in certified reference materials, and tap and seawater samples.

  4. Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples.

    PubMed

    Suvardhan, K; Rekha, D; Kumar, K Suresh; Prasad, P Reddy; Kumar, J Dilip; Jayaraj, B; Chiranjeevi, P

    2007-06-01

    Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 degrees C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ngml(-1). The extraction efficiency was investigated at different nickel concentrations (20-80 ngml(-1)) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level.

  5. Utility of 7,7,8,8-tetracyanoquinodimethane charge transfer reagent for the spectrophotometric determination of trazodone, amineptine and amitriptyline hydrochlorides

    NASA Astrophysics Data System (ADS)

    Mohamed, Gehad G.; El-Dien, Faten A. F. Nour; Mohamed, Nehad A.

    2007-12-01

    A simple and rapid spectrophotometric method has been developed for the determination of tricyclic anti-depressant drugs such as trazodone (TZH), amineptine (APH) and amitriptyline (ATPH) hydrochlorides in pure form and in different pharmaceutical preparations. The charge transfer (CT) reaction between TZH, APH and ATPH as electron donors and TCNQ as electron acceptor was utilized for their spectrophotometric determination. The optimum experimental conditions, like time, temperature, stoichiometry, solvents, for the CT complex formation are established. The method permits the determination of TZH, APH and ATPH over a concentration range of 10-400, 10-440 and 10-300 μg ml -1, respectively. The sensitivity ( S) is found to be 0.09, 0.087 and 0.069 g cm -2 for TZH, APH and ATPH, respectively. The SD values are found to be 0.146-0.293, 0.154-0.285 and 0.091-0.212 and RSD values are 0.142-1.92, 0.297-1.92 and 0.212-0.915 for TZH, APH and ATPH, respectively. The low values of the relative standard deviation indicate the high accuracy and precision of the method. The mean recovery values obtained together with a high correlation coefficient values, amount in the range 98-101.5, 98.7-102.9 and 93-101.9 for TZH, APH and ATPH, respectively. The method is applicable for the assay of the investigated drugs in different dosage forms and the results are in good agreement with those obtained by the official method.

  6. Utility of eosin Y as a complexing reagent for the determination of citalopram hydrobromide in commercial dosage forms by fluorescence spectrophotometry.

    PubMed

    Azmi, Syed Najmul Hejaz; Al-Fazari, Ahlam; Al-Badaei, Munira; Al-Mahrazi, Ruqiya

    2015-12-01

    An accurate, selective and sensitive spectrofluorimetric method was developed for the determination of citalopram hydrobromide in commercial dosage forms. The method was based on the formation of a fluorescent ion-pair complex between citalopram hydrobromide and eosin Y in the presence of a disodium hydrogen phosphate/citric acid buffer solution of pH 3.4 that was extractable in dichloromethane. The extracted complex showed fluorescence intensity at λem = 554 nm after excitation at 259 nm. The calibration curve was linear over at concentrations of 2.0-26.0 µg/mL. Under optimized experimental conditions, the proposed method was validated as per ICH guidelines. The effect of common excipients used as additives was tested and the tolerance limit calculated. The limit of detection for the proposed method was 0.121 μg/mL. The proposed method was successfully applied to the determination of citalopram hydrobromide in commercial dosage forms. The results were compared with the reference RP-HPLC method. Copyright © 2015 John Wiley & Sons, Ltd.

  7. Hydroxyamidines as new extracting reagents for spectrophotometric determination of cadmium with 4-(2-pyridylazo)naphthol in industrial effluents, coal, and fly ash

    SciTech Connect

    Chakravarty, S.; Deb, M.K.; Mishra, R.K. )

    1993-05-01

    A simple, sensitive, and selective extractive spectrophotometric method for the determination of cadmium in trace quantities with N1-hydroxy-N1,N2-diphenylbenzamidine (HDPBA) and 4-(2-pyridylazo)naphthol (PAN) is described. The method is based on the extraction of cadmium with HDPBA into chloroform at pH 9.0 +/- 0.2 and simultaneous spectrophotometric determination with PAN. The binary Cd(II)-HDPBA complex extracted into chloroform has a molar absorptivity of 1.96 x 10(4) L/mol/cm at lambda max 400 nm. The sensitivity of the yellow Cd(II)-HDPBA complex was increased remarkably by the addition of PAN to the binary complex. With 6 different hydroxyamidines tested, the red-orange complex in chloroform exhibited maximum absorbance at 530-550 nm, with molar absorptivity values of 3.2-5.6 x 10(4) L/mol/cm. The method adheres to Beer's law up to 1.5 micrograms cadmium/mL organic phase. The detection limit of the method is 0.02 micrograms Cd/mL. Investigations of the effect of foreign ions revealed that the present method is free from matrix interference of most of the common ions (e.g., Fe(III), Ni(II), Cu(II), Mn(II), V(V), Co(II), Al(III), Cu(II), Mg(II), and Mo(VI)). The relative standard deviation for 10 repetitive analyses of the metal was 1.4%. The validity of the method was tested successfully with various environmental samples.

  8. Hydroxyamidines as new extracting reagents for spectrophotometric determination of cadmium with 4-(2-pyridylazo)naphthol in industrial effluents, coal, and fly ash.

    PubMed

    Chakravarty, S; Deb, M K; Mishra, R K

    1993-01-01

    A simple, sensitive, and selective extractive spectrophotometric method for the determination of cadmium in trace quantities with N1-hydroxy-N1,N2-diphenylbenzamidine (HDPBA) and 4-(2-pyridylazo)naphthol (PAN) is described. The method is based on the extraction of cadmium with HDPBA into chloroform at pH 9.0 +/- 0.2 and simultaneous spectrophotometric determination with PAN. The binary Cd(II)-HDPBA complex extracted into chloroform has a molar absorptivity of 1.96 x 10(4) L/mol/cm at lambda max 400 nm. The sensitivity of the yellow Cd(II)-HDPBA complex was increased remarkably by the addition of PAN to the binary complex. With 6 different hydroxyamidines tested, the red-orange complex in chloroform exhibited maximum absorbance at 530-550 nm, with molar absorptivity values of 3.2-5.6 x 10(4) L/mol/cm. The method adheres to Beer's law up to 1.5 micrograms cadmium/mL organic phase. The detection limit of the method is 0.02 micrograms Cd/mL. Investigations of the effect of foreign ions revealed that the present method is free from matrix interference of most of the common ions (e.g., Fe(III), Ni(II), Cu(II), Mn(II), V(V), Co(II), Al(III), Cu(II), Mg(II), and Mo(VI)). The relative standard deviation for 10 repetitive analyses of the metal was 1.4%. The validity of the method was tested successfully with various environmental samples.

  9. The determination of psilocin and psilocybin in hallucinogenic mushrooms by HPLC utilizing a dual reagent acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection system.

    PubMed

    Anastos, Nicole; Lewis, Simon W; Barnett, Neil W; Sims, D Noel

    2006-01-01

    This paper describes a procedure for the determination of psilocin and psilocybin in mushroom extracts using high-performance liquid chromatography with postcolumn chemiluminescence detection. A number of extraction methods for psilocin and psilocybin in hallucinogenic mushrooms were investigated, with a simple methanolic extraction being found to be most effective. Psilocin and psilocybin were extracted from a variety of hallucinogenic mushrooms using methanol. The analytes were separated on a C12 column using a (95:5% v/v) methanol:10 mM ammonium formate, pH 3.5 mobile phase with a run time of 5 min. Detection was realized through a dual reagent chemiluminescence detection system of acidic potassium permanganate and tris(2,2'-bipyridyl)ruthenium(II). The chemiluminescence detection system gave improved detectability when compared with UV absorption at 269 nm, with detection limits of 1.2 x 10(-8) and 3.5 x 10(-9) mol/L being obtained for psilocin and psilocybin, respectively. The procedure was applied to the determination of psilocin and psilocybin in three Australian species of hallucinogenic mushroom.

  10. Sensitive determination of carnosine in urine by high-performance liquid chromatography using 4-(5,6-dimethoxy-2-phthalimidinyl)-2-methoxyphenylsulfonyl chloride as a fluorescent labeling reagent.

    PubMed

    Tsuruta, Yasuto; Maruyama, Kiyoshi; Inoue, Hirofumi; Kosha, Keiko; Date, Yuuko; Okamura, Nobuyuki; Eto, Seiji; Kojima, Eijiro

    2010-02-01

    A simple and highly sensitive high-performance liquid chromatography procedure was developed for the determination of carnosine in urine. Carnosine was derivatized with 4-(5,6-dimethoxy-2-phthalimidinyl)-2-methoxyphenylsulfonyl chloride at 70 degrees C for 15 min in borate buffer (20 mmol l(-1), pH 9.0) to produce fluorescent sulfonamides. After hydrolysis of the reaction mixture with formic acid at 100 degrees C for 15 min, the fluorescent derivative of carnosine was separated on a reversed-phase column with a linear gradient elution using solvents of (A) acetate buffer (0.1 mmol l(-1), pH 7.0) and (B) acetonitrile at a flow-rate of 1.0 ml/min and was detected at excitation and emission wavelengths of 318 and 400 nm, respectively. The detection limit of carnosine was 4 fmol at a signal-to-noise ratio of 3. The within-day and day-to-day relative standard deviations were 2.7-4.6% and 0.4-5.2%, respectively. The concentration of carnosine in normal human urine was found to be 4.6-125 nmol (mg creatinine)(-1) (mean+/-SD: 21.6+/-26.6 nmol (mg creatinine)(-1), n=20). 2009 Elsevier B.V. All rights reserved.

  11. Radiochemical Assays of Irradiated VVER-440 Fuel for Use in Spent Fuel Burnup Credit Activities

    SciTech Connect

    Jardine, L J

    2005-04-25

    The objective of this spent fuel burnup credit work was to study and describe a VVER-440 reactor spent fuel assembly (FA) initial state before irradiation, its operational irradiation history and the resulting radionuclide distribution in the fuel assembly after irradiation. This work includes the following stages: (1) to pick out and select a specific spent (irradiated) FA for examination; (2) to describe the FA initial state before irradiation; (3) to describe the irradiation history, including thermal calculations; (4) to examine the burnup distribution of select radionuclides along the FA height and cross-section; (5) to examine the radionuclide distributions; (6) to determine the Kr-85 release into the plenum; (7) to select and prepare FA rod specimens for destructive examinations; (8) to determine the radionuclide compositions, isotope masses and burnup in the rod specimens; and (9) to analyze, document and process the results. The specific workscope included the destructive assay (DA) of spent fuel assembly rod segments with an {approx}38.5 MWd/KgU burnup from a single VVER-440 fuel assembly from the Novovorenezh reactor in Russia. Based on irradiation history criteria, four rods from the fuel assembly were selected and removed from the assembly for examination. Next, 8 sections were cut from the four rods and sent for destructive analysis of radionuclides by radiochemical analyses. The results were documented in a series of seven reports over a period of {approx}1 1/2 years.

  12. Using Safranin T as a Charge Transfer-Sensitive Ion-Pairing Reagent in Ultrasound-Assisted Cloud Point Extraction: Determination of Bisphenol A in Selected Beverages.

    PubMed

    Temel, Nuket Kartal; Gürkan, Ramazan

    2017-08-02

    In this study, a new ultrasonic-assisted cloud point extraction method coupled with spectrophotometry was developed to extract from and determine bisphenol A (BPA) in a sample matrix. The method is based on charge transfer-sensitive ion-pairing complex formation between BPA and Safranin T in the presence of nitrate in a micellar interface at pH 5.0. The variables affecting extraction efficiency were optimized. A good linear relationship with a significant sensitivity difference was obtained in the ranges of 2-40 and 2-120 µg/L with LODs of 0.54 and 0.38 µg/L after preconcentration with two different extractants, respectively. From a preconcentration of a 15 mL sample, a preconcentration factor of 60 was obtained. Due to the lack of a certified material compatible with the sample matrix, the method was validated by conducting intraday and interday accuracy and precision studies based on two spiked QC samples (with a recovery rate greater than 94% and an RSD ranging from 3.8 to 5.9%). Moreover, the beverage samples were analyzed by the standard addition method to control for possible matrix effects. BPA was detected in the range of 1.8-7.2 µg/L in beverages with Triton X-114, whereas the levels changed to a range of 1.8-7.3 µg/L with Triton X-45. In such a way not to create a threat, these levels were considerably lower than the specific migration limit set by the European Union.

  13. 21 CFR 1271.210 - Supplies and reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... supply or reagent, or by the vendor of the supply or reagent. (b) Reagents. Reagents used in processing... supply or reagent, including the type, quantity, manufacturer, lot number, date of receipt, and...

  14. Chemical Amplification with Encapsulated Reagents

    NASA Technical Reports Server (NTRS)

    Chen, Jian; Koemer, Steffi; Craig, Stephen; Lin, Shirley; Rudkevich, Dmitry M.; Rebek, Julius, Jr.

    2002-01-01

    Autocatalysis and chemical amplification are characteristic properties of living systems, and they give rise to behaviors such as increased sensitivity, responsiveness, and self-replication. Here we report a synthetic system in which a unique form of compartmentalization leads to nonlinear, autocatalytic behavior. The compartment is a reversibly formed capsule in which a reagent is sequestered. Reaction products displace the reagent from the capsule into solution and the reaction rate is accelerated. The resulting self-regulation is sensitive to the highly selective molecular recognition properties of the capsule.

  15. Chemical Amplification with Encapsulated Reagents

    NASA Technical Reports Server (NTRS)

    Chen, Jian; Koemer, Steffi; Craig, Stephen; Lin, Shirley; Rudkevich, Dmitry M.; Rebek, Julius, Jr.

    2002-01-01

    Autocatalysis and chemical amplification are characteristic properties of living systems, and they give rise to behaviors such as increased sensitivity, responsiveness, and self-replication. Here we report a synthetic system in which a unique form of compartmentalization leads to nonlinear, autocatalytic behavior. The compartment is a reversibly formed capsule in which a reagent is sequestered. Reaction products displace the reagent from the capsule into solution and the reaction rate is accelerated. The resulting self-regulation is sensitive to the highly selective molecular recognition properties of the capsule.

  16. Validation of a reverse-phase high-performance liquid chromatography method for the determination of amino acids in gelatins by application of 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate reagent.

    PubMed

    Azilawati, M I; Hashim, D M; Jamilah, B; Amin, I

    2014-08-01

    In-house method validation was conducted to determine amino acid composition in gelatin by a pre-column derivatization procedure with the 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate reagent. The analytical parameters revealed that the validated method was capable of selectively performing a good chromatographic separation for 18 amino acids in less than 40 min; the overall detection and quantitation limit for amino acids fell into ranges of 5.68-12.48 and 36.0-39.0 pmol/μl, respectively; the matrix effect was not observed, and the linearity range was 37.5-1000 pmol/μl. The accuracy (precision and recovery) analyses of the method were conducted under repeatable conditions on different days in random order. Method precision revealed by HorRat values was significantly less than 2, except for histidine with a precision of 2.19, and the method recoveries had a range of 80-115% except for alanine which was recovered at 79.4%. The findings were reproducible and accurately defined, and the method was found to be suited to routine analysis of amino acid composition in gelatin-based ingredients. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. [Preparation of 1-(2-naphthyl) -3-methyl-5-pyrazolone as pre-column derivatization reagent for the determination of saccharides using high performance liquid chromatography-mass spectrometry].

    PubMed

    Sun, Zhiwei; Liu, Lingjun; Hu, Baojun; Sheng, Xiao; Wang, Xiaoyan; Suo, Yourui; You, Jinmao

    2008-03-01

    Eight saccharides were derivatized using 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) as pre-column derivatizing reagent, and separated on a reversed-phase Hypersil ODS 2 column (4.6 mm x 200 mm, 5 microm), by high performance liquid chromatography (HPLC) in conjunction with a gradient elution, detected by a diode array detector (DAD), and identified by electrospray ionization-mass spectrometry (ESI-MS) in positive ion mode. NMP reacted with reductive saccharides easily in the presence of 17% ammonia water at 70 degrees C. All linear correlation coefficients for saccharide derivatives were over 0.998 5. The detection limits (at signal-to-noise of 3:1) were 0.58 - 1.1 pmol for saccharide derivatives. The characteristic fragment ions, especially m/z 473, from the cleavage of NMP-labeled saccharides exhibited high regularity for the identification of the composition of saccharide mixture. The established method is sensitive and repeatable for the determination of saccharides.

  18. Rapid and sensitive determination of free thiols by capillary zone electrophoresis with near-infrared laser-induced fluorescence detection using a new BODIPY-based probe as labeling reagent.

    PubMed

    Zhang, Li-Yun; Tu, Feng-Qin; Guo, Xiao-Feng; Wang, Hong; Wang, Peng; Zhang, Hua-Shan

    2014-10-01

    A CZE with near-infrared (NIR) LIF detection method has been developed for the analysis of six low molecular weight thiols including glutathione, homocysteine, cysteine, γ-glutamylcysteine, cysteinylglycine, and N-acetylcysteine. For this purpose, a new NIR fluorescent probe, 1,7-dimethyl-3,5-distyryl-8-phenyl-(4'-iodoacetamido)difluoroboradiaza-s-indacene was utilized as the labeling reagent, whose excitation wavelength matches the commercially available NIR laser line of 635 nm. The optimum procedure included a derivatization step of the free thiols at 45°C for 25 min and CZE analysis conducted within 14 min in the running buffer containing 16 mmol/L pH 7.0 sodium citrate and 60% v/v ACN. The LODs (S/N = 3) ranged from 0.11 nmol/L for N-acetylcysteine to 0.31 nmol/L for γ-glutamylcysteine, which are better than or comparable to those reported with other derivatization-based CE-LIF methods. As the first trial of NIR CE-LIF method for thiol determination, the practical application of the proposed method has been validated by detecting thiols in cucumber and tomato samples with recoveries of 96.5-104.3%.

  19. Detection of DBD-carbamoyl amino acids in amino acid sequence and D/L configuration determination of peptides with fluorogenic Edman reagent 7-[(N,N-dimethylamino)sulfonyl]-2,1,3-benzoxadiazol-4-yl isothiocyanate.

    PubMed

    Huang, Y; Matsunaga, H; Toriba, A; Santa, T; Fukushima, T; Imai, K

    1999-06-01

    A method for amino acid sequence and D/L configuration identification of peptides by using fluorogenic Edman reagent 7-[(N, N-dimethylamino)sulfonyl]-2,1,3-benzoxadiazol-4-yl isothiocyanate (DBD-NCS) has been developed. This method was based on the Edman degradation principle with some modifications. A peptide or protein was coupled with DBD-NCS under basic conditions and then cyclized/cleaved to produce DBD-thiazolinone (TZ) derivative by BF3, a Lewis acid, which could significantly suppress the amino acid racemization. The liberated DBD-TZ amino acid was hydrolyzed to DBD-thiocarbamoyl (TC) amino acid under a weakly acidic condition and then oxidized by NaNO2/H+ to DBD-carbamoyl (CA) amino acid which was a stable and had a strong fluorescence intensity. The individual DBD-CA amino acids were separated on a reversed-phase high-performance liquid chromatography (RP-HPLC) for amino acid sequencing and their enantiomers were resolved on a chiral stationary-phase HPLC for identifying their D/L configurations. Combination of the two HPLC systems, the amino acid sequence and D/L configuration of peptides could be determined. This method will be useful for searching D-amino-acid-containing peptides in animals.

  20. Radiochemical neutron activation analysis of Fe, Co, Zn, Sb and Se in biomedical and environmental samples.

    PubMed

    Garg, A N; Weginwar, R G; Chutke, N L

    1993-11-01

    A radiochemical neutron activation method has been developed for the simultaneous determination of Fe, Co, Zn, Sb and Se levels in cancerous breast tissue, milk samples and fugitive cement dust particulates. Various Standard Reference Materials from NIST, USA (Bovine Liver 1577a, Milk Powder 1549, Coal Fly Ash 1633a and Urban Particulate Matter 1648), IAEA Vienna (Animal Muscle H-4, Milk powder A-11 and Soil-5) and NIES Japan (Pond Sediment) were also analysed for quality control. Samples together with standards were irradiated at a thermal neutron fluence of 10(13) ncm-2s-1 for 2 weeks. After dissolution/fusion together with carriers, the Fe was first separated by extracting with diethyl ether followed by extraction with cupferron in chloroform. From the aqueous phase Co and Zn were extracted using alpha-nitroso-beta-naphthol in chloroform and 2-thenoyltrifluoroacetone in isobutylmethyl ketone, respectively. From another aliquot, Se was first complexed with o-phenylenediamine and extracted in benzene. Later Sb was extracted using KI and 4-(2-pyridylazo)-resorcinol (PAR) in benzene. The method yields reasonably accurate data for monitoring of trace elements in biomedical and environmental specimens.

  1. The Radiochemical Analysis of Gaseous Samples (RAGS) Apparatus for Nuclear Diagnostics at the National Ignition Facility

    SciTech Connect

    Shaughnessy, D A; Velsko, C A; Jedlovec, D R; Yeamans, C B; Moody, K J; Tereshatov, E; Stoeffl, W; Riddle, A

    2012-05-11

    The RAGS (Radiochemical Analysis of Gaseous Samples) diagnostic apparatus was recently installed at the National Ignition Facility. Following a NIF shot, RAGS is used to pump the gas load from the NIF chamber for purification and isolation of the noble gases. After collection, the activated gaseous species are counted via gamma spectroscopy for measurement of the capsule areal density and fuel-ablator mix. Collection efficiency was determined by injecting a known amount of {sup 135}Xe into the NIF chamber, which was then collected with RAGS. Commissioning was performed with an exploding pusher capsule filled with isotopically enriched {sup 124}Xe and {sup 126}Xe added to the DT gas fill. Activated xenon species were recovered post-shot and counted via gamma spectroscopy. Results from the collection and commissioning tests are presented. The performance of RAGS allows us to establish a noble gas collection method for measurement of noble gas species produced via neutron and charged particle reactions in a NIF capsule.

  2. Preparation of 99mTc-MAG3: radiochemical purity is affected by the residence time of sodium chloride injection in a three-part syringe.

    PubMed

    Waight, Clinton C; Beattie, Lynn A; O'Brien, Lesley M; Millar, Alistair M

    2006-02-01

    Routine technetium-99m mercaptoacetyltriglycine (99mTc-MAG3) radiochemical purity measurements have revealed occasional unacceptably low values. Preliminary investigations suggested a causal link with the residence time of sodium chloride injection in the syringe used to reconstitute the MAG3 kit. To investigate the cause of this phenomenon, determine how it can be avoided and establish whether it occurs with other 99mTc radiopharmaceuticals. 99mTc-MAG3 was prepared by drawing sodium chloride injection into a lubricated, three-part, 10 ml Plastipak syringe and using it to reconstitute a MAG3 kit immediately or after a 15 min incubation period. The radiochemical purity was measured by high-performance liquid chromatography. The experiment was repeated using lubricant-free, two-part, Norm-Ject syringes and lubricated, two-part, Monoject syringes (15 min incubation only). To investigate the influence of Plastipak's rubber components on the radiochemical purity, samples were prepared using sodium chloride injection that had been incubated with lubricated or lubricant-free rubber plunger ends. Similar experiments were performed to determine the effect of Plastipak on 99mTc-exametazime, 99mTc-sestamibi and 99mTc-tetrofosmin. The radiochemical purities of 99mTc-MAG3 prepared with sodium chloride injection incubated for 0 and 15 min in Plastipak syringes were 96.4+/-0.5% and 89.4+/-5.5%, respectively. The difference was significant (P<0.05, n=10). With Norm-Ject syringes, the radiochemical purities were 96.5+/-0.5% and 96.6+/-0.5%, respectively. The difference was not significant (P>0.05, n=10). With Monoject syringes, the radiochemical purity was 96.6+/-0.4% (n=10). 99mTc-MAG3 prepared using sodium chloride injection treated with lubricated and unlubricated syringe rubber plunger ends had radiochemical purities of 85.3+/-6.6% and 82.1+/-6.5% (n=5), respectively. The radiochemical purities of other 99mTc radiopharmaceuticals prepared using sodium chloride injection

  3. Radiochemical neutron activation analysis for 36 elements in geological material: Au, Ag, Bi, Br, Cd, Cs, Ge, In, Ir, Ni, Os, Pd, Rb, Re, Sb, Se, Sn, Te, Tl, U, and Zn as well as Sc, Y, and REE

    SciTech Connect

    Anders, E; Wolf, R; Morgan, J W; Ebihara, M; Woodrow, A B; Janssens, M J; Hertogen, J

    1988-01-01

    In lunar and terrestrial rocks and in meteorites, the radiochemical neutron activation method decribed here enables determination of the 21 trace and ultratrace elements Ag, Au, Bi, Br, Cd, Cs, Ga, Ge, In, Ir, Ni, Os, Pd, Rb, Re, Sb, Se, Te, Tl, U, Zn, as well as 13 rare earth elements (REE), Sc and Y. Materials, techniques and procedures are discussed. 81 refs.

  4. [Supplies: inventory control and reagents].

    PubMed

    Szymanowicz, A

    2013-06-01

    The main relevant features useful for the management of reagents and consumables as well as documents to be developed to meet the requirements of the accreditation standard ISO/FDIS 15189-2012 are listed. This article is intended to help the medical laboratory to get mandatory accreditation.

  5. NMR-based approach to the analysis of radiopharmaceuticals: radiochemical purity, specific activity, and radioactive concentration values by proton and tritium NMR spectroscopy.

    PubMed

    Schenk, David J; Dormer, Peter G; Hesk, David; Pollack, Scott R; Lavey, Carolee Flader

    2015-06-15

    Compounds containing tritium are widely used across the drug discovery and development landscape. These materials are widely utilized because they can be efficiently synthesized and produced at high specific activity. Results from internally calibrated (3)H and (1)H nuclear magnetic resonance (NMR) spectroscopy suggests that at least in some cases, this calibrated approach could supplement or potentially replace radio-high-performance liquid chromatography for radiochemical purity, dilution and scintillation counting for the measurement of radioactivity per volume, and liquid chromatography/mass spectrometry analysis for the determination of specific activity. In summary, the NMR-derived values agreed with those from the standard approaches to within 1% to 9% for solution count and specific activity. Additionally, the NMR-derived values for radiochemical purity deviated by less than 5%. A benefit of this method is that these values may be calculated at the same time that (3)H NMR analysis provides the location and distribution of tritium atoms within the molecule. Presented and discussed here is the application of this method, advantages and disadvantages of the approach, and a rationale for utilizing internally calibrated (1)H and (3)H NMR spectroscopy for specific activity, radioactive concentration, and radiochemical purity whenever acquiring (3)H NMR for tritium location.

  6. Spot indole test: evaluation of four reagents.

    PubMed Central

    Miller, J M; Wright, J W

    1982-01-01

    Kovacs indole reagent, p-dimethylaminobenzaldehyde, Ehrlich indole reagent and p-dimethylaminocinnamaldehyde were used as spot indole reagents to test 359 strains of gram-negative rods growing on 5% sheep blood agar, Trypticase soy agar (BBL Microbiology Systems), and MacConkey agar. The p-dimethylaminocinnamaldehyde reagent was the most sensitive of those tested and provided results that were easiest to interpret. The p-dimethylaminocinnamaldehyde reagent was able to detect providencia alcalifaciens indole production because of the red-violet color unique to that organism. All reagents tested were accurate in detecting indole produced by members of the Enterobacteriaceae family, with the exception of P. alcalifaciens. PMID:7040458

  7. Sensitive determination of thiols in wine samples by a stable isotope-coded derivatization reagent d0/d4-acridone-10-ethyl-N-maleimide coupled with high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry analysis.

    PubMed

    Lv, Zhengxian; You, Jinmao; Lu, Shuaimin; Sun, Weidi; Ji, Zhongyin; Sun, Zhiwei; Song, Cuihua; Chen, Guang; Li, Guoliang; Hu, Na; Zhou, Wu; Suo, Yourui

    2017-03-31

    As the key aroma compounds, varietal thiols are the crucial odorants responsible for the flavor of wines. Quantitative analysis of thiols can provide crucial information for the aroma profiles of different wine styles. In this study, a rapid and sensitive method for the simultaneous determination of six thiols in wine using d0/d4-acridone-10-ethyl-N-maleimide (d0/d4-AENM) as stable isotope-coded derivatization reagent (SICD) by high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) has been developed. Quantification of thiols was performed by using d4-AENM labeled thiols as the internal standards (IS), followed by stable isotope dilution HPLC-ESI-MS/MS analysis. The AENM derivatization combined with multiple reactions monitoring (MRM) not only allowed trace analysis of thiols due to the extremely high sensitivity, but also efficiently corrected the matrix effects during HPLC-MS/MS and the fluctuation in MS/MS signal intensity due to instrument. The obtained internal standard calibration curves for six thiols were linear over the range of 25-10,000pmol/L (R(2)≥0.9961). Detection limits (LODs) for most of analytes were below 6.3pmol/L. The proposed method was successfully applied for the simultaneous determination of six kinds of thiols in wine samples with precisions ≤3.5% and recoveries ≥78.1%. In conclusion, the developed method is expected to be a promising tool for detection of trace thiols in wine and also in other complex matrix. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. A new approach for simultaneous determination of Co(II), Ni(II), Cu(II) and Pd(II) using 2-thiophenaldehyde-3-thiosemicarbazone as reagent by solid phase microextraction-high performance liquid chromatography.

    PubMed

    Kaur, Varinder; Aulakh, Jatinder Singh; Malik, Ashok Kumar

    2007-11-05

    A new method is proposed herein for the sorption, separation and simultaneous determination of Co(II), Ni(II), Cu(II) and Pd(II) using 2-thiophenaldehyde-3-thiosemicarbazone (TPTS) as a reagent by solid phase microextraction-high performance liquid chromatography-UV detection. The method is based upon the sorption of metal complexes on polydimethylsiloxane (PDMS) fiber from aqueous solution followed by desorption in the desorption chamber of solid phase microextraction-high performance liquid chromatography (SPME-HPLC) interface. Reversed phase high performance liquid chromatography using acetonitrile:water (65:35) as an eluent on a C18 column has been used to achieve the separation. The effects of agitation, addition of salts, extraction time and desorption time are examined to obtain optimized conditions. The detection limits for Co(II), Ni(II), Cu(II) and Pd(II) are 9, 6, 1 and 7 ng L(-1) based on 3sigma of blank response. The precision is calculated to be less than 3.5% (R.S.D.) for all species. A 10 time enhancement in the signal is observed for SPME when compared with direct analysis. The method is successfully applied to several synthetic mixtures without interference from other common metal ions such as Mo(VI), V(V), Ag(I), Sn(IV), Cd(II), Zn(II), Pb(II), Cr(III) and Cr(VI). The proposed method is tested for the determination of Co(II), Ni(II), Cu(II) and Pd(II) in alloys and water samples spiked with these metal ions.

  9. Study on determination of iron, cobalt, nickel, copper, zinc and manganese in drinking water by solid-phase extraction and RP-HPLC with 2-(2-quinolinylazo)-5-diethylaminophenol as precolumn derivatizing reagent.

    PubMed

    Hu, Qiufen; Yang, Guanyu; Yang, Jihong; Yin, Jiayuan

    2002-12-01

    A new method for the determination of iron, cobalt, nickel, copper, zinc and manganese in drinking water by the reversed-phase high-performance liquid chromatography (RP-HPLC) with 2-(2-quinolinylazo)-5-diethylaminophenol (QADEAP) as precolumn derivatizing reagent was studied in this paper. The iron, cobalt, nickel, copper, zinc, and manganese ions react with QADEAP to form color chelates in the presence of cetyl trimethylammonium bromide (CTMAB) and acetic acid-sodium acetic buffer solution medium of pH 4.0. These chelates were enriched by solid-phase extraction with a Waters Nova-Pak C18 cartridge and eluted the retained chelates from the cartridge with tetrahydrofuran (THF). The enrichment factor of 100 was achieved. Then the chelates were separated on a Waters Nova-Pak C18 column (3.9 x 150 mm, 5 microm) by gradient elution with methanol (containing 0.2% of acetic acid and 0.1% of CTMAB) and 0.05 mol L(-1) acetic acid-sodium acetic buffer solution (containing 0.1% of CTMAB) (pH 4.0) as mobile phase at a flow rate of 0.5 ml min(-1), and monitored with a photodiode array detector from 450 approximately 700 nm. The detection limits (S/N = 3) of iron, cobalt, nickel, copper, zinc and manganese are 0.8, 1.1, 0.9, 1.1, 1.5 and 2.0 ng L(-1), respectively, in the original sample. This method can be applied to determination at the microg L(-1) level of iron, cobalt, nickel, copper, zinc and manganese in drinking water with good results.

  10. Note: Radiochemical measurement of fuel and ablator areal densities in cryogenic implosions at the National Ignition Facility

    SciTech Connect

    Hagmann, C. Shaughnessy, D. A.; Moody, K. J.; Grant, P. M.; Gharibyan, N.; Gostic, J. M.; Wooddy, P. T.; Torretto, P. C.; Bandong, B. B.; Bionta, R.; Cerjan, C. J.; Bernstein, L. A.; Caggiano, J. A.; Sayre, D. B.; Schneider, D. H.; Henry, E. A.; Fortner, R. J.; Herrmann, H. W.; Knauer, J. P.

    2015-07-15

    A new radiochemical method for determining deuterium-tritium (DT) fuel and plastic ablator (CH) areal densities (ρR) in high-convergence, cryogenic inertial confinement fusion implosions at the National Ignition Facility is described. It is based on measuring the {sup 198}Au/{sup 196}Au activation ratio using the collected post-shot debris of the Au hohlraum. The Au ratio combined with the independently measured neutron down scatter ratio uniquely determines the areal densities ρR(DT) and ρR(CH) during burn in the context of a simple 1-dimensional capsule model. The results show larger than expected ρR(CH) values, hinting at the presence of cold fuel-ablator mix.

  11. Note: Radiochemical measurement of fuel and ablator areal densities in cryogenic implosions at the National Ignition Facility

    NASA Astrophysics Data System (ADS)

    Hagmann, C.; Shaughnessy, D. A.; Moody, K. J.; Grant, P. M.; Gharibyan, N.; Gostic, J. M.; Wooddy, P. T.; Torretto, P. C.; Bandong, B. B.; Bionta, R.; Cerjan, C. J.; Bernstein, L. A.; Caggiano, J. A.; Herrmann, H. W.; Knauer, J. P.; Sayre, D. B.; Schneider, D. H.; Henry, E. A.; Fortner, R. J.

    2015-07-01

    A new radiochemical method for determining deuterium-tritium (DT) fuel and plastic ablator (CH) areal densities (ρR) in high-convergence, cryogenic inertial confinement fusion implosions at the National Ignition Facility is described. It is based on measuring the 198Au/196Au activation ratio using the collected post-shot debris of the Au hohlraum. The Au ratio combined with the independently measured neutron down scatter ratio uniquely determines the areal densities ρR(DT) and ρR(CH) during burn in the context of a simple 1-dimensional capsule model. The results show larger than expected ρR(CH) values, hinting at the presence of cold fuel-ablator mix.

  12. Note: Radiochemical measurement of fuel and ablator areal densities in cryogenic implosions at the National Ignition Facility.

    PubMed

    Hagmann, C; Shaughnessy, D A; Moody, K J; Grant, P M; Gharibyan, N; Gostic, J M; Wooddy, P T; Torretto, P C; Bandong, B B; Bionta, R; Cerjan, C J; Bernstein, L A; Caggiano, J A; Herrmann, H W; Knauer, J P; Sayre, D B; Schneider, D H; Henry, E A; Fortner, R J

    2015-07-01

    A new radiochemical method for determining deuterium-tritium (DT) fuel and plastic ablator (CH) areal densities (ρR) in high-convergence, cryogenic inertial confinement fusion implosions at the National Ignition Facility is described. It is based on measuring the (198)Au/(196)Au activation ratio using the collected post-shot debris of the Au hohlraum. The Au ratio combined with the independently measured neutron down scatter ratio uniquely determines the areal densities ρR(DT) and ρR(CH) during burn in the context of a simple 1-dimensional capsule model. The results show larger than expected ρR(CH) values, hinting at the presence of cold fuel-ablator mix.

  13. Effect of residual monomer on radiochemical and light radiation processes in polymethyl methacrylate

    SciTech Connect

    Khamidova, L.G.; Zhdanov, G.S.; Milinchuk, V.K.

    1988-03-01

    The radiochemical yield of paramagnetic centers at 77 K varies from 1.2 in a polymer with a 0.2% weight concentration of MMA to 2.35 in a polymer containing 6.3% MMA. At 273 K, the radiochemical yield of macroradicals varies from 1.7 (0.2% MMA) to 3.2 (2.4% MMA). The high radiochemical yield of binding of residual monomer (G/sub MMA/ = 5.6 x 10/sup 2/ and 2.4 x 10/sup 2/ at 300 and 77 K) indicates the existence of associates of molecules of the monomer. It was hypothesized that radiation damage initially develops in defective regions of the polymer where the molecules of the monomer are primarily concentrated.

  14. Inorganic and Radiochemical Analysis of AW-101 and AN-107 Tank Waste

    SciTech Connect

    MW Urie; JJ Wagner; LR Greenwood; OT Farmer; SK Fiskum; RT Ratner; CZ Soderquist

    1999-11-11

    This report presents the inorganic and radiochemical analytical results for AW-101 and AN-107 as received materials. The analyses were conducted in support of the BNFL Proposal No. 30406/29274 Task 5.0. The inorganic and radiochemical analysis results obtained from the as received materials are used to provide initial characterization information for subsequent process testing and to provide data to support permit application activities. Quality Assurance (QA) Plan MCS-033 provides the operational and quality control protocols for the analytical activities, and whenever possible, analyses were performed to SW-846 equivalent methods and protocols.

  15. General formalism for the study of activation: application to radiochemical detectors

    SciTech Connect

    Poppe, C.H.

    1982-09-24

    This paper develops mathematical techniques required for the study of neutron-induced activation of importance to fission and fusion devices - reactors, nuclear weapons, etc. The formalism is presented as a guide for examining the dependence of activation products on flux time history, spatial gradients and the sensitivity to the assumed reactions and cross sections. Exact solutions in powers of the neutron fluence are presented and examined in various limits. As an example, radiochemical threshold (n,2n) detectors used to diagnose thermonuclear explosions are studied using approximations to these solutions. In particular, approximate formulas for the sensitivity of the radiochemical products to different cross sections are derived.

  16. Thionation using fluorous Lawesson's reagent.

    PubMed

    Kaleta, Zoltán; Makowski, Brian T; Soós, Tibor; Dembinski, Roman

    2006-04-13

    [reaction: see text] Thionation of amides, 1,4-diketones, N-(2-oxoalkyl)amides, N,N'-acylhydrazines, and acyl-protected uridines with the use of a fluorous analogue of the Lawesson's reagent leads to thioamides, thiophenes, 1,3-thiazoles, 1,3,4-thiadiazoles, and acyl-protected 4-thiouridines. The isolation of the final products in high yields is achieved in most cases by a simple filtration (fluorous solid-phase extraction).

  17. [Effect of composition of reagents for activated partial thromboplastin time on their sensitivity during analysis of blood coagulation factors].

    PubMed

    Berkovskiĭ, A L; Vasil'ev, S A; Sergeeva, E V; Kozlov, A A

    2000-04-01

    Brain cephaline-based reagents for evaluating activated partial thromboplastin time (APTT) and soybean phosphatides with ellagic acid complex activator with intermediate metal ions have been studied. The sensitivity of these reagents to internal clotting factors (VIII and IX) and heparin is determined by phospholipid nature and type of metal. The results help obtain highly active and sensitive APTT reagents.

  18. Radiochemical Analysis by High Sensitivity Micro X-Ray Fluorescence Detection

    SciTech Connect

    Ning Gao

    2006-05-12

    The primary objective of the project was to develop a novel dual-optic x-ray fluorescence instrument capable of doing radiochemical analysis of high-level radioactive wastes at DOE sites such as Savannah River Site and Hanford Site.

  19. [A comparison on radiochemical behavior and biological property of antisense oligonucleotide labeled with technetium-99m by two methods: NHS-MAG3 versus SHNHP].

    PubMed

    Li, Yunchun; Tan, Tianzhi; Zheng, Jianguo; Zhang, Chun

    2008-08-01

    This study was undertaken to explore and compare the radiochemical behavior and biological property of antisense oligonucleotide (ASON) labeled with Technetium-99m using two methods: N-hydroxysuccinimidyl S-acetylmercaptoacetyltriglycline (NHS-MAG3) versus hydrazino nicotinamide derivative (SHNH). After SHNH and NHS-MAG3 were synthesized, ASON was labeled with Technetium-99m using SHNH and NHS-MAG3 as a bifunctional chelator, separately. The stability in vivo and in vitro, the combination with plasma albumen of rabbit, the biodistribution in BALB/ C mice and the HT29 cellular uptake were compared between labeled compound 99mTc-SHNH-ASON, using SHNH as a bifunctional complex reagent, and 99mTc-MAG3-ASON, using NHS-MAG3 as a bifunctional chelator. The results revealed that the labeling rate and the stability of 99mTc-MAG3-ASON were evidently higher than that of 99mTc-SHNH-ASON (P < 0.05), the combination rate of 99mTc-MAG3-ASON with plasma albumen was markedly lower than that of 99mTc-SHNH-ASON (P < 0.05); the biodistribution of 99mTc-MAG3-ASON was markedly lower than that of 99mTc-SHNH-ASON in blood, heart, stomach and intestines (P < 0.05), slightly lower than that of 99mTc-SHNH-ASON in liver and spleen (P > 0.05), and markedly higher than that of 99mTc-SHNH-ASON in kidney (P < 0.05); the HT29 cellular uptake rates of 99mTc-MAG3-ASON was markedly higher than that of 99mTc-SHNH-ASON (P < 0.05). Therefore, the radiochemical behavior and biological property of 99mTc-MAG3-ASON labeled using NHS-MAG3 is better than that of 99mTc-SHNH-ASON labeled using SHNH.

  20. Literature search, review, and compilation of data for chemical and radiochemical sensors: Task 1 report

    SciTech Connect

    1993-01-01

    During the next several decades, the US Department of Energy is expected to spend tens of billions of dollars in the characterization, cleanup, and monitoring of DOE`s current and former installations that have various degrees of soil and groundwater contamination made up of both hazardous and mixed wastes. Each of these phases will require site surveys to determine type and quantity of hazardous and mixed wastes. It is generally recognized that these required survey and monitoring efforts cannot be performed using traditional chemistry methods based on laboratory evaluation of samples from the field. For that reason, a tremendous push during the past decade or so has been made on research and development of sensors. This report contains the results of an extensive literature search on sensors that are used or have applicability in environmental and waste management. While restricting the search to a relatively small part of the total chemistry spectrum, a sizable body of reference material is included. Results are presented in tabular form for general references obtained from data base searches, as narrative reviews of relevant chapters from proceedings, as book reviews, and as reviews of journal articles with particular relevance to the review. Four broad sensor types are covered: electrochemical processes, piezoelectric devices, fiber optics, and radiochemical processes. The topics of surface chemistry processes and biosensors are not treated separately because they often are an adjunct to one of the four sensors listed. About 1,000 tabular entries are listed, including selected journal articles, reviews of conference/meeting proceedings, and books. Literature to about mid-1992 is covered.

  1. Using Absolute Humidity and Radiochemical Analyses of Water Vapor Samples to Correct Underestimated Atmospheric Tritium Concentrations

    SciTech Connect

    Eberhart, C.F.

    1999-06-01

    Los Alamos National Laboratory (LANL) emits a wide variety of radioactive air contaminants. An extensive ambient air monitoring network, known as AIRNET, is operated on-site and in surrounding communities to estimate radioactive doses to the public. As part of this monitoring network, water vapor is sampled continuously at more than 50 sites. These water vapor samples are collected every two weeks by absorbing the water vapor in the sampled air with silica gel and then radiochemically analyzing the water for tritium. The data have consistently indicated that LANL emissions cause a small, but measurable impact on local concentrations of tritium. In early 1998, while trying to independently verify the presumed 100% water vapor collection efficiency, the author found that this efficiency was normally lower and reached a minimum of 10 to 20% in the middle of summer. This inefficient collection was discovered by comparing absolute humidity (g/m{sup 3}) calculated from relative humidity and temperature to the amount of water vapor collected by the silica gel per cubic meter of air sampled. Subsequent experiments confirmed that the elevated temperature inside the louvered housing was high enough to reduce the capacity of the silica gel by more than half. In addition, their experiments also demonstrated that, even under optimal conditions, there is not enough silica gel present in the sampling canister to absorb all of the moisture during the higher humidity periods. However, there is a solution to this problem. Ambient tritium concentrations have been recalculated by using the absolute humidity values and the tritium analyses. These recalculated tritium concentrations were two to three times higher than previously reported. Future tritium concentrations will also be determined in the same manner. Finally, the water vapor collection process will be changed by relocating the sampling canister outside the housing to increase collection efficiency and, therefore

  2. The Northern Marshall Islands radiological survey: A quality control program for radiochemical and gamma spectroscopy analysis

    SciTech Connect

    Kehl, S.R.; Mount, M.E.; Robison, W.L.

    1995-09-01

    From 1979 to 1989, approximately 25,000 Post Northern Marshall Islands Radiological Survey (PNMIRS) samples were collected, and over 71,400 radiochemical and gamma spectroscopy analyses were performed to establish the concentration of {sup 90}Sr, {sup 137}Cs, {sup 241}Am, and plutonium isotopes in soil, vegetation, fish, and animals in the Northern Marshall Islands. While the Low Level Gamma Counting Facility (B379) in the Health and Ecological Assessment (HEA) division accounted for over 80% of all gamma spectroscopy analyses, approximately 4889 radiochemical and 5437 gamma spectroscopy analyses were performed on 4784 samples of soil, vegetation, terrestrial animal, and marine organisms by outside laboratories. Four laboratories were used by Lawrence Livermore National Laboratory (LLNL) to perform the radiochemical analyses: Thermo Analytical Norcal, Richmond, California (TMA); Nuclear Energy Services, North Carolina State University (NCSU); Laboratory of Radiation Ecology, University of Washington (LRE); and Health and Ecological Assessment (HEA) division, LLNL, Livermore, California. Additionally, LRE and NCSU were used to perform gamma spectroscopy analyses. The analytical precision and accuracy were monitored by including blind duplicates and natural matrix standards in each group of samples analyzed. On the basis of reported analytical values for duplicates and standards, 88% of the gamma and 87% of the radiochemical analyses in this survey were accepted. By laboratory, 93% of the radiochemical analyses by TMA; 88% of the gamma-ray spectrometry and 100% of the radiochemistry analyses by NCSU; 89% of the gamma spectroscopy and 87% of the radiochemistry analyses by LRE; and 90% of the radiochemistry analyses performed by HEA`s radiochemistry department were accepted.

  3. Renewable-reagent electrochemical sensor

    DOEpatents

    Wang, Joseph; Olsen, Khris B.

    1999-01-01

    A new electrochemical probe(s) design allowing for continuous (renewable) reagent delivery. The probe comprises an integrated membrane-sampling/electrochemical sensor that prevents interferences from surface-active materials and greatly extends the linear range. The probe(s) is useful for remote or laboratory-based monitoring in connection with microdialysis sampling and electrochemical measurements of metals and organic compounds that are not readily detected in the absence of reacting with the compound. Also disclosed is a method of using the probe(s).

  4. Renewable-reagent electrochemical sensor

    DOEpatents

    Wang, J.; Olsen, K.B.

    1999-08-24

    A new electrochemical probe(s) design allowing for continuous (renewable) reagent delivery is described. The probe comprises an integrated membrane sampling/electrochemical sensor that prevents interferences from surface-active materials and greatly extends the linear range. The probe(s) is useful for remote or laboratory-based monitoring in connection with microdialysis sampling and electrochemical measurements of metals and organic compounds that are not readily detected in the absence of reacting with the compound. Also disclosed is a method of using the probe(s). 19 figs.

  5. Features of the reaction of heterocyclic analogs of chalcone with lanthanide shift reagents

    SciTech Connect

    Turov, A.V.; Khilya, V.P.

    1994-10-01

    The PMR spectra of heterocyclic analogs of 2-hydroxychalcone containing thiazole, benzofuran, triazole, imidazole, benzodioxane, or pyridine rings in the presence of lanthanide shift reagents are studied. It is found that the most effective reagent for modifying the spectra of these compounds is Yb(fod)3. The broadening of the spectra of 2-hydroxy chalcones in the presence of lanthanide shift reagents is explained by the dynamic effects of complex formation. An example is given of the determination of the conformation of molecules of 2-hydroxychalcone by the simultaneous use of lanthanide shift reagents and the homonuclear Overhauser effect. 9 refs., 1 fig., 1 tab.

  6. 2'-hydroxychalcone as an analytical reagent for beryllium.

    PubMed

    Naidu, R R

    1975-07-01

    Several o-hydroxychalcones were examined to develop specific reagents for the precipitation of beryllium in the presence of elements such as aluminium and iron, which occur in its ores. All these reagents showed specificity only in the presence of EDTA. Among them, the readily obtainable 2'-hydroxychalcone is proposed as a new specific reagent for beryllium. The chalcone complex can be dried to constant weight at 105-110 degrees and the conversion factor is 0.01978. A probable structure for the complex has been suggested. Quantitative separation of beryllium from aluminium and iron carried out by this method gave good results. This method was applied for the gravimetric determination of beryllium in beryl and the results were in good agreement with those obtained by the oxide and pyrophosphate methods.

  7. OPERATIONAL EXPERIENCE: UPGRADED MPC AND A SYSTEMS FOR THE RADIOCHEMICAL PLANT OF THE SIBERIAN CHEMICAL COMBINE

    SciTech Connect

    RODRIGUEZ,C.GOLOSKOKOV,I.FISHBONE,L.GOODEY,K.LOOMIS,M.CRAIN,B.JR.LARSEN,R.

    2003-07-18

    The success of reducing the risk of nuclear proliferation through physical protection and material control/accounting systems depends upon the development of an effective design that includes consideration of the objectives of the systems and the resources available to implement the design. Included among the objectives of the design are facility characterization, definition of threat, and identification of targets. When considering resources, the designer must consider funds available, rapid low-cost elements, technology elements, human resources, and the availability of resources to sustain operation of the end system. The Siberian Chemical Combine (SCC) is a multi-function nuclear facility located in the Tomsk region of Siberia, Russia. Beginning in 1996, SCC joined with the United States Department of Energy (US/DOE) Material Protection, Control, and Accounting (MPC&A) Program to develop and implement MPC&A upgrades for the Radiochemical, Chemical Metallurgical, Conversion, Uranium Enrichment, and Reactor Plants of the SCC. At the Radiochemical Plant the MPC&A design and implementation process has been largely completed for the Plutonium Storage Facility and related areas of the Radiochemical Plant. Design and implementation of upgrades for the Radiochemical Plant include rapid physical protection upgrades such as bricking up of doors and windows, and installation of security-hardened doors. Rapid material control and accounting upgrades include installation of modern balances and bar code equipment. Comprehensive MPC&A upgrades include the installation of access controls to sensitive areas of the Plant, alarm communication and display (AC&D) systems to detect and annunciate alarm conditions, closed circuit (CCTV) systems to assess alarm conditions, central and secondary alarm station upgrades that enable security forces to assess and respond to alarm conditions, material control and accounting upgrades that include upgraded physical inventory procedures, and

  8. A review of reagents for fluorescence microscopy of cellular compartments and structures, Part III: reagents for actin, tubulin, cellular membranes, and whole cell and cytoplasm.

    PubMed

    Kilgore, Jason A; Dolman, Nick J; Davidson, Michael W

    2014-01-02

    Non-antibody commercial fluorescent reagents for imaging of cytoskeletal structures have been limited primarily to tubulin and actin, with the main factor in choice based mainly on whether cells are live or fixed and permeabilized. A wider range of options exist for cell membrane dyes, and the choice of reagent primarily depends on the preferred localization in the cell (i.e., all membranes or only the plasma membrane) and usage (i.e., whether the protocol involves fixation and permeabilization). For whole-cell or cytoplasmic imaging, the choice of reagent is determined mostly by the length of time that the cells need to be visualized (hours or days) and by fixation status. Presented here is a discussion on choosing commercially available reagents for these cellular structures, with an emphasis on use for microscopic imaging, with a featured reagent for each structure, a recommended protocol, troubleshooting guide, and example image.

  9. The Interchangeability of Viscoelastographic Instruments and Reagents

    DTIC Science & Technology

    2014-01-01

    each manufacturer. METHODS: We tested three sets of reagents as follows: (1) in-tem and ex-tem (Tem International GmbH); (2) kaolin and RapidTEG...parameter. Significant differences between the instruments were found in the > angle and maximum firmness of the clot for ex-tem and kaolin reagents as well... kaolin and RapidTEG (Haemonetics); (3) a well-characterized control recombinant tissue factorYphospholipid reagent. Blood was drawn from six healthy donors

  10. Reagent removal of manganese from ground water

    NASA Astrophysics Data System (ADS)

    Brayalovsky, G.; Migalaty, E.; Naschetnikova, O.

    2017-06-01

    The study is aimed at the technology development of treating drinking water from ground waters with high manganese content and oxidizability. Current technologies, physical/chemical mechanisms and factors affecting in ground treatment efficiency are reviewed. Research has been conducted on manganese compound removal from ground waters with high manganese content (5 ppm) and oxidizability. The studies were carried out on granular sorbent industrial ODM-2F filters (0.7-1.5 mm fraction). It was determined that conventional reagent oxidization technologies followed by filtration do not allow us to obtain the manganese content below 0.1 ppm when treating ground waters with high oxidizability. The innovative oxidation-based manganese removal technology with continuous introduction of reaction catalytic agent is suggested. This technology is effective in alkalization up to pH 8.8-9. Potassium permanganate was used as a catalytic agent, sodium hypochlorite was an oxidizer and cauistic soda served an alkalifying agent.

  11. Nonmicrobial alternative to reagent quality control testing.

    PubMed Central

    Reynolds, S M

    1982-01-01

    The traditional approach to quality control in microbiology involves the routine testing of both media and reagents with live microbial cultures. This is expensive, time consuming, and subject to the variables associated with the use of live organisms. A system of reagent quality control based on the pure chemical form of the metabolic end products important to the identification of the Enterobacteriaceae was evaluated. The metabolite reagent control system is simple, reliable, and extremely cost effective, and it eliminates the need for live microbial cultures and media for reagent quality control. PMID:6759528

  12. Renewable Reagent Fiber Optic Based Ammonia Sensor

    NASA Astrophysics Data System (ADS)

    Berman, Richard J.; Burgess, Lloyd W.

    1990-02-01

    Many fiber optic based chemical sensors have been described which rely on a reagent chemistry fixed at the fiber endface to provide analyte specificity. In such systems, problems involving probe-to-probe reproducibility, reagent photolability and reagent leaching are frequently encountered. As a result, calibration and standardization of these sensors becomes difficult or impossible and thus inhibits their application for long term in situ chemical monitoring. Many of these problems can be addressed and several additional advantages gained by continuously renewing the reagent chemistry. To illustrate this concept, a fiber optic ammonia sensor is described in which the reagent is delivered under direct control to a sensing volume of approximately 400 nanoliters located at the probe tip. Using an acid-base indicator (bromothymol blue) as the reagent, the sample ammonia concentrations are related to modulations in light intensity with a lower limit of detection of 10 ppb. The sensor performance was studied with respect to reagent pH, concentration and reagent delivery rate. Compared with previous fiber optic ammonia sensors, the ability to reproducibly renew the reagent has resulted in improvements with respect to response and return times, probe-to-probe reproducibility, probe lifetime and flexibility of use.

  13. Nuclear and radiochemical techniques in chemical analysis. Final report

    SciTech Connect

    Finston, H.L.; Williams, E.T.

    1981-06-01

    The areas studied during the period of the contract included determinations of cross sections for nuclear reactions, determination of neutron capture cross sections of radionuclides, application of special activation techniques, and x-ray counting, elucidation of synergic solvent extraction mechanisms and development of new solvent extraction techniques, and the development of a PIXE analytical facility. The thermal neutron capture cross section of /sup 22/Na was determined, and cross sections and energy levels were determined for /sup 20/Ne(n,..cap alpha..)/sup 17/O, /sup 20/Ne(n,P)/sup 20/F, and /sup 40/Ar(n,..cap alpha..)/sup 37/S. Inelastic scattering with 2 to 3 MeV neutrons followed by counting of the metastable states permits analysis of the following elements: In, Sr, Cd, Hg, and Pb. Bromine can be detected in the presence of a 500-fold excess of Na and/or K by thermal neutron activation and x-ray counting, and as little as 0.3 x 10/sup -9/ g of Hg can be detected by this technique. Mediun energy neutrons (10 to 160 MeV) have been used to determine Tl, Pb, and Bi by (n,Xn) and (n,PXn) reactions. The reaction /sup 19/F(P,..cap alpha..)/sup 76/O has been used to determine as little as 50 ..mu..mol of Freon -14. Mechanisms for synergic solvent extractions have been elucidated and a new technique of homogeneous liquid-liquid solvent extraction has been developed in which the neutral complex is rapidly extracted propylene carbonate by raising and lowering the temperature of the system. An external-beam PIXE system has been developed for trace element analyses of a variety of sample types. Various sample preparation techniques have been applied to a diverse range of samples including marine sediment, coral, coal, and blood.

  14. Radiochemical Signatures of Interfacial Areal Density and Mix in NIF Implosions

    NASA Astrophysics Data System (ADS)

    Cerjan, Charles; Cassata, William; Velsko, Carol; Hoffman, Rob; Sepke, Scott; Jedlovec, Donald; Stoeffl, Wolfgang; Shaughnessy, Dawn

    2015-11-01

    Recent experimental results from the Radiochemical Analysis of Gaseous Samples (RAGS) diagnostic facility fielded at the National Ignition Facility (NIF) have demonstrated 13N production from charged particle nuclear reactions. This radiochemical product is very sensitive to the fuel-ablator interface areal density. Two specific reactions dominate 13N production: 12C(d,n)13Nand13C(p,n)13N. The short range of the energetically up-scattered deuterons from the cold DT fuel layer restricts the production to the proximate ablator interface thus providing high sensitivity to the interfacial configuration. Although the proton-mediated reaction is almost equally favorable, the small natural abundance of 13C suppresses this contribution to 13N production. Representative HYDRA simulations are used to illustrate these observed effects. This work was performed under the auspices of the U. S. Department of Energy by the Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

  15. Improvement of a radiochemical separation for selenium 79: Applications to effluents and nuclear wastes.

    PubMed

    Frechou, Carole; Aguerre, Sandrine; Degros, Jean-Pierre; Kerlau, Gilles; Grangeon, Thomas

    2007-05-15

    Selenium 79 is a beta emitter produced from (235)U fission and is one of the long half-life radionuclides of interest in nuclear waste disposal problematic because of its potential migration capacity to the surface environment. Measurement of (79)Se is particularly difficult due to its low activity in waste matrices (about 10(-3)Bqg(-1)). A radiochemical procedure based on ion exchange separations was already described in a previous paper. This work presents different applications of the radiochemical separation to waste samples and an improvement of this procedure, including a selective extraction of selenium as diethylselenium in an organic solvent followed by a re-extraction in aqueous medium. This additional step allows the decontamination factor to be increased with the aim of counting (79)Se by liquid scintillation counting.

  16. On-Line Monitoring and Control of Radiochemical Streams at Spent Fuel Reprocessing Plant

    SciTech Connect

    Levitskaia, Tatiana G.; Bryan, Samuel A.

    2008-05-23

    Techniques are needed to provide on-line monitoring and control of the radiochemical processes that are being developed and demonstrated under the Global Nuclear Energy Partnership (GNEP) initiative. The instrumentation used to monitor these processes must be robust and must be able to withstand harsh radiation and chemical environments. A new on-line monitoring system satisfying these requirements featuring Raman spectroscopy combined with a Coriolis and conductivity probes, has been recently developed by our research team. It provides immediate chemical data and flow parameters of high-level radioactive waste streams with high brine/high alkalinity generated during retrieval from Hanford nuclear waste storage tanks. We are currently applying similar methodology for monitoring the radiochemical streams generated at the spent fuel reprocessing plant. The nature of these strems calls for additional spectroscopic information, which can be gained by the utilization of UV-vis-NIR capabilities.

  17. Investigation of reagent distributions on glass fiber membrane filters used in air sampling.

    PubMed

    Tucker, Samuel P

    2007-10-01

    This project has arisen from the need to produce GFFs (glass fiber filters) bearing a thin and evenly distributed coating of a selected reagent in the equatorial plane for breakthrough studies. However, it has been discovered that today's two general techniques for coating GFFs (total immersion and application of reagent solution to GFFs) have usually produced unevenly distributed coatings of reagent in the equatorial plane. In addition, quantities of reagent on GFFs from commercial sources may vary widely in the same lot of coated GFFs. Consequences are variability in capacity of coated filters at the point of breakthrough and, perhaps, wasted reagent. Although today's reagent-coated filters may be satisfactory for routine air sampling, such filters may be unacceptable for precise breakthrough studies. Research has been conducted successfully to produce nearly evenly distributed coatings of reagents in the equatorial plane of GFFs by application of reagent solutions to the centers of GFFs which are resting on crisscrossing, fine, stainless-steel wire. Distributions of coatings have been determined by punching out twenty-one 5-mm circles from each GFF and analyzing each circle by flow-injection with a UV detector. Lowest achievable relative standard deviations of measurement (RSDs) for reagents in 5-mm circles have been 5 to 7%. Reagents studied have included 1-(2-pyridyl)piperazine (1-2PP), 2,4-dinitrophenylhydrazine (DNPH), and 1-(9-anthracenylmethyl)piperazine (MAP). Factors affecting the distribution of such coatings include choice of reagent and choice of solvent for the reagent solution.

  18. N.S. Savannah Reactor Vessel Metal Extraction and Radiochemical Analysis

    SciTech Connect

    Ranellone, Richard; Bowen, John; Stouky, Jon; Wiegand, John

    2008-01-15

    In early 2006 a project was concluded to determine radioisotopic inventory and Curie content of the N.S. Savannah Reactor Pressure Vessel (RPV), Internals and Neutron Shield Tank (NST) by extracting metal samples and performing radiochemical analysis. The objective of this project was to determine if the RPV and internals could be removed, packaged, shipped and disposed as Class A radioactive waste without opening the RPV or conducting further sampling of the RPV/Internals. The N.S. Savannah is de-fueled and has been shut down for 37 years. The following conclusions can be drawn from this project: - Results are consistent with previous analyses and are based upon conservative methodology and assumptions. - Nuclide concentration for the N/S Savannah reactor pressure vessel and internals package are shown to be within Class A disposal limits when averaged over the entire volume of metal in the Reactor Pressure Vessel and internals. - Performance of N.S. Savannah's nuclear reactor was excellent. During normal operations, the reactor seldom operated above 80% of its rated power level, thereby minimizing thermal stresses on the fuel cladding. In addition, the fuel rods were not subjected to any accident or severe transient conditions that could result in cladding breeches with subsequent release of fission products and fuel particles to the primary coolant loop. The trace quantities of Cesium-137 observed in the primary loop water indicate that some pinhole penetrations of fuel rod cladding may have occurred during operations. Another source of Cesium-137 could be the presence of uranium fuel on the exterior of the fuel rod cladding (tramp uranium), a condition not uncommon in the N.S. Savannah fuel fabrication time frame. Fissioning of this 'tramp uranium' would cause the rapid release of chemically active Cesium-137 into the reactor coolant. However, the absence of other fission products (e.g., Strontium-90) as well as uranium and transuranic isotopes in the reactor

  19. Hydrologic conditions and distribution of selected radiochemical and chemical constituents in water, Snake River Plain aquifer, Idaho National Engineering Laboratory, Idaho, 1989 through 1991

    SciTech Connect

    Bartholomay, R.C.; Orr, B.R.; Liszewski, M.J.; Jensen, R.G.

    1995-08-01

    Radiochemical and chemical wastewater discharged since 1952 to infiltration ponds and disposal wells at the Idaho National Engineering Laboratory (INEL) has affected water quality in the Snake River Plain aquifer. The U.S. Geological Survey, in cooperation with the U.S. Department of Energy, maintains a continuous monitoring network at the INEL to determine hydrologic trends and to delineate the movement of radiochemical and chemical wastes in the aquifer. This report presents an analysis of water-level and water-quality data collected from the Snake River Plain aquifer during 1989-91. Water in the eastern Snake River Plain aquifer moves principally through fractures and interflow zones in basalt, generally flows southwestward, and eventually discharges at springs along the Snake River. The aquifer is recharged principally from irrigation water, infiltration of streamflow, and ground-water inflow from adjoining mountain drainage basins. Water levels in wells throughout the INEL generally declined during 1989-91 due to drought. Detectable concentrations of radiochemical constituents in water samples from wells in the Snake River Plain aquifer at the INEL decreased or remained constant during 1989-91. Decreased concentrations are attributed to reduced rates of radioactive-waste disposal, sorption processes, radioactive decay, and changes in waste-disposal practices. Detectable concentrations of chemical constituents in water from the Snake River Plain aquifer at the INEL were variable during 1989-91. Sodium and chloride concentrations in the southern part of the INEL increased slightly during 1989-91 because of increased waste-disposal rates and a lack of recharge from the Big Lost River. Plumes of 1,1,1-trichloroethane have developed near the Idaho Chemical Processing Plant and the Radioactive Waste Management Complex as a result of waste disposal practices.

  20. Interchangeability of rotational elastographic instruments and reagents.

    PubMed

    Aleshnick, Maya; Orfeo, Thomas; Brummel-Ziedins, Kathleen; Gissel, Matthew; Mann, Kenneth

    2014-01-01

    Viscoelastic measurements are frequently being used in clinical and research settings for a rapid assessment of the hemostatic processes of blood clot formation and degradation. These measurements are being performed on either of two instruments (TEG and ROTEM) using their proprietary reagents. Standardization between the instruments and the reagents has been lacking but is necessary to compare results across instruments. In this study, we perform a crossover analysis between the TEG and ROTEM instruments using proprietary reagents from each manufacturer. We tested three sets of reagents as follows: (1) in-tem and ex-tem (Tem International GmbH); (2) kaolin and RapidTEG (Haemonetics); (3) a well-characterized control recombinant tissue factor-phospholipid reagent. Blood was drawn from six healthy donors, and each reagent was run concurrently in the TEG and ROTEM instruments. The volume of commercial reagent and calcium used was adjusted for crossover measurements to maintain the same concentration of each reagent in the blood. The outputs of clot time, rate of clot formation, and maximum firmness of the clot of the ROTEM and the TEG tracings were evaluated. The in-tem and RapidTEG reagents showed no disparity between instruments for any parameter. Significant differences between the instruments were found in the α angle and maximum firmness of the clot for ex-tem and kaolin reagents as well as in the clot time and maximum firmness of the clot for the recombinant tissue factor-phospholipid reagent. Although significant differences were observed for some parameters, the magnitudes were small compared with the differences between tests or the normal range variation in parameter values observed for these tests. These findings indicate that the instruments are more interchangeable than previously reported.

  1. U. S. Veterinary Immune Reagents Network: Progress with poultry immune reagents development

    USDA-ARS?s Scientific Manuscript database

    A major obstacle to advances in veterinary immunology and disease research is the lack of sufficient immunological reagents specific for veterinary animal species. In 2006, U. S. Veterinary Immune Reagent Network (VIRN) Consortium (www.vetimm.org) was developed to develop immune reagents against ma...

  2. Measurement of radiation exposure of astronauts by radiochemical techniques

    NASA Technical Reports Server (NTRS)

    Brodzinski, R. L.

    1972-01-01

    Only two of the fecal specimens collected inflight during the Apollo 15 mission were returned for analysis. Difficulty in obtaining reasonably accurate radiation dose estimates based on the cosmogenic radionuclide content of the specimens was encountered due to the limited sampling. The concentrations of Na-22, K-40, Cr-51, Fe-59, and Cs-137 are reported. The concentrations of 24 major, minor, and trace elements in these two specimens were determined. Most concentrations are typical of those observed previously. Major exceptions are extremely low values for selenium and extraordinarily high values for rare earth elements. The net Po-210 activities in the Apollo 11 and 12 Solar Wind Composition foils and in the Apollo 8 and 12 spacecraft reflective coatings due to lunar exposure have been determined. Equilibrium concentrations of 0.082 + or - 0.012 disintegrations /sq cm sec of Rn-222 in the lunar atmosphere and 0.0238 + or - 0.0035 disintegrations /sq cm sec of Po-210 on the lunar surface have been calculated for Oceanus Procellarum.

  3. A rapid radiochemical purity testing method for 99mTc-tetrofosmin.

    PubMed

    Eggert, Laura A; Dick, Michael D; Mahoney, Douglas W; Olson, Joseph P; Werner, Gregory L; Hung, Joseph C

    2010-06-01

    The standard radiochemical purity (RCP) testing method for (99m)Tc-tetrofosmin as described in the package insert requires extensive time (20-30 min) and considerable skill to achieve accurate results. Additionally, the instant thin-layer chromatography strip impregnated with silica gel (2x20 cm) used in the standard method will not be commercially available in the future. The purpose of this study was to evaluate whether a method developed by our laboratory for RCP testing of (99m)Tc-sestamibi could also be used as an alternative method for the RCP assay of (99m)Tc-tetrofosmin. The alternative RCP testing system consisted of a precut paper strip (1x8.5 cm) from solvent saturation pads (Pall Corp.) as the stationary phase, with 1:1 chloroform:tetrahydrofuran used as the mobile phase. To validate the reliability of the alternative method, RCP values from 17 kit preparations were compared with the 2 methods. Kits were reconstituted according to the package insert instructions, and 4 additions of (99m)Tc-sodium pertechnetate were purposely added to create trials with RCP values below the accepted limit of 90% purity. Two hundred four trials (100 of which were replicated) were run from the 17 kit preparations. Sixty-four (31%) of the 204 trials were below 90% purity based on the standard method. The overall agreement between the standard and alternative methods was 94% (192/204). The sensitivity of the alternative method for unacceptable RCP limits was 86% (55/64), and the specificity for acceptable RCP values was 98% (137/140). The agreement between the replicated trials of the alternative method was 99% (99/100), and for the standard method it was 92% (92/100). The standard method proved to be a much slower method and requires much more precision and attention. The alternative method is much faster, is easier, requires less attention to the solvent-development process, and can be used for RCP testing of both (99m)Tc-tetrofosmin and (99m)Tc-sestamibi. Furthermore, the

  4. Radiochemical Separation and Quantification of Tritium in Metallic Radwastes Generated from CANDU Type NPP - 13279

    SciTech Connect

    Ahn, H.J.; Choi, K.C.; Choi, K.S.; Park, T.H.; Park, Y.J.; Song, K.

    2013-07-01

    As a destructive quantification method of {sup 3}H in low and intermediate level radwastes, bomb oxidation, sample oxidation, and wet oxidation methods have been introduced. These methods have some merits and demerits in the radiochemical separation of {sup 3}H radionuclides. That is, since the bomb oxidation and sample oxidation methods are techniques using heating at high temperature, the separation methods of the radionuclides are relatively simple. However, since {sup 3}H radionuclide has a property of being diffused deeply into the inside of metals, {sup 3}H which is distributed on the surface of the metals can only be extracted if the methods are applied. As an another separation method, the wet oxidation method makes {sup 3}H oxidized with an acidic solution, and extracted completely to an oxidized HTO compound. However, incomplete oxidized {sup 3}H compounds, which are produced by reactions of acidic solutions and metallic radwastes, can be released into the air. Thus, in this study, a wet oxidation method to extract and quantify the {sup 3}H radionuclide from metallic radwastes was established. In particular, a complete extraction method and complete oxidation method of incomplete chemical compounds of {sup 3}H using a Pt catalyst were studied. The radioactivity of {sup 3}H in metallic radwastes is extracted and measured using a wet oxidation method and liquid scintillation counter. Considering the surface dose rate of the sample, the appropriate size of the sample was determined and weighed, and a mixture of oxidants was added to a 200 ml round flask with 3 tubes. The flask was quickly connected to the distilling apparatus. 20 mL of 16 wt% H{sub 2}SO{sub 4} was given into the 200-ml round flask through a dropping funnel while under stirring and refluxing. After dropping, the temperature of the mixture was raised to 96 deg. C and the sample was leached and oxidized by refluxing for 3 hours. At that time, the incomplete oxidized {sup 3}H compounds were

  5. A New Chelating Reagent: Its Synthesis/Characterization and Application for the Determination of Cd(II) and Ni(II) in Various Food and Make-Up Product Samples by FAAS Using Simultaneous Microextraction Sampling.

    PubMed

    Saçmacı, Şerife; Saçmacı, Mustafa

    2016-07-01

    A new and simple dispersive liquid-liquid simultaneous microextraction procedure was developed for the rapid separation and simultaneous extraction/preconcentration of Cd(II) and Ni(II) at ultratrace amounts. Microextraction of the analytes was carried out in the presence of 2-methyl-5-[(Z)-pyridin-4-yldiazenyl]quinolin-8-ol as the chelating reagent. Chloroform and ethanol were used as the extraction and dispersive solvents. Various parameters that influence the microextraction procedure's efficiency-such as pH, centrifugation rate and time, reagent concentration, and sampling volume on the recovery of analytes-were examined. The calibration curves were linear in the range of 0.01-1.25 and 0.075-5 mg/L with LODs of 0.25 and 0.84 μg/L, and with a preconcentration factor of 94, for Cd(II) and Ni(II), respectively. Precision was >1.0%. The accuracy of the method was confirmed by analyzing the Certified Standard Reference Material (CWW-TMD: Certified wastewater-Trace metals, wastewater). The results show that the dispersive liquid-liquid simultaneous microextraction pretreatment is a sensitive, rapid, simple, green, and safe method for the separation/preconcentration of cadmium and nickel.

  6. 21 CFR 866.4100 - Complement reagent.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Complement reagent. 866.4100 Section 866.4100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Immunology Laboratory Equipment and Reagents § 866.4100...

  7. 21 CFR 866.4100 - Complement reagent.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Complement reagent. 866.4100 Section 866.4100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Immunology Laboratory Equipment and Reagents § 866.4100...

  8. 21 CFR 866.4100 - Complement reagent.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Complement reagent. 866.4100 Section 866.4100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Immunology Laboratory Equipment and Reagents § 866.4100...

  9. 21 CFR 866.4100 - Complement reagent.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Complement reagent. 866.4100 Section 866.4100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Immunology Laboratory Equipment and Reagents § 866.4100...

  10. 21 CFR 866.4100 - Complement reagent.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Complement reagent. 866.4100 Section 866.4100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Immunology Laboratory Equipment and Reagents § 866.4100...

  11. The measurement of radiation exposure of astronauts by radiochemical techniques

    NASA Technical Reports Server (NTRS)

    Brodzinski, R. L.

    1971-01-01

    Gamma analyses of the neutron-activated fecal samples from the Apollo 12 and 13 missions were completed, and the data are being evaluated. Samples of the exposed Apollo 12 solar wind composition foil and blank foils were obtained for analysis of the Po-2/0 (Pb-210, Rn-222) content. It is expected that the determination of the Po-210 content of these foils will yield the concentration of radon atoms incident on the foil while exposed to the lunar atmosphere, and this indirectly will permit an estimate of the average uranium concentration of the lunar surface. Proposals to measure the cosmic-ray intensity and energy spectra inside and outside of late Apollo and Project Skylab spacecraft by exposing and subsequently analyzing pure metal foils, and to measure the elemental mass balance in Project Skylab astronauts by instrumental neutron activation analysis of the intake and excreta are summarized.

  12. The measurement of radiation exposure of astronauts by radiochemical techniques

    NASA Technical Reports Server (NTRS)

    Brodzinski, R. L.

    1972-01-01

    The principal gamma-ray emitting radioisotopes, produced in the body of astronauts by cosmic-ray bombardment, which have half-lives long enough to be useful for radiation dose evaluation, are Be-7, Na-22, and Na-24. The sodium isotopes were measured in the preflight and postflight urine and feces, and those feces specimens collected during the manned Apollo missions, by analysis of the urine salts and the raw feces in large crystal multidimensional gamma-ray spectrometers. The Be-7 was chemically separated, and its concentration measured in an all NaI (TL), anticoincidence shielded, scintillation well crystal. The astronaut radiation dose in millirads, as determined for the Apollo 7, 8, 9, 10, 11, 12, and 13 missions, was 330, 160, smaller than 315, 870 plus or minus 550, 31, 110, and smaller than 250, respectively.

  13. The measurement of radiation exposure of astronauts by radiochemical techniques

    NASA Technical Reports Server (NTRS)

    Brodzinski, R. L.

    1971-01-01

    The concentrations of 23 major, minor, and trace elements in the fecal samples from the Apollo 12 and 13 astronauts are reported. Most elemental excretion rates are comparable to rates reported for earlier missions. Exceptions are noted for calcium, iron, and tin. Body calcium and iron losses appear to be reduced during the Apollo 12 and 13 missions such that losses now seem to be insignificant. Refined measurements of tin excretion rates agree with normal dietary intakes. Earlier reported tin values are in error. A new passive dosimetry canister was designed which contains foils of tantalum, copper, titanium, iron, cobalt, aluminum, and scandium. By measuring the concentrations of the various products of nuclear reactions in these metals after space exposure, the characteristics of the incident cosmic particles can be determined.

  14. The Measurement of Radiation Exposure of Astronauts by Radiochemical Techniques

    NASA Technical Reports Server (NTRS)

    Brodzinski, R. L.

    1970-01-01

    The principal gamma-ray-omitting radioisotopes produced in the body of astronauts by cosmic-ray bombardment which have half-lives long enough to be useful for radiation dose evaluation are Be-7, Na-22, and Na-24. The sodium isotopes were measured in the preflight and postflight urine and feces, and those feces specimens collected during the manned Apollo missions, by analysis of the urine salts and the raw feces in large crystal multidimensional gamma-ray spectrometers. The Be-7 was chemically separated, and its concentration measured in an all Na(T1), anticoincidence shielded, scintillation well crystal. The overall sensitivity of the experiment was reduced by almost all variables such as low concentrations of excreted cosmogenic radionuclides, high concentrations of injected radionuclides, low sample sizes, long delay periods before analysis, and uncertain excretion rates. The astronaut radiation dose in millirads, as determined by this technique, for the Apollo 7, 8, 9, 10, 11, 12, and 13 missions was 330, 160, 315, 870 ? 550, 31, 110, and 250 respectively. In view of these limitations this technique would be best applied to cases of unusually high exposures, such as that encountered from solar flares.

  15. Radiochemical synthesis of 105gAg-labelled silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Ichedef, C.; Simonelli, F.; Holzwarth, U.; Bagaria, J. Piella; Puntes, V. F.; Cotogno, G.; Gilliland, D.; Gibson, N.

    2013-11-01

    A method for synthesis of radiolabelled silver nanoparticles is reported. The method is based on proton activation of silver metal powder, enriched in 107Ag, with a 30.7 MeV proton beam. At this proton energy 105gAg is efficiently created, mainly via the 107Ag(p,3n)105Cd → 105gAg reaction. 105gAg has a half-life of 41.29 days and emits easily detectable gamma radiation on decay to 105Pd. This makes it very useful as a tracing radionuclide for experiments over several weeks or months. Following activation and a period to allow short-lived radionuclides to decay, the powder was dissolved in concentrated nitric acid in order to form silver nitrate (AgNO3), which was used to synthesise radiolabelled silver nanoparticles via the process of sodium borohydride reduction. For comparison, non-radioactive silver nanoparticles were synthesised using commercially supplied AgNO3 in order to check if the use of irradiated Ag powder as a starting material would alter in any way the final nanoparticle characteristics. Both nanoparticle types were characterised using dynamic light scattering, zeta-potential and X-ray diffraction measurements, while additionally the non-radioactive samples were analysed by transmission electron microscopy and UV-Vis spectrometry. A hydrodynamic diameter of about 16 nm was determined for both radiolabelled and non-radioactive nanoparticles, while the electron microscopy on the non-radioactive samples indicated that the physical size of the metal NPs was (7.3 ± 1.4) nm.

  16. Critical ligand binding reagent preparation/selection: when specificity depends on reagents.

    PubMed

    Rup, Bonita; O'Hara, Denise

    2007-05-11

    Throughout the life cycle of biopharmaceutical products, bioanalytical support is provided using ligand binding assays to measure the drug product for pharmacokinetic, pharmacodynamic, and immunogenicity studies. The specificity and selectivity of these ligand binding assays are highly dependent on the ligand binding reagents. Thus the selection, characterization, and management processes for ligand binding reagents are crucial to successful assay development and application. This report describes process considerations for selection and characterization of ligand binding reagents that are integral parts of the different phases of assay development. Changes in expression, purification, modification, and storage of the ligand binding reagents may have a profound effect on the ligand binding assay performance. Thus long-term management of the critical ligand binding assay reagents is addressed including suggested characterization criteria that allow ligand binding reagents to be used in as consistent a manner as possible. Examples of challenges related to the selection, modification, and characterization of ligand binding reagents are included.

  17. Methodical aspects of blood coagulation measurements in birds applying commercial reagents--a pilot study.

    PubMed

    Guddorf, Vanessa; Kummerfeld, Norbert; Mischke, Reinhard

    2014-01-01

    The aim of this study was to examine the suitability of commercially available reagents for measurements of coagulation parameters in citrated plasma from birds. Therefore, plasma samples of 17 healthy donor birds of different species were used to determine prothrombin time (PT), activated partial thromboplastin time (aPTT) and thrombin time (TT) applying various commercial reagents which are routinely used in coagulation diagnostics in humans and mammals. A PT reagent based on human placental thromboplastin yielded not only shorter clotting times than a reagent containing recombinant human tissue factor (median 49 vs. 84 s), but also showed a minor range of distribution of values (43-55 s vs. 30-147 s, minimum-maximum, n = 5 turkeys). An aPTT reagent containing kaolin and phospholipids of animal origin delivered the shortest clotting times and the lowest range of variation in comparison to three other reagents of different composition. However, even when this reagent was used, aPTTs were partially extremely long (> 200 s). Thrombin time was 38 s (28-57 s, n = 5 chicken) when measured with bovine thrombin at a final concentration of 2 IU thrombin/ ml. Coefficients of variation for within-run precision analysis (20 repetitions) of PT was 8.0% and 4.7% for aPTT measurements using selected reagents of mammalian origin. In conclusion, of the commercially available reagents tested, a PT reagent based on human placental thromboplastin and an aPTT reagent including rabbit brain phospholipid and kaolin, show some promise for potential use in birds.

  18. Validity of HydraTrend reagent strips for the assessment of hydration status.

    PubMed

    Abbey, Bryce M; Heelan, Kate A; Brown, Gregory A; Bartee, Rodrick T

    2014-09-01

    Hydration is used by athletic governing organizations for weight class eligibility. The measurement of urine specific gravity (USG) as a measure of hydration by reagent strips is a controversial issue. The purpose of this study was to determine the validity of HydraTrend reagent strips that facilitate the correction of USG for alkaline urine samples against refractometry for the assessment of USG. Fifty-one participants (33 males, age = 22.3 ± 1.3 years; 18 females, age = 22.4 ± 1.2 years) provided 84 urine samples. The samples were tested for USG using refractometry and reagent strips and for pH using reagent strips and a digital pH meter. Strong correlation coefficients were found between refractometry and reagent strips for USG (rs(82) = 0.812, p < 0.01) and between reagent strips and pH meter for pH (rs(82) = 0.939, p < 0.01). It was observed that false negative results for National Collegiate Athletic Association (NCAA) requirements (fail refractometry with USG >1.020, pass reagent strips with USG ≤1.020) occurred 39% (33/84) of the time and false negative results for National Federation of State High School Association (NFHS) requirements (fail refractometry with USG >1.025, pass reagent strips with USG ≤1.025) occurred 14% (12/84) of the time. There were no false positives (pass refractometry and fail reagent strips) for NCAA or NFHS requirements. These data show that refractometry and reagent strips have strong positive correlations. However, the risk of a false negative result leading to incorrect certification of euhydration status outweighs the benefits of the HydraTrend reagent strips for the measurement of USG.

  19. Immobilized Bioluminescent Reagents in Flow Injection Analysis.

    NASA Astrophysics Data System (ADS)

    Nabi, Abdul

    Available from UMI in association with The British Library. Bioluminescent reactions exhibits two important characteristics from an analytical viewpoint; they are selective and highly sensitive. Furthermore, bioluminescent emissions are easily measured with a simple flow-through detector based on a photomultiplier tube and the rapid and reproducible mixing of sample and expensive reagent is best achieved by a flow injection manifold. The two most important bioluminescent systems are the enzyme (luciferase)/substrate (luciferin) combinations extracted from fireflies (Photinus pyralis) and marine bacteria (Virio harveyi) which requires ATP and NAD(P)H respectively as cofactors. Reactions that generate or consume these cofactors can also be coupled to the bioluminescent reaction to provide assays for a wide range of clinically important species. A flow injection manifold for the study of bioluminescent reactions is described, as are procedures for the extraction, purification and immobilization of firefly and bacterial luciferase and oxidoreductase. Results are presented for the determination of ATP using firefly system and the determination of other enzymes and substrates participating in ATP-converting reactions e.g. creatine kinase, ATP-sulphurylase, pyruvate kinase, creatine phosphate, pyrophosphate and phophoenolypyruvate. Similarly results are presented for the determination of NAD(P)H, FMN, FMNH_2 and several dehydrogenases which produce NAD(P)H and their substrates, e.g. alcohol, L-lactate, L-malate, L-glutamate, Glucose-6-phosphate and primary bile acid.

  20. Stoichiometric and irreversible cysteine-selective protein modification using carbonylacrylic reagents

    PubMed Central

    Bernardim, Barbara; Cal, Pedro M.S.D.; Matos, Maria J.; Oliveira, Bruno L.; Martínez-Sáez, Nuria; Albuquerque, Inês S.; Perkins, Elizabeth; Corzana, Francisco; Burtoloso, Antonio C.B.; Jiménez-Osés, Gonzalo; Bernardes, Gonçalo J. L.

    2016-01-01

    Maleimides remain the reagents of choice for the preparation of therapeutic and imaging protein conjugates despite the known instability of the resulting products that undergo thiol-exchange reactions in vivo. Here we present the rational design of carbonylacrylic reagents for chemoselective cysteine bioconjugation. These reagents undergo rapid thiol Michael-addition under biocompatible conditions in stoichiometric amounts. When using carbonylacrylic reagents equipped with PEG or fluorophore moieties, this method enables access to protein and antibody conjugates precisely modified at pre-determined sites. Importantly, the conjugates formed are resistant to degradation in plasma and are biologically functional, as demonstrated by the selective imaging and detection of apoptotic and HER2+ cells, respectively. The straightforward preparation, stoichiometric use and exquisite cysteine selectivity of the carbonylacrylic reagents combined with the stability of the products and the availability of biologically relevant cysteine-tagged proteins make this method suitable for the routine preparation of chemically defined conjugates for in vivo applications. PMID:27782215

  1. Stoichiometric and irreversible cysteine-selective protein modification using carbonylacrylic reagents

    NASA Astrophysics Data System (ADS)

    Bernardim, Barbara; Cal, Pedro M. S. D.; Matos, Maria J.; Oliveira, Bruno L.; Martínez-Sáez, Nuria; Albuquerque, Inês S.; Perkins, Elizabeth; Corzana, Francisco; Burtoloso, Antonio C. B.; Jiménez-Osés, Gonzalo; Bernardes, Gonçalo J. L.

    2016-10-01

    Maleimides remain the reagents of choice for the preparation of therapeutic and imaging protein conjugates despite the known instability of the resulting products that undergo thiol-exchange reactions in vivo. Here we present the rational design of carbonylacrylic reagents for chemoselective cysteine bioconjugation. These reagents undergo rapid thiol Michael-addition under biocompatible conditions in stoichiometric amounts. When using carbonylacrylic reagents equipped with PEG or fluorophore moieties, this method enables access to protein and antibody conjugates precisely modified at pre-determined sites. Importantly, the conjugates formed are resistant to degradation in plasma and are biologically functional, as demonstrated by the selective imaging and detection of apoptotic and HER2+ cells, respectively. The straightforward preparation, stoichiometric use and exquisite cysteine selectivity of the carbonylacrylic reagents combined with the stability of the products and the availability of biologically relevant cysteine-tagged proteins make this method suitable for the routine preparation of chemically defined conjugates for in vivo applications.

  2. Model fluids representing aqueous in-vitro diagnostic reagents for the development of dispensing systems.

    PubMed

    Losleben, Nadine; Spinke, Jürgen; Adler, Sabrina; Oranth, Norbert; Zengerle, Roland

    2013-11-01

    Analyzers for in-vitro diagnostic (IVD) testing facilitate the determination of medical information from biological samples. To reach a high quality, the detection reagents have to be dispensed with a high degree of precision and accuracy. A technology change from conventional pipetting systems to contact-free dispensers provides the opportunity to reduce carry-over and handle reagents in the microliter range. A great challenge for the development and validation of new systems is the huge variety of the IVD reagents. This work presents the fluidic properties of 646 different aqueous IVD reagents and how they can be represented by a set of easy-to-prepare model fluids, covering the rheological range of the reagents. In addition, based on the model fluids, a standardized approach is presented for the evaluation of dispensers for IVD applications.

  3. Optimizing Transfection of Primary Human Umbilical Vein Endothelial Cells Using Commercially Available Chemical Transfection Reagents

    PubMed Central

    Hunt, Michelle A.; Currie, Margaret J.; Robinson, Bridget A.; Dachs, Gabi U.

    2010-01-01

    Primary cells, such as HUVEC, are notoriously difficult to transfect and are susceptible to the toxic effects of transfection reagents. A transfection reagent with a high transfection efficiency and low cytotoxicity was sought to retain sufficient viability of transfected HUVEC for subsequent assays. Nine chemical transfection reagents, currently commercially available, were compared for their ability to transfect HUVEC in vitro. A plasmid expressing the enhanced GFP (EGFP) was used for transfection, followed by flow cytometry of transfected HUVEC to determine the proportion of EGFP-expressing cells as a measure of transfection efficiency. Lipofectamine 2000 and Lipofectamine LTX (Invitrogen, Carlsbad, CA, USA) gave the highest transfection efficiencies of the reagents tested. Lipofectamine LTX was identified as the optimal transfection reagent as a result of its higher transfection efficiency at shorter periods of time following transfection when cytotoxicity was limited, allowing sufficient yield of transfected HUVEC for use in subsequent assays. PMID:20592869

  4. Effects of the order of addition of reagents and alkali on modification of wheat starches.

    PubMed

    Sui, Zhongquan; Huber, Kerry C; BeMiller, James N

    2015-07-10

    The objective of this research was to determine if adding reactive reagents to wheat starch granules before addition of alkali (the TRF method) would produce products that are different than those obtained with the conventional procedure (adding alkali before addition of reagent). Laboratory-isolated (LI) and commercial (C) normal (NWS) and waxy (WWS) wheat starches were each reacted with 6 reagents (acetic-adipic mixed anhydride (AAMA), phosphoryl chloride (POCl3), sodium trimetaphosphate (STMP), acetic anhydride (AA), succinic anhydride (SA), octenylsuccinic anhydride (OSA)). Data obtained were similar to those previously obtained with maize starches (Sui, Huber, & BeMiller, 2013). Almost no starch polymer molecule modification occurred when the TRF method and AAMA or AA were used; less than a third as much reaction when SA was the reagent used, and about the same amount of reaction when POCl3, STMP, or OSA were the reagents used (for different reasons).

  5. Radiochemical processes in polymer films containing N,N,N{sup {prime}},N{sup {prime}}-tetra-methyl-4,4{sup {prime}}-diaminodiphenylmethane induced by accelerated electron pulses

    SciTech Connect

    Kolotilkin, A.S.; Tkachev, V.A.; Mal`tsev, E.I.; Vannikov, A.V.

    1992-01-01

    The mechanism of radiochemical oxidation of N,N,N{prime},N{prime}-tetramethyl-4,4{prime}-diaminodiphenylmethane (TMDH) in solid solutions of polyvinyl chloride (PVC) and polyethyl methacrylate (PMMA) in the presence and absence of an electron acceptor, CBr{sub 4}, was investigated by pulsed radiolysis. The absorption spectra were recorded and the short-lived products of radiolysis of TMDH were identified. The radiochemical yields were determined and the rate constants of formation of a stable colored product of radiolysis, Michler`s Hydrol, were calculated. The rate constants for the PVC-TMDH-CBr{sub 4} and PMMA-TMDH-CBr{sub 4} systems were respectively equal to 240 {plus_minus} 25 and 20 {plus_minus} 3 sec{sup -1}. 15 refs., 3 figs., 1 tab.

  6. Recommendations for appropriate activated partial thromboplastin time reagent selection and utilization.

    PubMed

    Fritsma, George A; Dembitzer, Francine R; Randhawa, Ankush; Marques, Marisa B; Van Cott, Elizabeth M; Adcock-Funk, Dorothy; Peerschke, Ellinor I

    2012-06-01

    The activated partial thromboplastin time (aPTT) is widely used as a screening coagulation test and for monitoring unfractionated heparin therapy. Various commercial reagents are available, with different performance characteristics, particularly responsiveness to the lupus anticoagulant (LA). Because aPTT reagent selection significantly affects the interpretation of results, we reviewed College of American Pathologists proficiency testing data involving approximately 4,000 coagulation laboratories, and conducted a survey of coagulation laboratories (n = 93) using The Fritsma Factor hemostasis Web site to determine the basis for aPTT reagent selection. The data demonstrate that for routine aPTT testing, most laboratories use reagents with high/moderate responsiveness to LA. Significant misunderstanding was apparent regarding the use of appropriate aPTT reagent for routine testing and LA identification. We recommend aPTT reagents with low LA responsiveness to screen for coagulation factor deficiencies and heparin monitoring, and suggest continued education of laboratory professionals and reagent manufacturers about appropriate aPTT reagent use.

  7. Inactivation of rabies diagnostic reagents by gamma radiation

    SciTech Connect

    Gamble, W.C.; Chappell, W.A.; George, E.H.

    1980-11-01

    Treatment of CVS-11 rabies adsorbing suspensions and street rabies infected mouse brains with gamma radiation resulted in inactivated reagents that are safer to distribute and use. These irradiated reagents were as sensitive and reactive as the nonirradiated control reagents.

  8. 21 CFR 866.3740 - Streptococcus spp. serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3740 Streptococcus spp. serological reagents. (a) Identification. Streptococcus spp. serological reagents are devices... streptococci are associated with infections, such as sore throat, impetigo (an infection characterized by...

  9. Synthesis of the isotope-labeled derivatization reagent for carboxylic acids, 7-(N,N-dimethylaminosulfonyl)-4-(aminoethyl)piperazino-2,1,3-benzoxadiazole (d6) [DBD-PZ-NH2 (D)], and its application to the quantification and the determination of relative amount of fatty acids in rat plasma samples by high-performance liquid chromatography/mass spectrometry.

    PubMed

    Tsukamoto, Yuhki; Santa, Tomofumi; Yoshida, Hiroo; Miyano, Hiroshi; Fukushima, Takeshi; Hirayama, Kazuo; Imai, Kazuhiro; Funatsu, Takashi

    2006-04-01

    The isotope-labeled benzofurazan derivatization reagent for carboxylic acids, 7-(N,N-dimethylaminosulfonyl)-4-(aminoethyl)piperazino-2,1,3-benzoxadiazole (d6) [DBD-PZ-NH2 (D)] was synthesized. DBD-PZ-NH2 (D) was used for the accurate quantification of fatty acids by liquid chromatography/mass spectrometry (LC/MS). The standard fatty acids were derivatized with DBD-PZ-NH2 (D) to the stable isotope-labeled compounds for the fatty acids derivatives of DBD-PZ-NH2 and used for the internal standards. The obtained calibration curves for fatty acids were linear over the range 0.1-200 microM (r2 > 0.999). Fatty acids in plasma samples were determined after derivatization with DBD-PZ-NH2 and analyzed by LC/MS using standard fatty acid DBD-PZ-NH2 (D) derivatives as internal standards. Furthermore, the relative amounts of fatty acids in two plasma samples were determined after derivatization with DBD-PZ-NH2 and DBD-PZ-NH2) (D). The isotope-labeled derivatization reagent was useful for accurate quantification and the determination of relative amounts of the metabolites in biological samples having the target functional group.

  10. Conceptual Design for the Pilot-Scale Plutonium Oxide Processing Unit in the Radiochemical Processing Laboratory

    SciTech Connect

    Lumetta, Gregg J.; Meier, David E.; Tingey, Joel M.; Casella, Amanda J.; Delegard, Calvin H.; Edwards, Matthew K.; Jones, Susan A.; Rapko, Brian M.

    2014-08-05

    This report describes a conceptual design for a pilot-scale capability to produce plutonium oxide for use as exercise and reference materials, and for use in identifying and validating nuclear forensics signatures associated with plutonium production. This capability is referred to as the Pilot-scale Plutonium oxide Processing Unit (P3U), and it will be located in the Radiochemical Processing Laboratory at the Pacific Northwest National Laboratory. The key unit operations are described, including plutonium dioxide (PuO2) dissolution, purification of the Pu by ion exchange, precipitation, and conversion to oxide by calcination.

  11. Radiochemical neutron activation analysis for certification of ion-implanted phosphorus in silicon.

    PubMed

    Paul, Rick L; Simons, David S; Guthrie, William F; Lu, John

    2003-08-15

    A radiochemical neutron activation analysis procedure has been developed, critically evaluated, and shown to have the necessary sensitivity, chemical specificity, matrix independence, and precision to certify phosphorus at ion implantation levels in silicon. 32P, produced by neutron capture of 31P, is chemically separated from the sample matrix and measured using a beta proportional counter. The method is used here to certify the amount of phosphorus in SRM 2133 (Phosphorus Implant in Silicon Depth Profile Standard) as (9.58 +/- 0.16) x 10(14) atoms x cm(-2). A detailed evaluation of uncertainties is given.

  12. Preparation of Radiochemical-Labeled Compounds for the U.S. Army Drug Development Program

    DTIC Science & Technology

    1992-04-20

    which was 95% radiochemically pure. Recrystal- lization of the preduct from methanol- water 6 failed to improve its purity, but purification was...chloroperbonzoic acid (MCPBA) gave 12.3 mCi (61% yield) of [14 C]-8 after purification by chromatography on alumina (basic, Act I1I). A s.,cond portion (48.8 mCi...of [14C]-7 was sixt- larly oxidized, but gave only 14 mCi (14% yield) of [14C]-_ after purification by chromatography. The lower yield was attributed

  13. Energy and Water Conservation Assessment of the Radiochemical Processing Laboratory (RPL) at Pacific Northwest National Laboratory

    SciTech Connect

    Johnson, Stephanie R.; Koehler, Theresa M.; Boyd, Brian K.

    2014-05-31

    This report summarizes the results of an energy and water conservation assessment of the Radiochemical Processing Laboratory (RPL) at Pacific Northwest National Laboratory (PNNL). The assessment was performed in October 2013 by engineers from the PNNL Building Performance Team with the support of the dedicated RPL staff and several Facilities and Operations (F&O) department engineers. The assessment was completed for the Facilities and Operations (F&O) department at PNNL in support of the requirements within Section 432 of the Energy Independence and Security Act (EISA) of 2007.

  14. Dielectric and mechanical spectroscopies for the study of thermal and radiochemical ageing of polymers

    NASA Astrophysics Data System (ADS)

    Boiteux, G.; Chailan, J. F.; Chauchard, J.; Seytre, G.

    1997-08-01

    Thermal and/or radiochemical ageing of polymer has been extensively studied by thermal, FTIR, UV or static mechanical analysis. The aim of this work was to make a parallel study of dynamic mechanical and dielectrical properties of EPDM elastomers, and to present the possibility of using such methods for studying ageing. These analyses reflect not only the molecular dynamic, but also through dielectric spectroscopy the chemical evolution due to modification of dipolar species. Changes in the main relaxation peak, both in mechanical and dielectrical spectra, allow the degradation to be quantified.

  15. Design of the Laboratory-Scale Plutonium Oxide Processing Unit in the Radiochemical Processing Laboratory

    SciTech Connect

    Lumetta, Gregg J.; Meier, David E.; Tingey, Joel M.; Casella, Amanda J.; Delegard, Calvin H.; Edwards, Matthew K.; Orton, Robert D.; Rapko, Brian M.; Smart, John E.

    2015-05-01

    This report describes a design for a laboratory-scale capability to produce plutonium oxide (PuO2) for use in identifying and validating nuclear forensics signatures associated with plutonium production, as well as for use as exercise and reference materials. This capability will be located in the Radiochemical Processing Laboratory at the Pacific Northwest National Laboratory. The key unit operations are described, including PuO2 dissolution, purification of the Pu by ion exchange, precipitation, and re-conversion to PuO2 by calcination.

  16. The Radiochemical Analysis of Gaseous Samples (RAGS) apparatus for nuclear diagnostics at the National Ignition Facility (invited)

    SciTech Connect

    Shaughnessy, D. A.; Velsko, C. A.; Jedlovec, D. R.; Yeamans, C. B.; Moody, K. J.; Tereshatov, E.; Stoeffl, W.; Riddle, A.

    2012-10-15

    The Radiochemical Analysis of Gaseous Samples (RAGS) diagnostic apparatus was recently installed at the National Ignition Facility (NIF). Following a NIF shot, RAGS is used to pump the gas load from the NIF chamber for purification and isolation of the noble gases. After collection, the activated gaseous species are counted via gamma spectroscopy for measurement of the capsule areal density and fuel-ablator mix. Collection efficiency was determined by injecting a known amount of {sup 135}Xe into the NIF chamber, which was then collected with RAGS. Commissioning was performed with an exploding pusher capsule filled with isotopically enriched {sup 124}Xe and {sup 126}Xe added to the DT gas fill. Activated xenon species were recovered post-shot and counted via gamma spectroscopy. Results from the collection and commissioning tests are presented. The performance of RAGS allows us to establish a noble gas collection method for measurement of noble gas species produced via neutron and charged particle reactions in a NIF capsule.

  17. Laser Raman spectroscopy and omegatron mass spectrometry applied to investigations of the radiochemical reactions between methane and tritium

    SciTech Connect

    Engelmann, U.; Glugla, M.; Penzhorn, R.D.; Ache, H.J. . Inst. fuer Radiochemie)

    1992-03-01

    This paper reports that the radiochemical reactions between methane and tritium were vicariously chosen for the evaluation of an omegatron type mass spectrometer and a laser Raman spectrometer in view of their analytical application in tritium systems. Assessment of the omegatron was extended beyond previous work on the quantitative analysis of all hydrogen isotopes and stable helium isotopes to include the determination of tritiated hydrocarbons. As opposed to mass spectrometry, laser Raman spectroscopy is an absolute method, which in principle is applicable to all polyatomic gases. For the employment in tritium systems an uhv-tight stainless steel gas cell using windows mounted in CF flanges with a flatness better than 1 lambda was constructed and tested. The Raman spectra of H{sub 2}, HD and D{sub 2} were measured and the pure rotation and rotation vibration branches assigned. The fundamental vibrations of methane and deuterated methanes have also been identified. First kinetic data on the {beta}-radiation induced exchange reaction between tritium and methane have been obtained with an omegatron.

  18. Evaluation of Two Spot-Indole Reagents

    PubMed Central

    Lowrance, B. L.; Reich, P.; Traub, W. H.

    1969-01-01

    Two spot-indole reagents, p-dimethylaminobenzaldehyde (DMABA) and p-dimethylaminocinnamaldehyde, were evaluated quantitatively. Although fourfold less sensitive, DMABA proved to be more stable and economical. PMID:4894726

  19. Iodine(III) Reagents in Radical Chemistry

    PubMed Central

    2017-01-01

    Conspectus The chemistry of hypervalent iodine(III) compounds has gained great interest over the past 30 years. Hypervalent iodine(III) compounds show valuable ionic reactivity due to their high electrophilicity but also express radical reactivity as single electron oxidants for carbon and heteroatom radical generation. Looking at ionic chemistry, these iodine(III) reagents can act as electrophiles to efficiently construct C–CF3, X–CF3 (X = heteroatom), C–Rf (Rf = perfluoroalkyl), X–Rf, C–N3, C–CN, S–CN, and C–X bonds. In some cases, a Lewis or a Bronsted acid is necessary to increase their electrophilicity. In these transformations, the iodine(III) compounds react as formal “CF3+”, “Rf+”, “N3+”, “Ar+”, “CN+”, and “X+” equivalents. On the other hand, one electron reduction of the I(III) reagents opens the door to the radical world, which is the topic of this Account that focuses on radical reactivity of hypervalent iodine(III) compounds such as the Togni reagent, Zhdankin reagent, diaryliodonium salts, aryliodonium ylides, aryl(cyano)iodonium triflates, and aryl(perfluoroalkyl)iodonium triflates. Radical generation starting with I(III) reagents can also occur via thermal or light mediated homolysis of the weak hypervalent bond in such reagents. This reactivity can be used for alkane C–H functionalization. We will address important pioneering work in the area but will mainly focus on studies that have been conducted by our group over the last 5 years. We entered the field by investigating transition metal free single electron reduction of Togni type reagents using the readily available sodium 2,2,6,6-tetramethylpiperidine-1-oxyl salt (TEMPONa) as an organic one electron reductant for clean generation of the trifluoromethyl radical and perfluoroalkyl radicals. That valuable approach was later successfully also applied to the generation of azidyl and aryl radicals starting with the corresponding benziodoxole (Zhdankin reagent

  20. A simple and rapid technique for radiochemical separation of iodine radionuclides from irradiated tellurium using an activated charcoal column.

    PubMed

    Chattopadhyay, Sankha; Saha Das, Sujata

    2009-10-01

    A simple and inexpensive method for the separation of medically useful no-carrier-added (nca) iodine radionuclides from bulk amounts of irradiated tellurium dioxide (TeO(2)) target was developed. The beta(-) emitting (131)I radionuclide, produced by the decay of (131)Te through the (nat)Te(n, gamma)(131)Te nuclear reaction, was used for standardization of the radiochemical separation procedure. The radiochemical separation was performed by precipitation followed by column (activated charcoal) chromatography. Quantitative post-irradiation recovery of the TeO(2) target material (98-99%), in a form suitable for reuse in future irradiations, was achieved. The overall radiochemical yield for the complete separation of (131)I was 75-85% (n=8). The separated nca (131)I was of high, approximately 99%, radionuclidic and radiochemical purities and did not contain detectable amounts of the target material. This method can be adopted for the radiochemical separation of other different iodine radionuclides produced from tellurium matrices through cyclotron as well as reactor irradiation.

  1. Use of fission track analysis technique for the determination of MicroBequerel level of 239Pu in urine samples from radiation workers handling MOX fuel.

    PubMed

    Yadav, J R; Rao, D D; Kumar, Ranjeet; Aggarwal, S K

    2011-07-01

    Fission track analysis (FTA) technique for the determination of (239)Pu excreted through urine has been standardized using blank samples, tracer and (239)Pu spikes. Double stage anion exchange separation protocol has been applied and an average radiochemical recovery of (239)Pu of 18% was obtained. An average track registration efficiency of 11 tracks per μBq of (239)Pu, irradiated to 0.35×10(17) 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 34μBqL(-1) of urine sample was obtained and will be useful for monitoring chronic exposure cases handling MOX fuel.

  2. Spectroscopic Online Monitoring for Process Control and Safeguarding of Radiochemical Fuel Reprocessing Streams

    SciTech Connect

    Bryan, Samuel A.; Levitskaia, Tatiana G.; Casella, Amanda J.; Peterson, James M.

    2013-02-24

    There is a renewed interest worldwide to promote the use of nuclear power and close the nuclear fuel cycle. The long term successful use of nuclear power is critically dependent upon adequate and safe processing and disposition of the spent nuclear fuel. Liquid-liquid extraction is a separation technique commonly employed for the processing of the dissolved spent nuclear fuel. The instrumentation used to monitor these processes must be robust, require little or no maintenance, and be able to withstand harsh environments such as high radiation fields and aggressive chemical matrices. In addition, the ability for continuous online monitoring allows for numerous benefits. This paper reviews application of the absorption and vibrational spectroscopic techniques supplemented by physicochemical measurements for radiochemical process monitoring. In this context, our team experimentally assessed the potential of Raman and spectrophotometric techniques for on-line real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. Both techniques demonstrated robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Static spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. Satisfactory prediction of the analytes concentrations in these preliminary experiments warrants further development of the spectroscopy-based methods for radiochemical safeguards and process control.

  3. On the Radiochemical Separations of the Beta-emitting Fission Products

    NASA Astrophysics Data System (ADS)

    Chang, Zheng; Sudowe, Ralf

    2013-04-01

    This research aims at developing fast and effective radiochemical procedures for separation of the beta-emitting fission products that are difficult to analyze by gamma-spectrometry. Post-detonation analysis, as one of the major tasks of nuclear forensics, can provide crucial information for identification of the explosion levels, fuel sources, and industrial processes of a nuclear device. However, a dozen of radionuclides with high fission yields such as Zr-93, Tc-99, Sr-90 are either pure beta-emitters or only emitting gamma-rays that are difficult to analyze. Although the analysis of these radionuclides was thoroughly studied, samples from unknown nuclear detonations can be complicated by the number of fission products, radioactivity levels, sample matrices, and time limits for analysis. The challenge facing the forensic analysis should not be underestimated. A sequential separation procedure is designed to analyze the major beta-emitting fission products. Radiochemical techniques such as solvent extraction, precipitation, and column chromatography are utilized. The procedure will be tested and improved by experiments. The final procedure should be capable of analyzing the fission products under various sample conditions effectively and rapidly.

  4. Spectroscopic Online Monitoring for Process Control and Safeguarding of Radiochemical Fuel Reprocessing Streams - 13553

    SciTech Connect

    Bryan, S.A.; Levitskaia, T.G.; Casella, Amanda; Peterson, James

    2013-07-01

    There is a renewed interest worldwide to promote the use of nuclear power and close the nuclear fuel cycle. The long term successful use of nuclear power is critically dependent upon adequate and safe processing and disposition of the used nuclear fuel. Liquid-liquid extraction is a separation technique commonly employed for the processing of the dissolved spent nuclear fuel. The instrumentation used to monitor these processes must be robust, require little or no maintenance, and be able to withstand harsh environments such as high radiation fields and aggressive chemical matrices. This paper discusses application of absorption and vibrational spectroscopic techniques supplemented by physicochemical measurements for radiochemical process monitoring. In this context, our team experimentally assessed the potential of Raman and spectrophotometric techniques for on-line real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. Both techniques demonstrated robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Static spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. Satisfactory prediction of the analytes concentrations in these preliminary experiments warrants further development of the spectroscopy-based methods for radiochemical safeguards and process control. (authors)

  5. Spectroscopic online monitoring for process control and safeguarding of radiochemical streams

    SciTech Connect

    Bryan, S.A.; Levitskaia, T.G.

    2013-07-01

    This paper summarizes application of the absorption and vibrational spectroscopic techniques supplemented by physicochemical measurements for radiochemical process monitoring. In this context, our team experimentally assessed the potential of Raman and spectrophotometric techniques for online real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. These techniques demonstrate robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. Satisfactory prediction of the analytes concentrations in these preliminary experiments warrants further development of the spectroscopy-based methods for radiochemical process control and safeguarding. Additionally, the ability to identify material intentionally diverted from a liquid-liquid extraction contactor system was successfully tested using on-line process monitoring as a means to detect the amount of material diverted. (authors)

  6. Suppression of thiol exchange reaction in the determination of reduced-form thiols by high-performance liquid chromatography with fluorescence detection after derivatization with fluorogenic benzofurazan reagent, 7-fluoro-2,1,3-benzoxadiazole-4-sulfonate and 4-aminosulfonyl-7-fluoro-2,1,3-benzoxadiazole.

    PubMed

    Santa, Tomofumi; Aoyama, Chiaki; Fukushima, Takeshi; Imai, Kazuhiro; Funatsu, Takashi

    2006-01-01

    The derivatization of the reduced-form thiols with SBD-F (7-fluoro-2,1,3-benzoxadiazole-4-sulfonate) and ABD-F (4-aminosulfonyl-7-fluoro-2,1,3-benzoxadiazole) was studied. The yields of the derivatives of the reduced-form thiols (cysteine, homocysteine, reduced-form glutathione) with SBD-F at 60 degrees C for 45 min in the borate buffer (pH 9.3) were significantly decreased in the presence of the oxidized-form thiols (cystine, homocystine, oxidized-form glutathione) because of the thiol exchange reaction between the reduced-form and the oxidized-form thiols. The use of ABD-F at low temperature enabled the suppression of these thiol exchange reactions, and the recommended conditions were below 5 degrees C for 90 min in borate buffer (pH 9.3). These results suggest that ABD-F is a preferred derivatization reagent for the accurate determination of the reduced-form thiols in samples containing the oxidized-form thiols. In addition, it was also suggested that the derivatization of the reduced-form thiols should also be performed at low temperature when derivatization reagents such as o-phthalaldehyde (OPA) and monobromobimane (BrB) are used.

  7. Identification and determination of carboxylic acids in food samples using 2-(2-(anthracen-10-yl)-1H-phenanthro[9,10-d]imidazol-1-yl)ethyl 4-methylbenzenesulfonate (APIETS) as labeling reagent by HPLC with FLD and APCI/MS.

    PubMed

    Sun, Zhiwei; You, Jinmao; Song, Cuihua; Xia, Lian

    2011-08-15

    A new labeling reagent for carboxylic acids, 2-(2-(anthracen-10-yl)-1H-phenanthro[9,10-d]imidazol-1-yl)ethyl 4-methylbenzenesulfonate (APIETS) has been designed and synthesized. It was used to label eight fatty acids (lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, oleic acid, linoleic acid and linolenic acid) and four hydroxy pentacyclic triterpene acids (oleanolic acid, ursolic acid, betulinic acid and maslinic acid), successfully. APIETS could easily and quickly label carboxylic acids in the presence of K(2)CO(3) catalyst at 85°C for 35 min in N,N-dimethylformamide solvent. The carboxylic acids derivatives were separated on a C(8) reversed-phase column with gradient elution and fluorescence detection at λ(ex)/λ(em)=315/435 nm. Identification of these derivatives was carried out by online mass spectrometry with atmospheric pressure chemical ionization in positive ion mode. The detection limits obtained were 13.37-30.26fmol (signal-to-noise ratio of 3). The proposed method has been applied to the quantification of carboxylic acids in sultana raisin (Thompson seedless), hawthorn flake (Crataegus pinnatifida Bge.), Lycium barbarum seed oil and Microula sikkimensis seed oil with recoveries over 95.3%. It has been demonstrated that APIETS is a prominent labeling reagent for determining carboxylic acids with high performance liquid chromatography.

  8. 21 CFR 660.30 - Reagent Red Blood Cells.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 7 2011-04-01 2010-04-01 true Reagent Red Blood Cells. 660.30 Section 660.30 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Reagent Red Blood Cells § 660.30 Reagent Red Blood Cells. (a) Proper name and definition. The proper name of the product shall be Reagent...

  9. 21 CFR 866.3120 - Chlamydia serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Chlamydia serological reagents. 866.3120 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3120 Chlamydia serological reagents. (a) Identification. Chlamydia serological reagents are devices that consist of antigens...

  10. 21 CFR 866.3120 - Chlamydia serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Chlamydia serological reagents. 866.3120 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3120 Chlamydia serological reagents. (a) Identification. Chlamydia serological reagents are devices that consist of antigens...

  11. 21 CFR 866.3120 - Chlamydia serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Chlamydia serological reagents. 866.3120 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3120 Chlamydia serological reagents. (a) Identification. Chlamydia serological reagents are devices that consist of antigens...

  12. 21 CFR 866.3380 - Mumps virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Mumps virus serological reagents. 866.3380 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3380 Mumps virus serological reagents. (a) Identification. Mumps virus serological reagents consist of antigens and antisera...

  13. 21 CFR 866.3510 - Rubella virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Rubella virus serological reagents. 866.3510... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3510 Rubella virus serological reagents. (a) Identification. Rubella virus serological reagents are devices that consist of...

  14. 21 CFR 866.3380 - Mumps virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Mumps virus serological reagents. 866.3380 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3380 Mumps virus serological reagents. (a) Identification. Mumps virus serological reagents consist of antigens and antisera...

  15. 21 CFR 866.3510 - Rubella virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Rubella virus serological reagents. 866.3510... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3510 Rubella virus serological reagents. (a) Identification. Rubella virus serological reagents are devices that consist of...

  16. 21 CFR 866.3510 - Rubella virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Rubella virus serological reagents. 866.3510... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3510 Rubella virus serological reagents. (a) Identification. Rubella virus serological reagents are devices that consist of...

  17. 21 CFR 866.3380 - Mumps virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Mumps virus serological reagents. 866.3380 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3380 Mumps virus serological reagents. (a) Identification. Mumps virus serological reagents consist of antigens and antisera...

  18. 21 CFR 866.3510 - Rubella virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Rubella virus serological reagents. 866.3510... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3510 Rubella virus serological reagents. (a) Identification. Rubella virus serological reagents are devices that consist of...

  19. 21 CFR 866.3380 - Mumps virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Mumps virus serological reagents. 866.3380 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3380 Mumps virus serological reagents. (a) Identification. Mumps virus serological reagents consist of antigens and antisera...

  20. 21 CFR 866.3510 - Rubella virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Rubella virus serological reagents. 866.3510... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3510 Rubella virus serological reagents. (a) Identification. Rubella virus serological reagents are devices that consist of...

  1. 21 CFR 866.3380 - Mumps virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Mumps virus serological reagents. 866.3380 Section... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3380 Mumps virus serological reagents. (a) Identification. Mumps virus serological reagents consist of antigens and antisera...

  2. 40 CFR 160.83 - Reagents and solutions.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Reagents and solutions. 160.83 Section... LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 160.83 Reagents and solutions. All reagents and... requirements, and expiration date. Deteriorated or outdated reagents and solutions shall not be used....

  3. 21 CFR 866.3940 - West Nile virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false West Nile virus serological reagents. 866.3940... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3940 West Nile virus serological reagents. (a) Identification. West Nile virus serological reagents are devices that...

  4. 21 CFR 864.8540 - Red cell lysing reagent.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Red cell lysing reagent. 864.8540 Section 864.8540...) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8540 Red cell lysing reagent. (a) Identification. A red cell lysing reagent is a device used to lyse (destroy) red blood cells for...

  5. 21 CFR 864.8540 - Red cell lysing reagent.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Red cell lysing reagent. 864.8540 Section 864.8540...) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8540 Red cell lysing reagent. (a) Identification. A red cell lysing reagent is a device used to lyse (destroy) red blood cells for...

  6. 21 CFR 864.8540 - Red cell lysing reagent.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Red cell lysing reagent. 864.8540 Section 864.8540...) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8540 Red cell lysing reagent. (a) Identification. A red cell lysing reagent is a device used to lyse (destroy) red blood cells for...

  7. 21 CFR 864.8540 - Red cell lysing reagent.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Red cell lysing reagent. 864.8540 Section 864.8540...) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8540 Red cell lysing reagent. (a) Identification. A red cell lysing reagent is a device used to lyse (destroy) red blood cells for...

  8. 21 CFR 866.3110 - Campylobacter fetus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Campylobacter fetus serological reagents. 866.3110... (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents § 866.3110 Campylobacter fetus serological reagents. (a) Identification. Campylobacter fetus serological reagents are devices...

  9. U.S. VETERINARY IMMUNE REAGENTS NETWORK: PROGRESS WITH POULTRY IMMUNE REAGENTS

    USDA-ARS?s Scientific Manuscript database

    A major obstacle to advances in veterinary immunology and disease control is the lack of sufficient immunological reagents specific for ruminants, swine, poultry, equine and aquaculture species. Sets of reagents, i.e., monoclonal (mAb) and polyclonal antibodies, that can identify the major leukocyt...

  10. Modern affinity reagents: Recombinant antibodies and aptamers.

    PubMed

    Groff, Katherine; Brown, Jeffrey; Clippinger, Amy J

    2015-12-01

    Affinity reagents are essential tools in both basic and applied research; however, there is a growing concern about the reproducibility of animal-derived monoclonal antibodies. The need for higher quality affinity reagents has prompted the development of methods that provide scientific, economic, and time-saving advantages and do not require the use of animals. This review describes two types of affinity reagents, recombinant antibodies and aptamers, which are non-animal technologies that can replace the use of animal-derived monoclonal antibodies. Recombinant antibodies are protein-based reagents, while aptamers are nucleic-acid-based. In light of the scientific advantages of these technologies, this review also discusses ways to gain momentum in the use of modern affinity reagents, including an update to the 1999 National Academy of Sciences monoclonal antibody production report and federal incentives for recombinant antibody and aptamer efforts. In the long-term, these efforts have the potential to improve the overall quality and decrease the cost of scientific research. Copyright © 2015 Elsevier Inc. All rights reserved.

  11. On the Efect of the Oxidative Reagents on the Conductivity of Polyaniline/MMT Nanocomposites

    NASA Astrophysics Data System (ADS)

    Garcia-Bernabé, A.; Gil-Agustí, M.; Ortega, G.; Llovera, P.; Almarza, A.; Vázquez, S.; Amantia, D.; Aubouy, L.

    2010-06-01

    The synthesis of polyaniline has been reported using three different oxidative reagents: ammonium persulfate, potassium iodate and potassium iodate+sodium hypochlorite. This polyaniline has been used to prepare several nanocomposites with different percentage of Montmorillonite. The DC conductivity of the nanocomposites was determined by impedance spectroscopy. The oxidative reagent that gives higher conductivity is ammonium persulfate. The temperature dependence of the conductivity was studied.

  12. Kinetics of combined heterogeneous catalytic reactions with a common reagent

    SciTech Connect

    Pyatnitskii, Yu.I.

    1995-01-01

    The kinetics of combined catalytic reactions with a common reagent (competitive reactions) is analyzed assuming that no changes in the reaction mechanisms occur under their conjugation. A simplified approach is advanced for determining the relative rates of competitive reactions characterized by a similar mechanism of the initial stage for the interaction between the competitive reactants and catalyst. This includes the complex reactions, in which one of the reaction product serves as a competitive agent. The effects of nontrivial mutual influence of the competitive catalytic reactions are discussed. One type of this mutual influence manifests itself as a drastic inhibition of one reaction by another; this is not due to the catalyst surface blocking. This effect is inherent to the reactions involving the reversible dissociation of a heteroatomic reagent. The other type of the mutual influence is revealed in the promotion of one reaction by another when at least one of the reaction follows the Langmuir-Hinshelwood mechanism and the adsorption of a common reagent is far from the equilibrium.

  13. New reagents, new reactions: Computers in chemistry

    SciTech Connect

    Dessy, R.E.

    1996-12-31

    There is a new reagent in chemical reaction vessels-the computer. From data collection, through information processing, to knowledge creation the computer is an integral partner of today`s chemist. Despite its ability to be a Sorcerer`s Apprentice, it has become a leading weapon in overcoming some of the fiscal and technical demands placed upon research and development teams by global competition. In the process it is forcing changes in our work habits that arc, stressing both the Corporation and the individual, this article explores the uses, abuses, and possible future of the new reagent, and explores the meta-physics of the electronic web. 42 refs.

  14. Investigation of the possibility of using hydrogranulation in reprocessing radioactive wastes of radiochemical production facilities

    SciTech Connect

    Revyakin, V.; Borisov, L.M.

    1996-05-01

    Radio-chemical production facilities are constantly accumulating liquid radioactive wastes (still residues as the result of evaporation of extraction and adsorption solutions etc.) which are a complex multicomponent mixtures. The wastes are frequently stored for extended periods of time while awaiting disposition and in some cases, and this is much worse, they are released into the environment. In this report, I would like to draw your attention to some results we have obtained from investigations aimed at simplifying handing of such wastes by the precipitation of hard to dissolve metal hydroxides, the flocculation of the above into granules with the help of surface-active agents (in this case a polyacrylamide - PAA), quickly precipitated and easily filtered. The precipitate may be quickly dried and calcinated, if necessary, and transformed into a dense oxide sinter. In other words it may be transformed into a material convenient for storage or burial.

  15. Radiochemical Separation of Group 5 Elements. Model Experiments for Investigation of Dubnium Chemical Behaviour

    SciTech Connect

    Tereshatov, E. E.; Bozhikov, G. A.; Aksenov, N. V.; Starodub, G. Ya.; Vostokin, G. K.; Shishkin, S. V.; Dmitriev, S. N.; Bruchertseifer, H.; Gaeggeler, H. W.

    2007-05-22

    Chemical behaviour of group 5 elements in the aqueous hydrofluoric acid solutions was studied. The radiochemical method for the cation exchange separation of Nb (Pa) and Ta from Zr, Hf and lanthanides is presented. The developed scheme allows excluding of the presence of SF heavy actinides in fractions of separated elements. On the basis of the data of the present work, it is possible to suggest the following order of the stability of the fluoride complexes of group 4 and 5 elements: Nb {approx_equal} Pa > Zr > Hf > Ta. The order of the complex formation is in agreement with theoretical predictions. This analytical procedure can be used in future heavy nuclei synthesis experiments for the separation of dubnium (Db) from other reactions products and for its chemical identification.

  16. Radiochemical analyses of surface water from U.S. Geological Survey hydrologic bench-mark stations

    USGS Publications Warehouse

    Janzer, V.J.; Saindon, L.G.

    1972-01-01

    The U.S. Geological Survey's program for collecting and analyzing surface-water samples for radiochemical constituents at hydrologic bench-mark stations is described. Analytical methods used during the study are described briefly and data obtained from 55 of the network stations in the United States during the period from 1967 to 1971 are given in tabular form.Concentration values are reported for dissolved uranium, radium, gross alpha and gross beta radioactivity. Values are also given for suspended gross alpha radioactivity in terms of natural uranium. Suspended gross beta radioactivity is expressed both as the equilibrium mixture of strontium-90/yttrium-90 and as cesium-137.Other physical parameters reported which describe the samples include the concentrations of dissolved and suspended solids, the water temperature and stream discharge at the time of the sample collection.

  17. Registration of 71Ge rare decays in radiochemical gallium experiments SAGE and BEST

    NASA Astrophysics Data System (ADS)

    Shikhin, A. A.; Gavrin, V. N.; Gorbachev, V. V.; Ibragimova, T. V.; Kalikhov, A. V.; Yants, V. E.

    2017-01-01

    Registration systems of rare events from 71Ge decay in radiochemical gallium experiments SAGE and BEST are presented, where miniature proportional counters are used as detectors. The registration of the events is provided by eight counting channels simultaneously in the energy range of 0.4–15 keV which includes the 71Ge decays in the region of the L and K peaks with total efficiency up to 75%. Data analysis is based on full charge pulse shape recording using digital oscilloscope. Effective background discrimination is basically obtained due to low noise (<0.32 keV) and wide bandwidth (>100 MHz) of the system electronics. The design and main parameters of base components of the registration systems, description of electronics and comparison of their electrical and counting characteristics are given.

  18. Radiochemical method for evaluating the effect of antibiotics on Escherichia coli biofilms

    SciTech Connect

    Dix, B.A.; Cohen, P.S.; Laux, D.C.; Cleeland, R.

    1988-05-01

    A simple radiochemical method for evaluating the action of antibiotics on Escherichia coli cells in biofilms is reported. After growth, biofilms of E. coli ATCC 25922 on disks of urinary catheter material were suspended in fresh medium containing or lacking an antibiotic, incubated for 4 h at 37 degrees C, and pulse-labeled with (/sup 3/H)leucine for 5 min. Radioactivity in trichloracetic acid-precipitable material in the biofilm and in the surrounding medium (planktonic E. coli) was then measured. Antibiotic-induced inhibition of incorporation of (/sup 3/H)leucine into the cells in the biofilm was far less pronounced than incorporation into planktonic cells and, furthermore, correlated well with loss in viable counts. The method is simple, inexpensive, and extremely timesaving.

  19. On the degelation of networks – Case of the radiochemical degradation of methyl methacrylate – ethylene glycol dimethacrylate copolymers

    SciTech Connect

    Richaud, Emmanuel; Gilormini, Pierre; Verdu, Jacques

    2016-05-18

    Methyl methacrylate networks were synthetized and submitted to radiochemical degradation. Ageing was monitored by means of sol-gel analysis and glass transition temperature measurements. Networks were shown to undergo exclusively chain scission process leading to the degelation of network. The critical conversion degree corresponding to degelation (loss of all elastically active chains) is discussed regarding a statistical theory.

  20. On the degelation of networks - Case of the radiochemical degradation of methyl methacrylate - ethylene glycol dimethacrylate copolymers

    NASA Astrophysics Data System (ADS)

    Richaud, Emmanuel; Gilormini, Pierre; Verdu, Jacques

    2016-05-01

    Methyl methacrylate networks were synthetized and submitted to radiochemical degradation. Ageing was monitored by means of sol-gel analysis and glass transition temperature measurements. Networks were shown to undergo exclusively chain scission process leading to the degelation of network. The critical conversion degree corresponding to degelation (loss of all elastically active chains) is discussed regarding a statistical theory.

  1. Qualitative Gas Chromatography-Mass Spectrometry Analyses Using Amines as Chemical Ionization Reagent Gases

    NASA Astrophysics Data System (ADS)

    Little, James L.; Howard, Adam S.

    2013-12-01

    Ammonia is a very useful chemical ionization (CI) reagent gas for the qualitative analyses of compounds by positive ion gas chromatography-mass spectrometry (GCMS). The gas is readily available, inexpensive, and leaves no carbon contamination in the MS source. Compounds of interest to our laboratory typically yield abundant protonated or ammoniated species, which are indicative of a compound's molecular weight. Nevertheless, some labile compounds fragment extensively by substitution and elimination reactions and yield no molecular weight information. In these cases, a CI reagent gas mixture of methylamine in methane prepared dynamically was found to be very useful in obtaining molecular weight data. Likewise, deuterated ammonia and deuterated methylamine are useful CI reagent gases for determining the exchangeable protons in organic compounds. Deuterated methylamine CI reagent gas is conveniently prepared by dynamically mixing small amounts of methylamine with excess deuterated ammonia.

  2. Controlled release of reagents in capillary-driven microfluidics using reagent integrators.

    PubMed

    Hitzbleck, Martina; Gervais, Luc; Delamarche, Emmanuel

    2011-08-21

    The integration and release of reagents in microfluidics as used for point-of-care testing is essential for an easy and accurate operation of these promising diagnostic devices. Here, we present microfluidic functional structures, which we call reagent integrators (RIs), for integrating and releasing small amounts of dried reagents (ng quantities and less) into microlitres of sample in a capillary-driven microfluidic chip. Typically, a RI is less than 1 mm(2) in area and has an inlet splitting into a central reagent channel, in which reagents can be loaded using an inkjet spotter, and two diluter channels. During filling of the microfluidic chip, spotted reagents reconstitute and exit the RI with a dilution factor that relates to the relative hydraulic resistance of the channels forming the RI. We exemplify the working principle of RIs by (i) distributing ∼100 pg of horseradish peroxidase (HRP) in different volume fractions of a 1 μL solution containing a fluorogenic substrate for HRP and (ii) performing an immunoassay for C-reactive protein (CRP) using 450 pg of fluorescently labeled detection antibodies (dAbs) that reconstitute in ∼5 to 30% of a 1 μL sample of human serum. RIs preserve the conceptual simplicity of lateral flow assays while providing a great degree of control over the integration and release of reagents in a stream of sample. We believe RIs to be broadly applicable to microfluidic devices as used for biological assays.

  3. Reagent Selector: using Synthon Analysis to visualize reagent properties and assist in combinatorial library design.

    PubMed

    Mosley, Ralph T; Culberson, J Christopher; Kraker, Bryan; Feuston, Bradley P; Sheridan, Robert P; Conway, John F; Forbes, Joseph K; Chakravorty, Subhas J; Kearsley, Simon K

    2005-01-01

    Reagent Selector is an intranet-based tool that aids in the selection of reagents for use in combinatorial library construction. The user selects an appropriate reagent group as a query, for example, primary amines, and further refines it on the basis of various physicochemical properties, resulting in a list of potential reagents. The results of this selection process are, in turn, converted into synthons: the fragments or R-groups that are to be incorporated into the combinatorial library. The Synthon Analysis interface graphically depicts the chemical properties for each synthon as a function of the topological bond distance from the scaffold attachment point. Displayed in this fashion, the user is able to visualize the property space for the universe of synthons as well as that of the synthons selected. Ultimately, the reagent list that embodies the selected synthons is made available to the user for reagent procurement. Application of the approach to a sample reagent list for a G-protein coupled receptor targeted library is described.

  4. [The evaluation of different agglutination and adhesion tests with erythrocytic reagents in determining antibodies to the O and H antigens of Salmonella typhimurium in comparison with immunoenzyme analysis (IEA)].

    PubMed

    Karal'nik, B V; Denisova, T G

    1996-01-01

    The comparison of the effectiveness of EIA with that of a number of agglutination and adhesion tests with erythrocyte diagnostica in the determination of antibodies to different S.typhimurium antigens demonstrated higher sensitivity of EIA. The relative specificity of the determination of O- and H-antibodies in EIA and in agglutination and adhesion tests depended on the isotype of antibodies to be determined and the specificity of sensitins used in the production of immunoreagents.

  5. Synthesis and properties of sulfhydryl-group-specific reagents containing 125I.

    PubMed

    Krueger, R J; Lin, C; Frank, J A

    1991-10-01

    125I-containing compounds that react specifically with sulfhydryl groups were prepared in yields of 30 to 40% on the basis of starting 125I quantity. The synthetic precursors were commercially available heterobifunctional crosslinkers and the peptide L-arginyl-L-tyrosine. Two types of sulfhydryl specific reagents were prepared: 3-(2-pyridyldithio)propionylarginyl-[125I]-monoiodotyrosine, which permits reversible incorporation of 125I at sulfhydryl sites, and 3-maleimidopropionylarginyl- [125I]monoiodotyrosine, an irreversible labeling reagent. These products were isolated in a highly radiochemically pure form by C18 HPLC. The second-order rate constants for the reaction of 3-(2-pyridyldithio)propionylarginylmonoiodotyrosine and 3-maleimidopropionylarginylmonoiodotyrosine with N-acetylcysteine were 28 +/- 3 M-1 s-1 and 154 +/- 4 M-1 s-1, respectively, at pH 7.3. Storage of carrier-free 3-(2-pyridyldithio)propionylarginyl-[125I]monoiodotyrosine and 3-maleimidopropionylarginyl-[125I]monoiodotyrosine at -80 degrees C at a radioactive concentration of 0.4 mCi/ml resulted in conversion of 125I to species that did not react covalently with sulfhydryl groups. This process occurred with first-order kinetics and a t1/2 of 5.7 days for the pyridyldithio compound and 7.5 days for the maleimido compound. No conversion was observed during storage at -80 degrees C at radioactive concentrations of 0.02 mCi/ml or less. The labeling properties of these compounds were examined using red blood cell proteins as a test system. 3-(2-Pyridyldithio)propionylarginyl- [125I]monoiodotyrosine and maleimidopropionylarginyl-[125I]monoiodotyrosine reacted preferentially with membrane - associated sulfhydryl groups when incubated with intact red blood cells.

  6. Tetramethyleneethane Equivalents: Recursive Reagents for Serialized Cycloadditions.

    PubMed

    Wender, Paul A; Jeffreys, Matthew S; Raub, Andrew G

    2015-07-22

    New reactions and reagents that allow for multiple bond-forming events per synthetic operation are required to achieve structural complexity and thus value with step-, time-, cost-, and waste-economy. Here we report a new class of reagents that function like tetramethyleneethane (TME), allowing for back-to-back [4 + 2] cycloadditions, thereby amplifying the complexity-increasing benefits of Diels-Alder and metal-catalyzed cycloadditions. The parent recursive reagent, 2,3-dimethylene-4-trimethylsilylbutan-1-ol (DMTB), is readily available from the metathesis of ethylene and THP-protected 4-trimethylsilylbutyn-1-ol. DMTB and related reagents engage diverse dienophiles in an initial Diels-Alder or metal-catalyzed [4 + 2] cycloaddition, triggering a subsequent vinylogous Peterson elimination that recursively generates a new diene for a second cycloaddition. Overall, this multicomponent catalytic cascade produces in one operation carbo- and heterobicyclic building blocks for the synthesis of a variety of natural products, therapeutic leads, imaging agents, and materials. Its application to the three step synthesis of a new solvatochromic fluorophore, N-ethyl(6-N,N-dimethylaminoanthracene-2,3-dicarboximide) (6-DMA), and the photophysical characterization of this fluorophore are described.

  7. Tetramethyleneethane Equivalents: Recursive Reagents for Serialized Cycloadditions

    PubMed Central

    2015-01-01

    New reactions and reagents that allow for multiple bond-forming events per synthetic operation are required to achieve structural complexity and thus value with step-, time-, cost-, and waste-economy. Here we report a new class of reagents that function like tetramethyleneethane (TME), allowing for back-to-back [4 + 2] cycloadditions, thereby amplifying the complexity-increasing benefits of Diels–Alder and metal-catalyzed cycloadditions. The parent recursive reagent, 2,3-dimethylene-4-trimethylsilylbutan-1-ol (DMTB), is readily available from the metathesis of ethylene and THP-protected 4-trimethylsilylbutyn-1-ol. DMTB and related reagents engage diverse dienophiles in an initial Diels–Alder or metal-catalyzed [4 + 2] cycloaddition, triggering a subsequent vinylogous Peterson elimination that recursively generates a new diene for a second cycloaddition. Overall, this multicomponent catalytic cascade produces in one operation carbo- and heterobicyclic building blocks for the synthesis of a variety of natural products, therapeutic leads, imaging agents, and materials. Its application to the three step synthesis of a new solvatochromic fluorophore, N-ethyl(6-N,N-dimethylaminoanthracene-2,3-dicarboximide) (6-DMA), and the photophysical characterization of this fluorophore are described. PMID:25961416

  8. DEGRADATION OF MTBE INTERMEDIATES USING FENTON'S REAGENT

    EPA Science Inventory

    In a previous study, the chemical oxidation of MTBE at low concentrations in water using the Fenton's reagent (FR) was investigated. At certain reaction conditions the process achieved 99.99% degradation of MTBE but it did not result in complete MTBE mineralization. In the pres...

  9. Remarks on preparation of indandione detection reagents

    NASA Technical Reports Server (NTRS)

    Stepan, J.; Kral, V.

    1985-01-01

    A modified Claisen condensation with sliced sodium at a higher temperature was recommended for the production of ungranulated charcoal. A new ninhydrin production method by oxidation of benzaldiketohydrinden using available reagents was tried and was unsuccessful. Triketohydrinden was obtained by boiling ninhydrin in acetic acid anhydrides.

  10. Chemistry Students' Erroneous Conceptions of Limiting Reagent.

    ERIC Educational Resources Information Center

    Mammen, K. J.

    1996-01-01

    Describes a study of 32 University of Transkei (South Africa) freshmen's conceptualization of "limiting reagent," a basic concept in chemistry, based on student responses to two written test questions and clinical interviews. Results indicated that a high percentage of students had misconceptions and could not apply the concept…

  11. Tritioacetylating reagents and processes for preparation thereof

    DOEpatents

    Saljoughian, Manoucher; Morimoto, Hiromi; Williams, Philip G.; Than, Chit

    2000-01-01

    Novel acetylating and tritioacetylating reagents suitable for preparation of nonlabelled and radiolabelled organic compounds. N-acetoxynaphthalimide, N-tritioacetoxyphthalimide, N-tritioacetoxysuccinimide, N-tritioacetoxynaphthalimide and processes of their preparation. The invention also concerns synthesis of nonlabelled acetylated and tritioacetylated organic compounds from precursors containing a free --NH.sub.2, --SH or --OH group.

  12. [Discussion about Management of In Vitro Diagnostic Reagent].

    PubMed

    Huang, Liang; Zhu, Jianghua; Gu, Haiyi; Geng, Yimin

    2015-03-01

    In order to adapt the rapid development of modern medicine, this paper is aimed to analyze the application of in vitro diagnostic reagents (IVD Reagents) in hospital management and improve the overall level of hospital management. By groping the management experience of IVD reagents, we discuss the internal hospital management mode of IVD reagents in reality. With the continuous improvements on the information platform of IVD reagents,we can realize benefit analysis of IVD reagents within the process of management. Reasonable management on IVD reagentscan improve the working efficiency in hospitals and provide swifter and better medical service for patients.

  13. X-Ray Crystallography Reagent

    NASA Technical Reports Server (NTRS)

    Morrison, Dennis R. (Inventor); Mosier, Benjamin (Inventor)

    2003-01-01

    Microcapsules prepared by encapsulating an aqueous solution of a protein, drug or other bioactive substance inside a semi-permeable membrane by are disclosed. The microcapsules are formed by interfacial coacervation under conditions where the shear forces are limited to 0-100 dynes per square centimeter at the interface. By placing the microcapsules in a high osmotic dewatering solution. the protein solution is gradually made saturated and then supersaturated. and the controlled nucleation and crystallization of the protein is achieved. The crystal-filled microcapsules prepared by this method can be conveniently harvested and stored while keeping the encapsulated crystals in essentially pristine condition due to the rugged. protective membrane. Because the membrane components themselves are x-ray transparent, large crystal-containing microcapsules can be individually selected, mounted in x-ray capillary tubes and subjected to high energy x-ray diffraction studies to determine the 3-D smucture of the protein molecules. Certain embodiments of the microcapsules of the invention have composite polymeric outer membranes which are somewhat elastic, water insoluble, permeable only to water, salts, and low molecular weight molecules and are structurally stable in fluid shear forces typically encountered in the human vascular system.

  14. Anion-exchange nanospheres as titration reagents for anionic analytes.

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-08-18

    We present here anion-exchange nanospheres as novel titration reagents for anions. The nanospheres contain a lipophilic cation for which the counterion is initially Cl(-). Ion exchange takes place between Cl(-) in the nanospheres and a more lipophilic anion in the sample, such as ClO4(-) and NO3(-). Consecutive titration in the same sample solution for ClO4(-) and NO3(-) were demonstrated. As an application, the concentration of NO3(-) in spinach was successfully determined using this method.

  15. Comparative Performance of Reagents and Platforms for Quantitation of Cytomegalovirus DNA by Digital PCR.

    PubMed

    Hayden, R T; Gu, Z; Sam, S S; Sun, Y; Tang, L; Pounds, S; Caliendo, A M

    2016-10-01

    A potential benefit of digital PCR is a reduction in result variability across assays and platforms. Three sets of PCR reagents were tested on two digital PCR systems (Bio-Rad and RainDance), using three different sets of PCR reagents for quantitation of cytomegalovirus (CMV). Both commercial quantitative viral standards and 16 patient samples (n = 16) were tested. Quantitative accuracy (compared to nominal values) and variability were determined based on viral standard testing results. Quantitative correlation and variability were assessed with pairwise comparisons across all reagent-platform combinations for clinical plasma sample results. The three reagent sets, when used to assay quantitative standards on the Bio-Rad system, all showed a high degree of accuracy, low variability, and close agreement with one another. When used on the RainDance system, one of the three reagent sets appeared to have a much better correlation to nominal values than did the other two. Quantitative results for patient samples showed good correlation in most pairwise comparisons, with some showing poorer correlations when testing samples with low viral loads. Digital PCR is a robust method for measuring CMV viral load. Some degree of result variation may be seen, depending on platform and reagents used; this variation appears to be greater in samples with low viral load values. Copyright © 2016, American Society for Microbiology. All Rights Reserved.

  16. An attempt to standardize APTT reagents used to monitor heparin therapy.

    PubMed

    Ray, M; Carroll, P; Smith, I; Hawson, G

    1992-12-01

    Citrated samples from 100 patients on i.v. heparin and 20 normal patients were tested with three batches each of three activated partial thromboplastin time (APTT) reagents: Thrombosil I (Ortho); Automated APTT (Organon Teknika) and Actin FSL (Baxter). The ratio of APTT over the geometric mean normal APTT for each heparinized sample was calculated. One batch of reagent arbitrarily chosen as a reference gave the ratios APTRREF (y). The remaining reagents to be standardized against the reference system gave the ratios APTRTEST (x). The best correlation between systems was given by log vs log x. Standard curves were prepared from the APTT ratios of the 20 normal patients and 65 of the heparinized samples. On plotting log APTRTEST vs log APTRREF the y intercept was close to zero so x was expressed in terms of y using; log x = HSI. log y, where HSI (Heparin Sensitivity Index) = slope. The APTRTEST results of the remaining 35 heparinized samples were transformed using; APTRTRANS = (APTRTEST)HSI.APTRTRANS was then compared to APTRREF to determine whether the transformation brought the results closer to the reference. We conclude that although some improvement was found by using the transform, it was not possible to mathematically relate APTT results due to a high degree of variation between results using different reagents. A standard APTT reagent for the monitoring of heparin therapy is recommended. A separate APTT reagent may be required for the screening of factor deficiencies and lupus anticoagulants.

  17. The Yariv reagent: behaviour in different solvents and interaction with a gum arabic arabinogalactan-protein.

    PubMed

    Paulsen, B S; Craik, D J; Dunstan, D E; Stone, B A; Bacic, A

    2014-06-15

    The β-D-Glc Yariv reagent is frequently used to isolate and to study the structure of arabinogalactan-proteins with the arabinogalactan type II structure. The present paper describes the aggregation features of the Yariv reagent in water, salt solutions and in organic solvents as determined by NMR, absorption spectroscopy and light scattering experiments. The results indicate that in water the Yariv reagent forms aggregates of up to 300 units and in 1% aqueous NaCl the degree of aggregation is approx. 150. The aggregates are formed both by H-bonds and hydrophobic interactions, the former appearing to be of most importance in water. The interaction between the Yariv reagent and an AGP fraction from gum arabic, showed a degree of aggregation of the Yariv reagent when using 1% NaCl to be of approx. 150 units, whereas disruption of the aggregate took place in 10% NaCl with an aggregation number of approx. 100. Partial acid hydrolysis of an AGP from gum Arabic (Acacia Senegal) and analyses of the linkage types remaining indicated that a certain length of (1→3)-β-linked galactose units was necessary for binding between the Yariv reagent and the AGP. This is in accordance to what also was recently observed by Kitazawa et al. (2013). Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Enhancing reactive species generation upon photo-activation of CdTe quantum dots for the chemiluminometric determination of unreacted reagent in UV/S2O8(2-) drug degradation process.

    PubMed

    Santana, Rodolfo M M; Oliveira, Thaís D; Rodrigues, S Sofia M; Frigerio, Christian; Santos, João L M; Korn, Mauro

    2015-04-01

    A new chemiluminescence (CL) flow method for persulfate determination was developed based on luminol oxidation by in-line generated radicals. Reactive oxygen species (ROS) generated by CdTe quantum dots (QDs) under a low energetic radiation (visible light emitted by LEDs) promoted the decomposition of persulfate ion (S2O8(2-)) into sulfate radical (SO4(∙-)), leading to subsequent radical chain reactions that yield the emission of light. Due to the inherent radical short lifetimes and the transient behavior of CL phenomena an automated multi-pumping flow system (MPFS) was proposed to improve sample manipulation and reaction zone implementation ensuring reproducible analysis time and high sampling rate. The developed approach allowed up to 60 determinations per hour and determine S2O8(2-) concentrations between 0.1 and 1 mmol with good linearity (R=0.9999). The method has shown good repeatability with relative standard deviations below 2.5% (n=3) for different persulfate concentrations (0.1 and 0.625 mmol L(-1)). Limits of detection (3σ) and quantification (10σ) were 2.7 and 9.1 µmol L(-1), respectively. The MPFS system was applied to persulfate determination in bench scale UV/S2O8(2-) drug degradation processes of model samples showing good versatility and providing real time information on the persulfate consumption in photo-chemical degradation methodologies.

  19. Kinetic method for determination of ascorbic acid on flow injection system by using its catalytic effect on the complexation reaction of an ultra sensitive colorimetric reagent of porphyrin with Cu(II)

    NASA Astrophysics Data System (ADS)

    Liu, Jianhua; Itoh, Jun-Ichi

    2007-06-01

    A kinetic method performed on a flow injection system is described for the determination of ascorbic acid by using its catalytic effect on the complexation reaction of Cu(II) with 5,10,15,20-tetrakis(4- N-trimethyl-aminophenyl)porphyrin. The characteristic spectrum of porphyrin (Soret band), which shows intense absorption around 400 nm ( ɛ > 2.0 × 10 5 cm -1 M -1), was used first time for determining ascorbic acid. By incorporating the complexation reaction into a flow injection system, ascorbic acid could be determined either over a broad dynamic range of 0.1-1000 μg/ml or at a trace level below 5 ng/ml. Good repeatability was also achieved by testing a working standard of 0.1 μg/ml with 10 injections at a throughput of 35 h -1, obtaining a relative standard deviation of 0.11%. Substances like amino acids, vitamins, sugars, organic acids and metal ions, showed no or little interference even present at high concentrations. The method was validated in the determination of ascorbic acid contents of some commercially available soft drinks by comparison with the official 2,6-dichloroindophenol method with reasonable agreement.

  20. The Grignard Reagent: Preparation, Structure, and Some Reactions.

    ERIC Educational Resources Information Center

    Orchin, Milton

    1989-01-01

    The Grignard reagent used in the laboratory synthesis of organic compounds is the product resulting from the reaction of an alkyl or aryl halide with elemental magnesium. Describes the structure, formation, and some reactions of the reagent. (YP)

  1. 21 CFR 866.3250 - Erysipelothrix rhusiopathiae serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Erysipelothrix rhusiopathiae serological reagents... Erysipelothrix rhusiopathiae serological reagents. (a) Identification. Erysipelothrix rhusiopathiae serological... Erysipelothrix rhusiopathiae from cultured isolates derived from clinical specimens. The identification aids...

  2. The Grignard Reagent: Preparation, Structure, and Some Reactions.

    ERIC Educational Resources Information Center

    Orchin, Milton

    1989-01-01

    The Grignard reagent used in the laboratory synthesis of organic compounds is the product resulting from the reaction of an alkyl or aryl halide with elemental magnesium. Describes the structure, formation, and some reactions of the reagent. (YP)

  3. CLAY AND CLAY-SUPPORTED REAGENTS IN ORGANIC SYNTHESES

    EPA Science Inventory

    CLAY AND CLAY-SUPPORTED REAGENTS HAVE BEEN USED EXTENSIVELY FOR SYNTHETIC ORGANIC TRANSFORMATIONS. THIS OVERVIEW DESCRIBES THE SALIENT STRUCTURAL PROPERTIES OF VARIOUS CLAY MATERIALS AND EXTENDS THE DISCUSSION TO PILLARED CLAYS AND REAGENTS SUPPORTED ON CLAY MATERIALS. A VARIET...

  4. Polymeric microspheres as protein transduction reagents.

    PubMed

    Nagel, David; Behrendt, Jonathan M; Chimonides, Gwen F; Torr, Elizabeth E; Devitt, Andrew; Sutherland, Andrew J; Hine, Anna V

    2014-06-01

    Discovering the function of an unknown protein, particularly one with neither structural nor functional correlates, is a daunting task. Interaction analyses determine binding partners, whereas DNA transfection, either transient or stable, leads to intracellular expression, though not necessarily at physiologically relevant levels. In theory, direct intracellular protein delivery (protein transduction) provides a conceptually simpler alternative, but in practice the approach is problematic. Domains such as HIV TAT protein are valuable, but their effectiveness is protein specific. Similarly, the delivery of intact proteins via endocytic pathways (e.g. using liposomes) is problematic for functional analysis because of the potential for protein degradation in the endosomes/lysosomes. Consequently, recent reports that microspheres can deliver bio-cargoes into cells via a non-endocytic, energy-independent pathway offer an exciting and promising alternative for in vitro delivery of functional protein. In order for such promise to be fully exploited, microspheres are required that (i) are stably linked to proteins, (ii) can deliver those proteins with good efficiency, (iii) release functional protein once inside the cells, and (iv) permit concomitant tracking. Herein, we report the application of microspheres to successfully address all of these criteria simultaneously, for the first time. After cellular uptake, protein release was autocatalyzed by the reducing cytoplasmic environment. Outside of cells, the covalent microsphere-protein linkage was stable for ≥90 h at 37 °C. Using conservative methods of estimation, 74.3% ± 5.6% of cells were shown to take up these microspheres after 24 h of incubation, with the whole process of delivery and intracellular protein release occurring within 36 h. Intended for in vitro functional protein research, this approach will enable study of the consequences of protein delivery at physiologically relevant levels, without recourse to

  5. SPECTROSCOPIC ONLINE MONITORING FOR PROCESS CONTROL AND SAFEGUARDING OF RADIOCHEMICAL STREAMS

    SciTech Connect

    Bryan, Samuel A.; Levitskaia, Tatiana G.

    2013-09-29

    There is a renewed interest worldwide to promote the use of nuclear power and close the nuclear fuel cycle. The long term successful use of nuclear power is critically dependent upon adequate and safe processing and disposition of the used nuclear fuel. Liquid-liquid extraction is a separation technique commonly employed for the processing of the dissolved used nuclear fuel. The instrumentation used to monitor these processes must be robust, require little or no maintenance, and be able to withstand harsh environments such as high radiation fields and aggressive chemical matrices. This paper summarizes application of the absorption and vibrational spectroscopic techniques supplemented by physicochemical measurements for radiochemical process monitoring. In this context, our team experimentally assessed the potential of Raman and spectrophotometric techniques for online real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. These techniques demonstrate robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. Satisfactory prediction of the analytes concentrations in these preliminary experiments warrants further development of the spectroscopy-based methods for radiochemical process control and safeguarding. Additionally, the ability to identify material intentionally diverted from a liquid-liquid extraction contactor system was successfully tested using on-line process monitoring as a means to detect the amount of material diverted. A chemical diversion and detection from a liquid-liquid extraction scheme was demonstrated using a centrifugal contactor system

  6. Thionation with the reagent combination of phosphorus pentasulfide and hexamethyldisiloxane.

    PubMed

    Curphey, Thomas J

    2002-09-06

    The combination of P4S10 and hexamethyldisiloxane efficiently converts esters, lactones, amides, lactams, and ketones to their corresponding thiono derivatives. In the presence of elemental sulfur, 3-oxoesters are converted to dithiolethiones by this reagent. Yields are comparable to or superior to those obtained with Lawesson's reagent. The method has the advantage that reagent-derived byproducts may be removed by a simple hydrolytic workup or by filtration through silica gel, rather than by chromatography, as required for Lawesson's reagent.

  7. Colorimetric Determination of the Iron(III)-Thiocyanate Reaction Equilibrium Constant with Calibration and Equilibrium Solutions Prepared in a Cuvette by Sequential Additions of One Reagent to the Other

    ERIC Educational Resources Information Center

    Nyasulu, Frazier; Barlag, Rebecca

    2011-01-01

    The well-known colorimetric determination of the equilibrium constant of the iron(III-thiocyanate complex is simplified by preparing solutions in a cuvette. For the calibration plot, 0.10 mL increments of 0.00100 M KSCN are added to 4.00 mL of 0.200 M Fe(NO[subscript 3])[subscript 3], and for the equilibrium solutions, 0.50 mL increments of…

  8. Colorimetric Determination of the Iron(III)-Thiocyanate Reaction Equilibrium Constant with Calibration and Equilibrium Solutions Prepared in a Cuvette by Sequential Additions of One Reagent to the Other

    ERIC Educational Resources Information Center

    Nyasulu, Frazier; Barlag, Rebecca

    2011-01-01

    The well-known colorimetric determination of the equilibrium constant of the iron(III-thiocyanate complex is simplified by preparing solutions in a cuvette. For the calibration plot, 0.10 mL increments of 0.00100 M KSCN are added to 4.00 mL of 0.200 M Fe(NO[subscript 3])[subscript 3], and for the equilibrium solutions, 0.50 mL increments of…

  9. Study of the sensitization of tetradecyl benzyl dimethyl ammonium chloride for spectrophotometric determination of dopamine hydrochloride using sodium 1,2-naphthoquinone-4-sulfonate as the chemical derivative chromogenic reagent.

    PubMed

    Li, Quanmin; Li, Juan; Yang, Zhanjun

    2007-01-30

    A new method has been established for the determination of dopamine hydrochloride (DPH) using sodium 1,2-naphthoquinone-4-sulfonate (NQS) and tetradecyl benzyl dimethyl ammonium chloride (Zeph). This method is based on the formation of a pink compound from the reaction of DPH, sodium 1,2-naphthoquinone-4-sulfonate and Zeph. The condensation reaction proceeds quantitatively in pH 9.40 buffer solution. The maximum absorption wavelength and the value of epsilon491 were 491 nm, and 7.51x10(3) l mol(-1) cm(-1), respectively, when the stoichiometric ratio of the reaction was 1:1:1. Beer's law was obeyed in the range of 0.16-40 mg l(-1) of DPH. The data have been filled to a linear regression equation A=0.5781+0.0254 C (mg l(-1)), with a correlation coefficient of 0.9993. The detection limit is 0.12 mg l(-1), R.S.D. is 0.64% (40 mg l(-1), n=11), and average recovery is over 99.7%. This paper further improves the determination of DPH compared to the previous methods. The kinetic property and reaction mechanism have also been discussed. This proposed method has been successfully applied to the determination of DPH in injection and biological samples with satisfactory results.

  10. Hydrazones as Singular Reagents in Asymmetric Organocatalysis.

    PubMed

    de Gracia Retamosa, María; Matador, Esteban; Monge, David; Lassaletta, José M; Fernández, Rosario

    2016-09-12

    This Minireview summarizes strategies and developments regarding the use of hydrazones as reagents in asymmetric organocatalysis, their distinct roles in nucleophile-electrophile, cycloaddition, and cyclization reactions. The key structural elements governing the reactivity of these reagents in a preferred pathway will be discussed, as well as their different interactions with organocatalysts, leading to diverse activation modes. Along these studies, the synthetic equivalence of N-monoalkyl, N,N-dialkyl, and N-acyl hydrazones with several synthons is also highlighted. Emphasis is also put on the mechanistic studies performed to understand the observed reactivities. Finally, the functional group transformations performed from the available products has also been analyzed, highlighting the synthetic value of these methodologies, which served to access numerous families of valuable multifunctional compounds and nitrogen-containing heterocycles.

  11. Monoclonal antibodies as blood grouping reagents.

    PubMed

    Voak, D

    1990-04-01

    The large volume requirements for high quality ABO and Rh(D) typing reagents can now be supplied by selected monoclonal antibodies. Superior anti-A and anti-B monoclonal reagents can be prepared, from blends of at least two antibodies, to optimize the intensity of agglutination for slide tests and the potency for the detection of the weaker sub-groups, including Ax and Bw, by tube techniques. New quality control steps have been described for some highly sensitive anti-A/anti-B antibodies to avoid the detection of traces of A on B cells or traces of B on A1 cells, which results from the non-specific activity of A and B transferases. Excellent anti-A,B reagents may also be made by blends of at least two antibodies to optimize both A and B reactions, but the need for their continued use is now debatable. The development of high titre IgM monoclonal anti-D reagents offers simple rapid saline Rh(D) typing of both patients and donors, but they cannot reliably detect weak D (Du) and some D variants, e.g. the epitopes on D category VI cells. However, this can be achieved by blending an IgM anti-D with IgG (polyclonal) anti-D which can detect these types after conversion of negative saline tests to an antiglobulin phase. In addition, high grade Du, D categories and variants can be reliably detected (for typing donors) by selected monoclonal IgM and IgG anti-Ds by use of suitably enhanced tests without the use of an antiglobulin test.(ABSTRACT TRUNCATED AT 250 WORDS)

  12. 21 CFR 660.30 - Reagent Red Blood Cells.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 7 2010-04-01 2010-04-01 false Reagent Red Blood Cells. 660.30 Section 660.30...) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Reagent Red Blood Cells § 660.30 Reagent Red Blood Cells. (a) Proper name and definition. The proper name of the product shall...

  13. 21 CFR 864.4010 - General purpose reagent.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... diagnostic test procedure or system constituting a finished in vitro diagnostic (IVD) test. General purpose reagents are appropriate for combining with one or more than one ASR in producing such systems and include... powered systems. General purpose reagents include cytological preservatives, decalcifying reagents...

  14. 21 CFR 864.8100 - Bothrops atrox reagent.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Bothrops atrox reagent. 864.8100 Section 864.8100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8100 Bothrops atrox reagent. (a...

  15. 21 CFR 864.8100 - Bothrops atrox reagent.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Bothrops atrox reagent. 864.8100 Section 864.8100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8100 Bothrops atrox reagent. (a...

  16. 21 CFR 864.8100 - Bothrops atrox reagent.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Bothrops atrox reagent. 864.8100 Section 864.8100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8100 Bothrops atrox reagent. (a...

  17. 21 CFR 864.8100 - Bothrops atrox reagent.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Bothrops atrox reagent. 864.8100 Section 864.8100 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES HEMATOLOGY AND PATHOLOGY DEVICES Hematology Reagents § 864.8100 Bothrops atrox reagent. (a...

  18. 21 CFR 866.3400 - Parainfluenza virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... respiratory illnesses ranging from the common cold to pneumonia. (b) Classification. Class I (general controls... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Parainfluenza virus serological reagents. 866.3400... virus serological reagents. (a) Identification. Parainfluenza virus serological reagents are devices...

  19. 21 CFR 866.3400 - Parainfluenza virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... respiratory illnesses ranging from the common cold to pneumonia. (b) Classification. Class I (general controls... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Parainfluenza virus serological reagents. 866.3400... virus serological reagents. (a) Identification. Parainfluenza virus serological reagents are devices...

  20. 21 CFR 866.3400 - Parainfluenza virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... respiratory illnesses ranging from the common cold to pneumonia. (b) Classification. Class I (general controls... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Parainfluenza virus serological reagents. 866.3400... virus serological reagents. (a) Identification. Parainfluenza virus serological reagents are devices...

  1. 21 CFR 866.3400 - Parainfluenza virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... respiratory illnesses ranging from the common cold to pneumonia. (b) Classification. Class I (general controls... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Parainfluenza virus serological reagents. 866.3400... virus serological reagents. (a) Identification. Parainfluenza virus serological reagents are devices...

  2. 21 CFR 866.3400 - Parainfluenza virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... respiratory illnesses ranging from the common cold to pneumonia. (b) Classification. Class I (general controls... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Parainfluenza virus serological reagents. 866.3400... virus serological reagents. (a) Identification. Parainfluenza virus serological reagents are devices...

  3. 21 CFR 660.20 - Blood Grouping Reagent.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 7 2010-04-01 2010-04-01 false Blood Grouping Reagent. 660.20 Section 660.20 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.20 Blood Grouping Reagent. (a) Proper name and definition. The proper name of this product shall be Blood...

  4. 21 CFR 866.3330 - Influenza virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Influenza virus serological reagents. 866.3330 Section 866.3330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... virus serological reagents. (a) Identification. Influenza virus serological reagents are devices that...

  5. 21 CFR 866.3330 - Influenza virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Influenza virus serological reagents. 866.3330 Section 866.3330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... virus serological reagents. (a) Identification. Influenza virus serological reagents are devices that...

  6. 21 CFR 866.3330 - Influenza virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Influenza virus serological reagents. 866.3330 Section 866.3330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... virus serological reagents. (a) Identification. Influenza virus serological reagents are devices that...

  7. 21 CFR 866.3940 - West Nile virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false West Nile virus serological reagents. 866.3940... virus serological reagents. (a) Identification. West Nile virus serological reagents are devices that consist of antigens and antisera for the detection of anti-West Nile virus IgM antibodies, in human serum...

  8. 21 CFR 866.3940 - West Nile virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false West Nile virus serological reagents. 866.3940... virus serological reagents. (a) Identification. West Nile virus serological reagents are devices that consist of antigens and antisera for the detection of anti-West Nile virus IgM antibodies, in human serum...

  9. 21 CFR 866.3330 - Influenza virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Influenza virus serological reagents. 866.3330 Section 866.3330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... virus serological reagents. (a) Identification. Influenza virus serological reagents are devices that...

  10. 21 CFR 866.3940 - West Nile virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false West Nile virus serological reagents. 866.3940... virus serological reagents. (a) Identification. West Nile virus serological reagents are devices that consist of antigens and antisera for the detection of anti-West Nile virus IgM antibodies, in human serum...

  11. 21 CFR 866.3940 - West Nile virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false West Nile virus serological reagents. 866.3940... virus serological reagents. (a) Identification. West Nile virus serological reagents are devices that consist of antigens and antisera for the detection of anti-West Nile virus IgM antibodies, in human serum...

  12. 21 CFR 866.3330 - Influenza virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Influenza virus serological reagents. 866.3330 Section 866.3330 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... virus serological reagents. (a) Identification. Influenza virus serological reagents are devices that...

  13. 21 CFR 866.3085 - Brucella spp. serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Brucella spp. serological reagents. 866.3085 Section 866.3085 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... these reagents consist of antisera conjugated with a fluorescent dye (immunofluorescent reagents)...

  14. 21 CFR 866.3085 - Brucella spp. serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Brucella spp. serological reagents. 866.3085 Section 866.3085 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... these reagents consist of antisera conjugated with a fluorescent dye (immunofluorescent reagents)...

  15. 21 CFR 866.3085 - Brucella spp. serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Brucella spp. serological reagents. 866.3085 Section 866.3085 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES... these reagents consist of antisera conjugated with a fluorescent dye (immunofluorescent reagents)...

  16. 21 CFR 866.3930 - Vibrio cholerae serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Vibrio cholerae serological reagents. 866.3930... cholerae serological reagents. (a) Identification. Vibrio cholerae serological reagents are devices that are used in the agglutination (an antigen-antibody clumping reaction) test to identify Vibrio cholerae...

  17. 40 CFR 792.83 - Reagents and solutions.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 31 2010-07-01 2010-07-01 true Reagents and solutions. 792.83 Section... ACT (CONTINUED) GOOD LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 792.83 Reagents and solutions. All reagents and solutions in the laboratory areas shall be labeled to indicate identity,...

  18. 21 CFR 660.30 - Reagent Red Blood Cells.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 7 2012-04-01 2012-04-01 false Reagent Red Blood Cells. 660.30 Section 660.30...) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Reagent Red Blood Cells § 660.30 Reagent Red Blood Cells. (a) Proper name and definition. The proper name of the product shall...

  19. 21 CFR 660.30 - Reagent Red Blood Cells.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 7 2014-04-01 2014-04-01 false Reagent Red Blood Cells. 660.30 Section 660.30...) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Reagent Red Blood Cells § 660.30 Reagent Red Blood Cells. (a) Proper name and definition. The proper name of the product shall...

  20. 21 CFR 660.30 - Reagent Red Blood Cells.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 7 2013-04-01 2013-04-01 false Reagent Red Blood Cells. 660.30 Section 660.30...) BIOLOGICS ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Reagent Red Blood Cells § 660.30 Reagent Red Blood Cells. (a) Proper name and definition. The proper name of the product shall...

  1. 40 CFR 160.83 - Reagents and solutions.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 25 2013-07-01 2013-07-01 false Reagents and solutions. 160.83 Section... LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 160.83 Reagents and solutions. All reagents and solutions in the laboratory areas shall be labeled to indicate identity, titer or concentration,...

  2. 40 CFR 160.83 - Reagents and solutions.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 25 2012-07-01 2012-07-01 false Reagents and solutions. 160.83 Section... LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 160.83 Reagents and solutions. All reagents and solutions in the laboratory areas shall be labeled to indicate identity, titer or concentration,...

  3. 40 CFR 160.83 - Reagents and solutions.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 24 2011-07-01 2011-07-01 false Reagents and solutions. 160.83 Section... LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 160.83 Reagents and solutions. All reagents and solutions in the laboratory areas shall be labeled to indicate identity, titer or concentration,...

  4. 40 CFR 160.83 - Reagents and solutions.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 24 2014-07-01 2014-07-01 false Reagents and solutions. 160.83 Section... LABORATORY PRACTICE STANDARDS Testing Facilities Operation § 160.83 Reagents and solutions. All reagents and solutions in the laboratory areas shall be labeled to indicate identity, titer or concentration,...

  5. 21 CFR 660.20 - Blood Grouping Reagent.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 7 2012-04-01 2012-04-01 false Blood Grouping Reagent. 660.20 Section 660.20 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.20 Blood Grouping Reagent. (a) Proper name and definition. The proper name of this product shall be Blood Grouping...

  6. 21 CFR 660.20 - Blood Grouping Reagent.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 7 2013-04-01 2013-04-01 false Blood Grouping Reagent. 660.20 Section 660.20 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.20 Blood Grouping Reagent. (a) Proper name and definition. The proper name of this product shall be Blood Grouping...

  7. 21 CFR 660.20 - Blood Grouping Reagent.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 7 2014-04-01 2014-04-01 false Blood Grouping Reagent. 660.20 Section 660.20 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.20 Blood Grouping Reagent. (a) Proper name and definition. The proper name of this product shall be Blood Grouping...

  8. 21 CFR 660.20 - Blood Grouping Reagent.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 7 2011-04-01 2010-04-01 true Blood Grouping Reagent. 660.20 Section 660.20 Food... ADDITIONAL STANDARDS FOR DIAGNOSTIC SUBSTANCES FOR LABORATORY TESTS Blood Grouping Reagent § 660.20 Blood Grouping Reagent. (a) Proper name and definition. The proper name of this product shall be Blood Grouping...

  9. 21 CFR 866.3255 - Escherichia coli serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Escherichia coli serological reagents. 866.3255... coli serological reagents. (a) Identification. Escherichia coli serological reagents are devices that consist of antigens and antisera used in serological tests to identify Escherichia coli from cultured...

  10. Cross-Institute Evaluations of Inhibitor-Resistant PCR Reagents for Direct Testing of Aerosol and Blood Samples Containing Biological Warfare Agent DNA

    PubMed Central

    Minogue, Timothy D.; Rachwal, Phillip A.; Trombley Hall, Adrienne; Koehler, Jeffery W.

    2014-01-01

    Rapid pathogen detection is crucial for the timely introduction of therapeutics. Two groups (one in the United Kingdom and one in the United States) independently evaluated inhibitor-resistant PCR reagents for the direct testing of substrates. In the United Kingdom, a multiplexed Bacillus anthracis (target) and Bacillus subtilis (internal-control) PCR was used to evaluate 4 reagents against 5 PCR inhibitors and down-selected the TaqMan Fast Virus 1-Step master mix (Life Technologies Inc.). In the United States, four real-time PCR assays (targeting B. anthracis, Brucella melitensis, Venezuelan equine encephalitis virus [VEEV], and Orthopoxvirus spp.) were used to evaluate 5 reagents (plus the Fast Virus master mix) against buffer, blood, and soil samples and down-selected the KAPA Blood Direct master mix (KAPA Biosystems Inc.) with added Platinum Taq (Life Technologies). The down-selected reagents underwent further testing. In the United Kingdom experiments, both reagents were tested against seven contrived aerosol collector samples containing B. anthracis Ames DNA and B. subtilis spores from a commercial formulation (BioBall). In PCR assays with reaction mixtures containing 40% crude sample, an airfield-collected sample induced inhibition of the B. subtilis PCR with the KAPA reagent and complete failure of both PCRs with the Fast Virus reagent. However, both reagents allowed successful PCR for all other samples—which inhibited PCRs with a non-inhibitor-resistant reagent. In the United States, a cross-assay limit-of-detection (LoD) study in blood was conducted. The KAPA Blood Direct reagent allowed the detection of agent DNA (by four PCRs) at higher concentrations of blood in the reaction mixture (2.5%) than the Fast Virus reagent (0.5%), although LoDs differed between assays and reagent combinations. Across both groups, the KAPA Blood Direct reagent was determined to be the optimal reagent for inhibition relief in PCR. PMID:24334660

  11. Cross-institute evaluations of inhibitor-resistant PCR reagents for direct testing of aerosol and blood samples containing biological warfare agent DNA.

    PubMed

    Minogue, Timothy D; Rachwal, Phillip A; Trombley Hall, Adrienne; Koehler, Jeffery W; Weller, Simon A

    2014-02-01

    Rapid pathogen detection is crucial for the timely introduction of therapeutics. Two groups (one in the United Kingdom and one in the United States) independently evaluated inhibitor-resistant PCR reagents for the direct testing of substrates. In the United Kingdom, a multiplexed Bacillus anthracis (target) and Bacillus subtilis (internal-control) PCR was used to evaluate 4 reagents against 5 PCR inhibitors and down-selected the TaqMan Fast Virus 1-Step master mix (Life Technologies Inc.). In the United States, four real-time PCR assays (targeting B. anthracis, Brucella melitensis, Venezuelan equine encephalitis virus [VEEV], and Orthopoxvirus spp.) were used to evaluate 5 reagents (plus the Fast Virus master mix) against buffer, blood, and soil samples and down-selected the KAPA Blood Direct master mix (KAPA Biosystems Inc.) with added Platinum Taq (Life Technologies). The down-selected reagents underwent further testing. In the United Kingdom experiments, both reagents were tested against seven contrived aerosol collector samples containing B. anthracis Ames DNA and B. subtilis spores from a commercial formulation (BioBall). In PCR assays with reaction mixtures containing 40% crude sample, an airfield-collected sample induced inhibition of the B. subtilis PCR with the KAPA reagent and complete failure of both PCRs with the Fast Virus reagent. However, both reagents allowed successful PCR for all other samples-which inhibited PCRs with a non-inhibitor-resistant reagent. In the United States, a cross-assay limit-of-detection (LoD) study in blood was conducted. The KAPA Blood Direct reagent allowed the detection of agent DNA (by four PCRs) at higher concentrations of blood in the reaction mixture (2.5%) than the Fast Virus reagent (0.5%), although LoDs differed between assays and reagent combinations. Across both groups, the KAPA Blood Direct reagent was determined to be the optimal reagent for inhibition relief in PCR.

  12. A Method for Simultaneous Determination of 25-Hydroxyvitamin D3 and Its 3-Sulfate in Newborn Plasma by LC/ESI-MS/MS after Derivatization with a Proton-Affinitive Cookson-Type Reagent

    PubMed Central

    Higashi, Tatsuya; Yokota, Mai; Goto, Ayaka; Komatsu, Kenji; Sugiura, Takahiro; Ogawa, Shoujiro; Satoh, Mamoru; Nomura, Fumio

    2016-01-01

    A method for the simultaneous determination of 25-hydroxyvitamin D3 [25(OH)D3] and its 3-sulfate [25(OH)D3S] in newborn plasma, which is expected to be helpful in the assessment of the vitamin D status, using stable isotope-dilution liquid chromatography/electrospray ionization-tandem mass spectrometry (LC/ESI-MS/MS) has been developed and validated. The plasma was pretreated based on the deproteinization and solid-phase extraction, then subjected to derivatization with 4-(4-dimethylaminophenyl)-1,2,4-triazoline-3,5-dione (DAPTAD). The derivatization enabled the accurate quantification of 25(OH)D3 without interference from 3-epi-25(OH)D3 and also facilitated the simultaneous determination of the two metabolites by LC/positive ESI-MS/MS. Quantification was based on the selected reaction monitoring with the characteristic fragmentation of the DAPTAD-derivatives during MS/MS. This method was reproducible (intra- and inter-assay relative standard deviations of 7.8% or lower for both metabolites) and accurate (analytical recovery, 95.4–105.6%). The limits of quantification were 1.0 ng/mL and 2.5 ng/mL for 25(OH)D3 and 25(OH)D3S, respectively, when using a 20-μL sample. The developed method was applied to the simultaneous determination of plasma 25(OH)D3 and 25(OH)D3S in newborns; it was recognized that the plasma concentration of 25(OH)D3S is significantly higher than that of 25(OH)D3, and preterm newborns have lower plasma 25(OH)D3S concentrations than full-term newborns. PMID:27656337

  13. 2-Nitroso-1-naphthol as a selective reagent for preconcentration of cobalt by vortex assisted combined with solidification of organic droplet and its determination by flame atomic absorption spectrometry.

    PubMed

    Chamsaz, Mahmoud; Eftekhari, Mohammad; Eftekhari, Ali; Yekkebashi, Ali

    2013-11-01

    Highly rapid and selective vortex-assisted liquid-liquid microextraction based on solidification of organic drop has been used for determination of cobalt ion. 2-Nitroso-1-naphthol (2N1N) was used as a selective complexing agent to form stable cobalt-2N1N complex which can be extracted with 1-undecanol at a short time by the assistance of vortex agitator system followed by its determination using flame atomic absorption spectrometry. In vortex assisted, vigorous vortex stream as well as the vibrant effect of vortex system cause very fine droplets of extraction solvent to be produced and extraction occurred at a short time. Some parameters influencing the extraction process such as pH of samples, concentration of 2-nitroso-1-naphthol, extraction solvent volume, extraction time, ionic strength and surfactant addition, as well as interferences were evaluated in detail and optimum conditions were selected. At the optimum conditions, the calibration curve was linear in the range of 15 to 400 μg L(-1) of cobalt ions. The relative standard deviation based on ten replicate analysis of sample solution containing 50 μg L(-1) of cobalt was 3.4%. The detection limit (calculated as the concentration equivalent to three times of the standard deviation of the blank divided by the slope of the calibration curve after preconcentration) was 5.4 μg L(-1). The accuracy of the proposed method was successfully evaluated by the analysis of certified reference materials. This selective and highly rapid method was used for determination of cobalt ions in different water samples.

  14. CPTC expand scope of Reagents and Resources Core - Office of Cancer Clinical Proteomics Research

    Cancer.gov

    Whether in determining if a women is pregnant or not by measuring human chorionic gonadotropin or determining whether someone is HIV positive, antibodies and other affinity reagents play a key role both in diagnostic decision making and advancing the research field.

  15. Estimation of uncertainty from method validation data: Application to a reverse-phase high-performance liquid chromatography method for the determination of amino acids in gelatin using 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate reagent.

    PubMed

    Azilawati, M I; Dzulkifly, M H; Jamilah, B; Shuhaimi, M; Amin, I

    2016-09-10

    A detailed procedure for estimating uncertainty according to the Laboratory of Government Chemists/Valid Analytical Measurement (LGC/VAM) protocol for determination of 18 amino acids in gelatin is proposed. The expanded uncertainty was estimated using mainly the method validation data (precision and trueness). Other sources of uncertainties were contributed by components in standard preparation measurements. The method scope covered a single matrix (gelatin) under a wide range of analyte concentrations. The uncertainty of method precision, μ(P) was 0.0237-0.1128pmolμl(-1) in which hydroxyproline and histidine represented the lowest and highest values of uncertainties, respectively. Proline and phenylalanine represented the lowest and highest uncertainties value for method recovery, μ(R) that was estimated within 0.0064-0.0995pmolμl(-1). The uncertainties from other sources, μ(Std) were 0.0325, 0.0428 and 0.0413pmolμl(-1) that were contributed by hydroxyproline, other amino acids and cystine, respectively. Hydroxyproline and phenylalanine represented the lowest and highest values of expanded uncertainty, U(y) that were determined at 0.0949 and 0.2473pmolμl(-1), respectively. The data were accurately defined and fulfill the technical requirements of ISO 17025:2005. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Correlation of physical parameters during radiochemical synthesis of (18)F positron emission tomography radiopharmaceuticals.

    PubMed

    Tiwari, Anjani K; Varshney, Raunak; Kaushik, Aruna; Datta, Anupama; Singh, Lokendra; Mishra, Anil K

    2011-06-01

    Positron emission tomography is a highly specialized imaging technique using short-lived radiolabel substances to produce extremely high resolution images of the body's biological function. The (18)F(-) ion is produced via the (18)O(p,n)(18)F reaction using a silver target cell filled with 1.4 mL of enriched [(18)O] water. On a typical run, the target is irradiated for 45 minutes with 16.5 MeV protons (on target) and an average beam current of 5-45 mA. When the same reaction takes place with [(16)O] water [(13)N] Ammonia is produced as the primary product by the abstraction of hydrogen from water. This study investigated the physical parameters of medical cyclotron during the radiochemical process with induced radioactivity flux and mutual correlation of physical parameters for 16.5 MeV medical cyclotron at the INMAS Delhi, India. It is observed that by getting farther from the target, the relative number of low-energy neutrons increases while the overall flux of neutrons decreases. This is due to multiple scattering of high-energy neutrons in the walls and eventually absorption of low-energy neutrons. The other parameters are also linked with each other which are correlatable.

  17. Placement of the radiochemical processing plant at Oak Ridge National Laboratory into a safe standby condition

    SciTech Connect

    Holladay, D.W.; Bopp, C.D.; Farmer, A.J.; Johnson, J.K.; Miller, C.H.; Powers, B.A.; Collins, E.D.

    1986-01-01

    Extensive upgrade, cleanup, and decontamination efforts are being conducted for appropriate areas in the Radiochemical Processing Plant (RPP) with the goal of achieving ''safe standby'' condition by the end of FY 1989. The ventilation system must maintain containment; thus, it is being upgraded via demolition and replacement of marginally adequate ductwork, fans, and control systems. Areas that are being decontaminated and stripped of various services (e.g., piping, ductwork, and process tanks) include hot cells, makeup rooms, and pipe tunnels. Operating equipment that is being decontaminated includes glove boxes and hoods. Replacement of the ventilation system and removal of equipment from pipe tunnels, cells, and makeup rooms are accomplished by contact labor by workers using proper attire, safety rules, and shielding. Removal of contaminated ductwork and piping is conducted with containment enclosures that are strategically located at breakpoints, and methods of separation are chosen to conform with health physics requirements. The methods of cutting contaminated piping and ductwork include portable reciprocating saws, pipe cutters, burning, and plasma torch. Specially designed containment enclosures will be used to prevent the spread of radioactive contamination while maintaining adequate ventilation. 6 figs.

  18. Overview of the application of nanosecond electron beams for radiochemical sterilization

    SciTech Connect

    Kotov, Y.A.; Sokovnin, S.Y.

    2000-02-01

    Problems concerning the use of nanosecond electron beams for sterilization of hermetically packed objects, and powdered or granulated materials, are discussed. The advantages and disadvantages of this type of radiation sterilization are demonstrated. The results are of interest to researchers who study the mechanism by which nanosecond electron beams act on microorganisms. It is worth considering repetitively pulsed electron accelerators as highly promising systems for use in commercial sterilization applications. Technologies and setups for the radiochemical sterilization (RCS) of medical glassware for blood products, beer bottles, bone meal used in food industry, medical instruments (surgical needles, systems for human kidneys), and of the external packaging for some biological materials used in ophthalmology are discussed. Such applications have been developed based on the use of the URT-0.2 and URT-0.5 repetitively nanosecond-pulsed electron accelerators. The observed sterilization of areas shaded from line-of-site irradiation and of the bottoms of, for example, glassware cannot be attributed to radiation sterilization alone, since the glass thickness was much larger than the range of electrons. Therefore, it can be conjectured that the demonstrated sterilization effect is due both to the electron beam and to the ozone and chemical radicals produced by the beam. Thus, one may introduce the notion of RCS.

  19. Radiochemical characterization of produced water from two production offshore oilfields in Ghana.

    PubMed

    Kpeglo, D O; Mantero, J; Darko, E O; Emi-Reynolds, G; Faanu, A; Manjón, G; Vioque, I; Akaho, E H K; Garcia-Tenorio, R

    2016-02-01

    Produced water from two Ghanaian offshore production oilfields has been characterized using alpha spectrometry after radiochemical separation, non-destructive gamma spectrometry and ICP-MS and other complimentary analytical tools. The measured concentrations of main NORM components were in the range of 6.2-22.3 Bq.L(-1), 6.4-35.5 Bq.L(-1), and 0.7-7.0 Bq.L(-1) for (226)Ra, (228)Ra and (224)Ra respectively. A good correlation between several physico-chemical parameters and radium isotopes was observed in each production oilfield. The radium concentrations obtained in this study for produced water from the two oilfields of Ghana are of radiological importance and hence there may be the need to put in place measures for future contamination concerns due to their bioavailability in the media and bioaccumulation characteristics. The results will assist in critical decision making for future set up of appropriate national guidelines for the management of NORM waste from the emerging oil and gas industry in Ghana. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Radium-223: From Radiochemical Development to Clinical Applications in Targeted Cancer Therapy

    SciTech Connect

    Bruland, Oyvind S.; Jonasdottir, Thora J.; Fisher, Darrell R.; Larsen, Roy H.

    2008-09-15

    The radiochemical properties of radium-223 (223Ra, T1/2 = 11.4 d) render this alpha-emitting radionuclide promising for targeted cancer therapy. Together with its short-lived daughters, each 223Ra decay produces four alpha-particle emissions—which enhance therapy effectiveness at the cellular level. In this paper, we review the recently published data reported for pre-clinical and clinical use of 223Ra in cancer treatment. We have evaluated two distinct chemical forms of 223Ra in vivo: 1) cationic 223Ra as dissolved RaCl2, and 2) liposome-encapsulated 223Ra. Cationic 223Ra seeks metabolically active osteoblastic bone and tumor lesions with high uptake and strong binding affinity based on its similarities to calcium. Based on these properties, we have advanced the clinical use of 223Ra for treating bone metastases from late-stage breast and prostate cancer. The results show impressive anti-tumor activity and improved overall survival in hormone-refractory prostate cancer patients with bone metastases. In other studies, we have evaluated the biodistribution and tumor uptake of liposomally encapsulated 223Ra in mice with human osteosarcoma xenografts, and in dogs with spontaneous osteosarcoma and associated soft tissue metastases. Results indicate excellent biodistributions in both species. In dogs, we found considerable uptake of liposomal 223Ra in cancer metastases in multiple organs, resulting in favorable tumor-to-normal soft tissue ratios. Collectively, these findings show an outstanding potential for 223Ra as a therapeutic agent.

  1. Hypoxanthine phosphoribosyltransferase: radiochemical assay procedures for the forward and reverse reactions

    SciTech Connect

    Smithers, G.W.; O'Sullivan, W.J.

    1985-02-15

    Simple and rapid radiochemical assay procedures for the forward (IMP synthesis) and reverse (IMP pyrophosphorolysis) reactions catalyzed by hypoxanthine phosphoribosyltransferase have been developed. Enzyme activity in the forward direction was assessed by measuring the amount of (8-/sup 14/C)IMP formed from (8-/sup 14/C)hypoxanthine following their separation by polyethyleneimine-cellulose TLC in methanol:water (1:1, v/v). (8-/sup 14/C)IMP has been synthesized from (8-/sup 14/C)hypoxanthine, using hypoxanthine phosphoribosyltransferase derived from human brain, with subsequent purification by elution from phenyl boronate-agarose. Enzyme activity in the reverse direction was assessed by measuring the amount of (8-/sup 14/C)uric acid formed from the labeled IMP following their separation by polyethyleneimine-cellulose TLC in 0.2 M LiCl saturated with boric acid (pH 4.5):95% ethanol (1:1, v/v), the transferase reaction being coupled with excess xanthine oxidase and catalase to overcome the unfavorable equilibrium.

  2. Sedimentological and radiochemical characteristics of marsh deposits from Assateague Island and the adjacent vicinity, Maryland and Virginia, following Hurricane Sandy

    USGS Publications Warehouse

    Smith, Christopher G.; Marot, Marci E.; Ellis, Alisha M.; Wheaton, Cathryn J.; Bernier, Julie C.; Adams, C. Scott

    2015-09-15

    This report serves as an archive for sedimentological and radiochemical data derived from the surface sediments and marsh cores collected March 26–April 4, 2014. Select surficial data are available for the additional sampling periods October 21–30, 2014. Downloadable data are available as Excel spreadsheets and as JPEG files. Additional files include: Field documentation, x-radiographs, photographs, detailed results of sediment grain size analyses, and formal Federal Geographic Data Committee metadata (data downloads).

  3. Production of latex agglutination reagents for pneumococcal serotyping

    PubMed Central

    2013-01-01

    Background The current ‘gold standard’ for serotyping pneumococci is the Quellung test. This technique is laborious and requires a certain level of training to correctly perform. Commercial pneumococcal latex agglutination serotyping reagents are available, but these are expensive. In-house production of latex agglutination reagents can be a cost-effective alternative to using commercially available reagents. This paper describes a method for the production and quality control (QC) of latex reagents, including problem solving recommendations, for pneumococcal serotyping. Results Here we describe a method for the production of latex agglutination reagents based on the passive adsorption of antibodies to latex particles. Sixty-five latex agglutination reagents were made using the PneuCarriage Project (PCP) method, of which 35 passed QC. The other 30 reagents failed QC due to auto-agglutination (n=2), no reactivity with target serotypes (n=8) or cross-reactivity with non-target serotypes (n=20). Dilution of antisera resulted in a further 27 reagents passing QC. The remaining three reagents passed QC when prepared without centrifugation and wash steps. Protein estimates indicated that latex reagents that failed QC when prepared using the PCP method passed when made with antiserum containing ≤ 500 μg/ml of protein. Sixty-one nasopharyngeal isolates were serotyped with our in-house latex agglutination reagents, with the results showing complete concordance with the Quellung reaction. Conclusions The method described here to produce latex agglutination reagents allows simple and efficient serotyping of pneumococci and may be applicable to latex agglutination reagents for typing or identification of other microorganisms. We recommend diluting antisera or removing centrifugation and wash steps for any latex reagents that fail QC. Our latex reagents are cost-effective, technically undemanding to prepare and remain stable for long periods of time, making them ideal for

  4. Production of latex agglutination reagents for pneumococcal serotyping.

    PubMed

    Ortika, Belinda D; Habib, Maha; Dunne, Eileen M; Porter, Barbara D; Satzke, Catherine

    2013-02-05

    The current 'gold standard' for serotyping pneumococci is the Quellung test. This technique is laborious and requires a certain level of training to correctly perform. Commercial pneumococcal latex agglutination serotyping reagents are available, but these are expensive. In-house production of latex agglutination reagents can be a cost-effective alternative to using commercially available reagents. This paper describes a method for the production and quality control (QC) of latex reagents, including problem solving recommendations, for pneumococcal serotyping. Here we describe a method for the production of latex agglutination reagents based on the passive adsorption of antibodies to latex particles. Sixty-five latex agglutination reagents were made using the PneuCarriage Project (PCP) method, of which 35 passed QC. The other 30 reagents failed QC due to auto-agglutination (n=2), no reactivity with target serotypes (n=8) or cross-reactivity with non-target serotypes (n=20). Dilution of antisera resulted in a further 27 reagents passing QC. The remaining three reagents passed QC when prepared without centrifugation and wash steps. Protein estimates indicated that latex reagents that failed QC when prepared using the PCP method passed when made with antiserum containing ≤ 500 μg/ml of protein. Sixty-one nasopharyngeal isolates were serotyped with our in-house latex agglutination reagents, with the results showing complete concordance with the Quellung reaction. The method described here to produce latex agglutination reagents allows simple and efficient serotyping of pneumococci and may be applicable to latex agglutination reagents for typing or identification of other microorganisms. We recommend diluting antisera or removing centrifugation and wash steps for any latex reagents that fail QC. Our latex reagents are cost-effective, technically undemanding to prepare and remain stable for long periods of time, making them ideal for use in low-income countries.

  5. A sensitive fluorescence reagent, 2-[2-(7H-dibenzo[a,g]carbazol-7-yl)-ethoxy]ethyl chloroformate, for amino acids determination in Saussurea involucrate and Artemisia capillaris Thunb using high-performance liquid chromatography with fluorescence detection and identification with mass spectroscopy/electrospray ionization source.

    PubMed

    Li, Guoliang; Sun, Zhiwei; Song, Cuihua; Xia, Lian; Zheng, Jie; Suo, Yourui; You, Jinmao

    2011-06-01

    Recent researches shows that amino acids (AA) are not only cell signaling molecules but are also regulators of gene expression and the protein phosphorylation cascade. More precise analysis of AA composition is reckoned to be one of the most important applications in the biomedical and pharmaceutical fields. In this paper, we develop a sample, sensitive and mild method using 2-[2-(7H-dibenzo[a,g]carbazol-7-yl)-ethoxy]ethyl chloroformate (DBCEC) as A labeling reagent for AA determination by high-performance liquid chromatography (HPLC) with fluorescence detection (FLD) and identification with mass spectroscopy. The maximum excitation and emission wavelengths for DBCEC-AA derivatives were 300 and 395 nm, respectively. This method, in conjunction with a gradient elution, offered a baseline resolution of 20 AA on a reversed-phase Hypersil BDS C(18) column. LC separation for the derivatized AA showed good reproducibility, and all AA were found to give excellent linear responses with correlation coefficients > 0.9993. The calculated detection limits with a 25.0 fmol injection of each AA (at a signal-to-noise ratio of 3:1) ranged from 2.62 to 22.6 fmol. This method was applied to determine the AA composition in Saussurea involucrate and Artemisia capillaris Thunb. Meanwhile, this method exhibits a powerful potential for trace analysis of AA from biomedicine, foodstuff and other complex samples.

  6. New osmium-based reagent for the dihydroxylation of alkenes.

    PubMed

    Donohoe, Timothy J; Harris, Robert M; Butterworth, Sam; Burrows, Jeremy N; Cowley, Andrew; Parker, Jeremy S

    2006-06-09

    The cis dihydroxylation of alkenes is most efficiently accomplished by reaction with osmium tetroxide. Recently, the expense and toxicity of osmium tetroxide have led to a number of attempts to harness alternative osmium-based reagents, including microencapsulation and solid support techniques. We describe here the development of a new nonvolatile, stable, and recoverable osmium-based reagent devised for the stoichiometric cis dihydroxylation of alkenes. Although attempts to make this new dihydroxylation work with catalytic amounts of this reagent were unsuccessful, we did develop a sensitive test for free osmium tetroxide leached from the reagent in situ: this test may well have uses in probing future applications of derivatized osmium reagents.

  7. Determination of D-amino acids labeled with fluorescent chiral reagents, R(-)- and S(+)-4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N, N-dimethylaminosulfonyl)-2,1,3-benzoxadiazoles, in biological and food samples by liquid chromatography.

    PubMed

    Jin, D; Miyahara, T; Oe, T; Toyo'oka, T

    1999-04-10

    D-Amino acids in food and biological samples labeled with R(-)- and S(+)-4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N, N-dimethylaminosulfonyl)-2,1,3-benzoxadiazoles (DBD-PyNCS) were separated by reversed-phase chromatography and detected fluorometrically at 550 nm (excitation at 460 nm). DL-Amino acids were efficiently labeled at 55 degrees C for 20 min in basic medium. The resulting thiocarbamoyl-amino acids were resolved by an isocratic elution using water:30% methanol in acetonitrile (72:28) containing 0.1% trifluoracetic acid as mobile phase for hydrophilic amino acids and gradient elutions using sodium acetate buffer (pH 5. 2)/acetonitrile as gradient solvent mixture for hydrophobic amino acids, respectively. The detection limits (S/N = 3) of DL-amino acids tested were in the range of 0.16-0.75 pmol. The proposed method was applied to determine the D-amino acid(s) in milk, cream, fermented dairy products (yogurt and yakult), tomato products (juice, puree, and catchup), fermented beverages (beer and red wine), and human urine. The existence of D-amino acid(s) was demonstrated in all the samples tested. Furthermore, the identification of the D-amino acid(s) was performed using both isomers of DBD-PyNCS and by on-line HPLC-electrospray ionization-MS.

  8. Investigation of benzoyloximes as benzoylating reagents: benzoyl-Oxyma as a selective benzoylating reagent.

    PubMed

    Burugupalli, Satvika; Shah, Sayali; van der Peet, Phillip L; Arora, Seep; White, Jonathan M; Williams, Spencer J

    2016-01-07

    Hydroxybenzotriazole (HOBt) and HOBt-derived reagents have been classified as Class I explosives, with restrictions on their transportation and storage. We explored a range of benzoylated oxime-based reagents as alternatives to benzoyloxybenzotriazole (BBTZ) for the selective benzoylation of carbohydrate polyols. Benzoylated oximes derived from 2-hydroximino-malononitrile, ethyl 2-hydroximino-2-cyanoacetate (Oxyma), and tert-butyl 2-hydroximino-2-cyanoacetate were most effective for benzoylation of a simple primary alcohol, with yields approaching that obtained for BBTZ. When applied to carbohydrate diols, the most effective reagent was identified as benzoyl-Oxyma. Benzoyl-Oxyma is a highly crystalline, readily prepared alternative to BBTZ, useful in the selective benzoylation of carbohydrate polyols.

  9. The presence of sodium nitrate in generator eluate decreases the radiochemical purity of 99mTc-sestamibi.

    PubMed

    Métayé, Thierry; Rosenberg, Thierry; Guilhot, Joëlle; Bouin-Pineau, Marie-Hélène; Perdrisot, Rémy

    2012-09-01

    A high radiochemical purity (RCP) is recommended for radiopharmaceutical compounds used in the clinical practice of nuclear medicine. However, some preparations of (99m)Tc-sestamibi contain excess impurities (>6%). To understand the origin of these impurities, we investigated the effect of sodium nitrate on the RCP of sestamibi preparations by testing eluates from 3 commercially available (99m)Tc generators. The sestamibi kits (Stamicis) were reconstituted with (99m)Tc eluate from nitrate-containing wet-column (NCWC), nitrate-free wet-column (NFWC), and nitrate-free dry-column (NFDC) generators. Sodium nitrate was 0.05 mg/mL in eluates from the NCWC generators. The RCP was determined using aluminum oxide sheets as the stationary phase and absolute ethanol as the mobile phase. Succimer, tetrofosmin, oxidronate, exametazine, albumin nanocolloid, and soluble albumin were also tested for their RCP values with eluates from the 3 different (99m)Tc generators. The RCP assessment of (99m)Tc-sestamibi was performed on 127 Stamicis preparations. Significantly lower RCP values were found for Stamicis kits prepared with the NCWC generator than for Stamicis prepared with the NFWC (P < 0.0001) and NFDC (P < 0.0001) generators. The number of Stamicis preparations with an RCP under 94% was greater with the NCWC generator (32 of 53 kits) than with the NFDC (2 of 51 kits) or NFWC (0 of 23 kits) generator. Furthermore, the addition of a 0.05 mg/mL concentration of nitrate in NFWC generator eluates significantly decreased the RCP of the Stamicis preparation. In the absence of nitrate in (99m)Tc eluate, no difference was observed between the RCP values of Stamicis kits prepared with the NFWC and NFDC generators. The (99m)Tc impurities generated by nitrates did not modify the quality of myocardial imaging (normal heart-to-lung ratio, 2.2), probably because these impurities are not in the heart field of view. No other tested (99m)Tc-radiopharmaceutical interfered with nitrates. We

  10. 324 Building radiochemical engineering cells, high-level vault, low-level vault, and associated areas closure plan

    SciTech Connect

    Barnett, J.M.

    1998-03-25

    The Hanford Site, located adjacent to and north of Richland, Washington, is operated by the US Department of Energy, Richland Operations Office (RL). The 324 Building is located in the 300 Area of the Hanford Site. The 324 Building was constructed in the 1960s to support materials and chemical process research and development activities ranging from laboratory/bench-scale studies to full engineering-scale pilot plant demonstrations. In the mid-1990s, it was determined that dangerous waste and waste residues were being stored for greater than 90 days in the 324 Building Radiochemical Engineering Cells (REC) and in the High-Level Vault/Low-Level Vault (HLV/LLV) tanks. [These areas are not Resource Conservation and Recovery Act of 1976 (RCRA) permitted portions of the 324 Building.] Through the Hanford Federal Facility Agreement and Consent Order (Tri-Party Agreement) Milestone M-89, agreement was reached to close the nonpermitted RCRA unit in the 324 Building. This closure plan, managed under TPA Milestone M-20-55, addresses the identified building areas targeted by the Tri-Party Agreement and provides commitments to achieve the highest degree of compliance practicable, given the special technical difficulties of managing mixed waste that contains high-activity radioactive materials, and the physical limitations of working remotely in the areas within the subject closure unit. This closure plan is divided into nine chapters. Chapter 1.0 provides the introduction, historical perspective, 324 Building history and current mission, and the regulatory basis and strategy for managing the closure unit. Chapters 2.0, 3.0, 4.0, and 5.0 discuss the detailed facility description, process information, waste characteristics, and groundwater monitoring respectively. Chapter 6.0 deals with the closure strategy and performance standard, including the closure activities for the B-Cell, D-Cell, HLV, LLV; piping and miscellaneous associated building areas. Chapter 7.0 addresses the

  11. Optically transparent, superhydrophobic methyltrimethoxysilane based silica coatings without silylating reagent

    NASA Astrophysics Data System (ADS)

    Kavale, Mahendra S.; Mahadik, D. B.; Parale, V. G.; Wagh, P. B.; Gupta, Satish C.; Rao, A. Venkateswara; Barshilia, Harish C.

    2011-10-01

    The superhydrophobic surfaces have drawn lot of interest, in both academic and industries because of optically transparent, adherent and self-cleaning behavior. Surface chemical composition and morphology plays an important role in determining the superhydrophobic nature of coating surface. Such concert of non-wettability can be achieved, using surface modifying reagents or co-precursor method in sol-gel process. Attempts have been made to increase the hydrophobicity and optical transparency of methyltrimethoxysilane (MTMS) based silica coatings using polymethylmethacrylate (PMMA) instead of formal routes like surface modification using silylating reagents. The optically transparent, superhydrophobic uniform coatings were obtained by simple dip coating method. The molar ratio of MTMS:MeOH:H 2O was kept constant at 1:5.63:1.58, respectively with 0.5 M NH 4F as a catalyst and the weight percent of PMMA varied from 1 to 8. The hydrophobicity of silica coatings was analyzed by FTIR and contact angle measurements. These substrates exhibited 91% optical transmittance as compared to glass and water drop contact angle as high as 171 ± 1°. The effect of humidity on hydrophobic nature of coating has been studied by exposing these films at relative humidity of 90% at constant temperature of 30 °C for a period of 45 days. The micro-structural studies carried out by transmission electron microscopy (TEM).

  12. Reaction rates between water and the Karl Fischer reagent.

    PubMed

    Cedergren, A

    1974-04-01

    Reaction rates between water and the Karl Fischer reagent have been determined by potentiometric measurement for various compositions of the Karl Fischer reagent. The study has been made with an iodine complex concentration of 0.3-1.2 mM and sulphur dioxide complex at 0.01-0.5M. The concentration of excess of pyridine had no measurable effect on the rate of the main reaction. The reaction was found to be first-order with respect to iodine complex, to sulphur dioxide complex, and to water. The rate constant was (1.2+/-0.2) x 10(3) 1(2). mole(-2). sec(-1). In an ordinary titration it is therefore essential to keep the sulphur dioxide concentration high for the reaction to go to completion within a reasonable time. The extent of side-reactions was found to be independent of the iodine concentration at low concentrations. The side-reactions increased somewhat with increasing sulphur dioxide pyridine concentrations and decreased to about 60% when the temperature was lowered from 24 degrees to 7 degrees.

  13. Facile Oxidative Rearrangements Using Hypervalent Iodine Reagents

    PubMed Central

    Singh, Fateh V; Rehbein, Julia; Wirth, Thomas

    2012-01-01

    Aromatic substituents migrate in a novel oxidative cyclization mediated by iodine(III) reagents. 4-Arylbut-3-enoic acids are cyclized and rearranged to 4-arylfuran-2(5H)-ones by hypervalent iodine compounds in good to excellent yields under mild reaction conditions. Other ring sizes are also accessible. The mechanism of the reaction is described in detail, and calculations highlight the cationic nature of the intermediates in the rearrangement. The fast access to heavily substituted furanones is used for the synthesis of biologically active derivatives. PMID:24551514

  14. DIAZOPHTHALOCYANINS AS REAGENTS FOR FINE STRUCTURAL CYTOCHEMISTRY

    PubMed Central

    Tice, Lois Withrow; Barrnett, Russell J.

    1965-01-01

    This paper reports the synthesis of 14 diazophthalocyanins containing Mg, Cu, or Pb as the chelated metal. To assess the usefulness of these compounds for fine structural cytochemistry, the relative coupling rates with naphthols were tested as well as the solubility of the resulting azo dyes. Three of the diazotates were reacted with tissue proteins in aldehyde-fixed material, and the density increases thus produced were compared in the electron microscope with those produced by staining similarly fixed material with the phthalocyanin dye, Alcian Blue. Finally, one of the diazotates was used as a capture reagent for the demonstration of the sites of acid phosphatase activity with the electron microscope. PMID:14283629

  15. A radiochemical, hydrochemical and dissolved gas study of groundwaters in the Molasse basin of Upper Austria

    NASA Astrophysics Data System (ADS)

    Andrews, J. N.; Goldbrunner, J. E.; Darling, W. G.; Hooker, P. J.; Wilson, G. B.; Youngman, M. J.; Eichinger, L.; Rauert, W.; Stichler, W.

    1985-05-01

    The Innviertel (Ottnangian) formation of the Molasse zone of Upper Austria is of major importance as a source of potable water. A hydrochemical, radiochemical and dissolved gas study was undertaken to establish the flow pattern in the Innviertel and its relationship to groundwaters in deeper formations in the Molasse basin. The Innviertel groundwaters could be differentiated into three groups on the basis of their chemical compositions. Waters from shallow boreholes which sampled very localised systems are oxidising waters of the Ca-bicarbonate type and may have high 3H contents. A transition to reducing groundwaters occurs in the second and third groups, with Na + replacing Ca 2+ as the dominant cation and sulphate being reduced to sulphide. The uranium solution chemistry also changes systematically with this change in redox conditions. The 234U/ 238U activity ratios are enhanced for group 2 groundwaters and decrease again in group 3 groundwaters. The low Cl contents of all the Innviertel groundwaters indicate that the marine sediments have been completely flushed by meteoric water and this is confirmed by the stable isotope composition of the water. Groundwater residence times have been estimated from hydrological data, radiogenic 4He accumulation rates and palaeotemperatures of recharge which were estimated from noble gas contents. The 3He/ 4He ratio shows that most radiogenic He diffuses from the basement granite and the He flux was estimated on the basis of diffusion theory. Groundwater residence times were assessed from this diffusive flux of helium and together with the recharge temperatures, indicate that the evolved groundwaters of the Innviertel were recharged during the interstadial which preceded the last glaciation.

  16. Influence of different chelators on the radiochemical properties of a 68-Gallium labelled bombesin analogue.

    PubMed

    Asti, Mattia; Iori, Michele; Capponi, Pier C; Atti, Giulia; Rubagotti, Sara; Martin, René; Brennauer, Albert; Müller, Marco; Bergmann, Ralf; Erba, Paola A; Versari, Annibale

    2014-01-01

    The radiolabelled bombesin analogue AMBA shows high potential for diagnosis and treatment of prostate and breast cancer, but the influence of different chelators, which differ in terms of radiochemical reactivity and stability, have not been explored so far. In order to find the best suitable chelator for labelling of AMBA, we synthesized AMBA analogues linked to the most commonly used chelators DOTA, NOTA and NODAGA and compared their reactivity and stability after labelling with 68-Gallium. For the synthesis of DO3A-, NO2A- and NODAGA-AMBA, a solid-phase synthesis approach was used. The influence of concentration, pH and temperature on the radiolabelling was analysed. The in vitro stability of all complexes in saline, human serum, human whole blood and against transchelation and transmetallation was analysed. The peptides were synthesised in high yield and purity. Purity and identity of products and impurities were confirmed using UHPLC coupled to ESI-MS. Radiolabelling of these peptides was optimal at elevated temperature, although room temperature labelling was reported previously for NOTA and NODAGA chelators. The highest reactivity was observed for NODAGA-AMBA. On preparation of NO2A-AMBA, the formation of a by-product was detected with HPLC. More detailed analysis revealed the formation of an isomer with the same mass to charge ratio which led to the conclusion that a coordination isomer was formed. All complexes showed high stability in saline, human serum or when challenged with DTPA, transferrin and varying metals (Fe(3+), Cu(2+), Zn(2+)). Conversely, the stability in human blood was low, and varying metabolites were detected and identified by ESI-MS. All three precursors are available in high yields suitable for routine production. NODAGA-AMBA showed the most favoured features when labelled with 68-gallium, but a further comparison in vivo should be performed in order to confirm the superior features found in vitro. © 2013.

  17. Radiochemically-Supported Microbial Communities: A Potential Mechanism for Biocolloid Production of Importance to Actinide Transport

    SciTech Connect

    Moser, Duane P.; Hamilton-Brehm, Scott D.; Fisher, Jenny C.; Bruckner, James C.; Kruger, Brittany; Sackett, Joshua; Russell, Charles E.; Onstott, Tullis C.; Czerwinski, Ken; Zavarin, Mavrik; Campbell, James H.

    2014-06-01

    Due to the legacy of Cold War nuclear weapons testing, the Nevada National Security Site (NNSS, formerly known as the Nevada Test Site (NTS)) contains millions of Curies of radioactive contamination. Presented here is a summary of the results of the first comprehensive study of subsurface microbial communities of radioactive and nonradioactive aquifers at this site. To achieve the objectives of this project, cooperative actions between the Desert Research Institute (DRI), the Nevada Field Office of the National Nuclear Security Administration (NNSA), the Underground Test Area Activity (UGTA), and contractors such as Navarro-Interra (NI), were required. Ultimately, fluids from 17 boreholes and two water-filled tunnels were sampled (sometimes on multiple occasions and from multiple depths) from the NNSS, the adjacent Nevada Test and Training Range (NTTR), and a reference hole in the Amargosa Valley near Death Valley. The sites sampled ranged from highly-radioactive nuclear device test cavities to uncontaminated perched and regional aquifers. Specific areas sampled included recharge, intermediate, and discharge zones of a 100,000-km2 internally-draining province, known as the Death Valley Regional Flow System (DVRFS), which encompasses the entirety of the NNSS/NTTR and surrounding areas. Specific geological features sampled included: West Pahute and Ranier Mesas (recharge zone), Yucca and Frenchman Flats (transitional zone), and the Western edge of the Amargosa Valley near Death Valley (discharge zone). The original overarching question underlying the proposal supporting this work was stated as: Can radiochemically-produced substrates support indigenous microbial communities and subsequently stimulate biocolloid formation that can affect radionuclides in NNSS subsurface nuclear test/detonation sites? Radioactive and non-radioactive groundwater samples were thus characterized for physical parameters, aqueous geochemistry, and microbial communities using both DNA- and

  18. Altered biodistribution of radiopharmaceuticals: role of radiochemical/pharmaceutical purity, physiological, and pharmacologic factors.

    PubMed

    Vallabhajosula, Shankar; Killeen, Ronan P; Osborne, Joseph R

    2010-07-01

    One of the most common problems associated with radiopharmaceuticals is an unanticipated or altered biodistribution, which can have a significant clinical impact on safety, scan interpretation, and diagnostic imaging accuracy. In their most extreme manifestations, unanticipated imaging results may even compromise the utility and or accuracy of nuclear medicine studies. We present here an overall summary of altered biodistribution of radiopharmaceuticals with a special emphasis on the molecular mechanisms involved. Important factors affecting the biodistribution of radiopharmaceuticals can be described in 5 major categories and include (1) radiopharmaceutical preparation and formulation problems; (2) problems caused by radiopharmaceutical administration techniques and procedures; (3) by changes in biochemical and pathophysiology; (4) previous medical procedures, such as surgery, radiation therapy and dialysis; and finally (5) by drug interactions. The altered biodistribution of (99m)Tc radiopharmaceuticals are generally associated with increased amounts of (99m)Tc radiochemical impurities, such as free (99m)TcO(4)(-) and particulate impurities, such as (99m)Tc colloids or (99m)Tc-reduced hydrolyzed species. Faulty injection, such as dose infiltration or contamination with antiseptics and aluminum during dose administration, may cause significant artifacts. The patient's own medical problems, such as abnormalities in the regulation of hormone levels; failure in the function of excretory organs and systems, such as hepatobiliary and genitourinary systems; and even simple conditions, such as excessive talking may contribute to altered biodistribution of radiopharmaceuticals. Previous medical procedures (chemotherapy, radiation therapy, dialysis) and drug interaction are the some of the nontechnical factors responsible for unanticipated biodistribution of radiotracers. This review provides a comprehensive summary of various factors and specific examples to illustrate

  19. Efficacy Assessment of Nucleic Acid Decontamination Reagents Used in Molecular Diagnostic Laboratories

    PubMed Central

    Fischer, Melina; Renevey, Nathalie; Thür, Barbara; Hoffmann, Donata; Beer, Martin; Hoffmann, Bernd

    2016-01-01

    The occurrence of nucleic acid cross contamination in the laboratory resulting in false positive results of diagnostic samples is seriously problematic. Despite precautions to minimize or even avoid nucleic acid cross contaminations, it may appear anyway. Until now, no standardized strategy is available to evaluate the efficacy of commercially offered decontamination reagents. Therefore, a protocol for the reliable determination of nucleic acid decontamination efficacy using highly standardized solution and surface tests was established and validated. All tested sodium hypochlorite-based reagents proved to be highly efficient in nucleic acid decontamination even after short reaction times. For DNA Away, a sodium hydroxide-based decontamination product, dose- and time-dependent effectiveness was ascertained. For two other commercial decontamination reagents, the phosphoric acid-based DNA Remover and the non-enzymatic reagent DNA-ExitusPlus™ IF, no reduction of amplifiable DNA/RNA was observed. In conclusion, a simple test procedure for evaluation of the elimination efficacy of decontamination reagents against amplifiable nucleic acid is presented. PMID:27410228

  20. Semi-reversible cross-linking. Synthesis and application of a novel heterobifunctional reagent.

    PubMed

    Friebel, K; Huth, H; Jany, K D; Trommer, W E

    1981-04-01

    The synthesis of a novel heterobifunctional cross-linking reagent, 3-(4-azido-2-nitrobenzoylseleno)propionic acid is described. The selenol ester function serves as a selective and reversible thiol reagent. Cross-linking is carried out photochemically via nitrene generation. The reagent is well suited for the identification of the environment of a defined cysteine residue according to the principle of semi-reversible cross-linking (Trommer, W.E., Friebel, K., Kiltz, H.-H. & Kolkenbrock. H. (1977) Adv. Exp. Med. Biol. 86A, 187-195). Cleavage of the thiol ester bond (the first anchor point) can be achieved by a variety of labels carrying an amino function thus giving rise to labelled amino acids or proteins in a distance of about 0.7 nm from the known cysteine residue. Optimal conditions were determined by reaction of 3-(4-azido-2-nitrobenzoylseleno)propionic acid and of its unsubstituted analog with glutathione and N alpha-benzoylglycyllysine. Nucleosidetriphosphate-adenylate kinase from pig muscle was chosen as an example to demonstrate the usefulness of the reagent. 14C-labelled aminobutyric acid was applied to cleave the thiol ester bond between the reagent and cysteine-25 leading to labelling of the N-terminal arginine peptide.

  1. Reaction of fluorogenic reagents with proteins

    PubMed Central

    Swearingen, Kristian E.; Dickerson, Jane A.; Turner, Emily H.; Ramsay, Lauren M.; Wojcik, Roza; Dovichi, Norman J.

    2009-01-01

    The fluorogenic reagent Chromeo P465 is considered for analysis of proteins by capillary electrophoresis with laser-induced fluorescence detection. The reagent was first used to label α-lactalbumin; the product was analyzed by capillary zone electrophoresis in a sub-micellar sodium dodecyl sulfate (SDS) buffer. The product generated a set of equally spaced but poorly resolved peaks that formed a broad envelope with a net mobility of 4 × 10−4 cm2 V−1 s−1. The components of the envelope were presumably protein that had reacted with different numbers of labels. The mobility of these components decreased by roughly 1 % with the addition of each label. The signal increased linearly from 1.0 nM to 100 nM α-lactalbumin (r2 = 0.99), with a 3σ detection limit of 70 pM. We then considered the separation of a mixture of ovalbumin, α-chymotrypsinogen A, and αlactalbumin labeled with Chromeo P465; unfortunately, baseline resolution was not achieved with a borax/SDS buffer. Better resolution was achieved with N-cyclohexyl-2-aminoethanesulfonic acid/Tris/SDS/dextran capillary sieving electrophoresis; however, dye interactions with this buffer system produced a less than ideal blank. PMID:18479693

  2. International Standard Reagents for HPV Detection

    PubMed Central

    Pagliusi, Sonia R.; Garland, Suzanne M.

    2007-01-01

    Humam papillomavirus is the commonest genital viral infection in healthy sexually active subjects, and the presence of chronic or persistent HPV types in genital cells may constitute a prognostic marker of underlying, or predict future HPV-associated diseases. A variety of novel tests for detecting the presence of oncogenic HPV types in biological specimens have been reported. These are based on the various stages of infection and viral life cycle. HPV infects squamous epithelium with expression of various gene products intimately linked to epithelial cell differentiation. Hence, there are basically three classes of detectable markers directly derived from HPVs: molecular markers based on detection of nucleic acid sequences, serological markers based on detection of antibodies against viral proteins, and cellular markers based on detection of proteins expressed intracellularly, upon either infection or carcinogenesis. The nature of various assays and the development of international standard reagents for qualitative and quantitative assessment of assay performance are outlined. There is an increasing demand to develop standard tools to assess the quality of HPV detection systems, for regulatory and clinical management purposes. International standard reagents for HPV will help defining the analytical sensitivity and specificity of various detection methods, and will allow assuring that laboratory services used to evaluate disease burden, HPV vaccines, and cancer prevention strategies are accurate and comparable worldwide. The advancement of prophylactic vaccine candidates against HPV infections and related diseases stresses the increasing importance of HPV assays in monitoring the impact of HPV vaccination on disease burden. PMID:17627063

  3. Organometallic Palladium Reagents for Cysteine Bioconjugation

    PubMed Central

    Vinogradova, Ekaterina V.; Zhang, Chi; Spokoyny, Alexander M.; Pentelute, Bradley L.; Buchwald, Stephen L.

    2015-01-01

    Transition-metal based reactions have found wide use in organic synthesis and are used frequently to functionalize small molecules.1,2 However, there are very few reports of using transition-metal based reactions to modify complex biomolecules3,4, which is due to the need for stringent reaction conditions (for example, aqueous media, low temperature, and mild pH) and the existence of multiple, reactive functional groups found in biopolymers. Here we report that palladium(II) complexes can be used for efficient and highly selective cysteine conjugation reactions. The bioconjugation reaction is rapid and robust under a range of biocompatible reaction conditions. The straightforward synthesis of the palladium reagents from diverse and easily accessible aryl halide and trifluoromethanesulfonate precursors makes the method highly practical, providing access to a large structural space for protein modification. The resulting aryl bioconjugates are stable towards acids, bases, oxidants, and external thiol nucleophiles. The broad utility of the new bioconjugation platform was further corroborated by the synthesis of new classes of stapled peptides and antibody-drug conjugates. These palladium complexes show potential as a new set of benchtop reagents for diverse bioconjugation applications. PMID:26511579

  4. Organometallic palladium reagents for cysteine bioconjugation

    NASA Astrophysics Data System (ADS)

    Vinogradova, Ekaterina V.; Zhang, Chi; Spokoyny, Alexander M.; Pentelute, Bradley L.; Buchwald, Stephen L.

    2015-10-01

    Reactions based on transition metals have found wide use in organic synthesis, in particular for the functionalization of small molecules. However, there are very few reports of using transition-metal-based reactions to modify complex biomolecules, which is due to the need for stringent reaction conditions (for example, aqueous media, low temperature and mild pH) and the existence of multiple reactive functional groups found in biomolecules. Here we report that palladium(II) complexes can be used for efficient and highly selective cysteine conjugation (bioconjugation) reactions that are rapid and robust under a range of bio-compatible reaction conditions. The straightforward synthesis of the palladium reagents from diverse and easily accessible aryl halide and trifluoromethanesulfonate precursors makes the method highly practical, providing access to a large structural space for protein modification. The resulting aryl bioconjugates are stable towards acids, bases, oxidants and external thiol nucleophiles. The broad utility of the bioconjugation platform was further corroborated by the synthesis of new classes of stapled peptides and antibody-drug conjugates. These palladium complexes show potential as benchtop reagents for diverse bioconjugation applications.

  5. Organometallic palladium reagents for cysteine bioconjugation.

    PubMed

    Vinogradova, Ekaterina V; Zhang, Chi; Spokoyny, Alexander M; Pentelute, Bradley L; Buchwald, Stephen L

    2015-10-29

    Reactions based on transition metals have found wide use in organic synthesis, in particular for the functionalization of small molecules. However, there are very few reports of using transition-metal-based reactions to modify complex biomolecules, which is due to the need for stringent reaction conditions (for example, aqueous media, low temperature and mild pH) and the existence of multiple reactive functional groups found in biomolecules. Here we report that palladium(II) complexes can be used for efficient and highly selective cysteine conjugation (bioconjugation) reactions that are rapid and robust under a range of bio-compatible reaction conditions. The straightforward synthesis of the palladium reagents from diverse and easily accessible aryl halide and trifluoromethanesulfonate precursors makes the method highly practical, providing access to a large structural space for protein modification. The resulting aryl bioconjugates are stable towards acids, bases, oxidants and external thiol nucleophiles. The broad utility of the bioconjugation platform was further corroborated by the synthesis of new classes of stapled peptides and antibody-drug conjugates. These palladium complexes show potential as benchtop reagents for diverse bioconjugation applications.

  6. U. S. VETERINARY IMMUNE REAGENTS NETWORK: PROGRESS WITH POULTRY IMMUNE REAGENTS

    USDA-ARS?s Scientific Manuscript database

    This poster will present a progress report on the CSREES-funded NRI grant to support a broad community approach to systematically address the immunological reagent gap for the US veterinary immunology research community including for the following groups: ruminants (concentrating on cattle but inclu...

  7. Silyl Glyoxylates. Conception and Realization of Flexible Conjunctive Reagents for Multicomponent Coupling

    PubMed Central

    Boyce, Gregory R.; Greszler, Stephen N.; Linghu, Xin; Malinowski, Justin T.; Nicewicz, David A.; Satterfield, Andrew D.; Schmitt, Daniel C.; Steward, Kimberly M.

    2012-01-01

    This Perspective describes the discovery and development of silyl glyoxylates, a new family of conjunctive reagents for use in multicomponent coupling reactions. The selection of the nucleophilic and electrophilic components determines whether the silyl glyoxylate reagent will function as a synthetic equivalent to the dipolar glycolic acid synthon, the glyoxylate anion synthon, or the α-keto ester homoenolate synthon. The ability to select for any of these reaction modes has translated to excellent structural diversity in the derived three- and four-component coupling adducts. Preliminary findings on the development of catalytic reactions using these reagents are detailed, as are the design and discovery of new reactions directed toward particular functional group arrays embedded within bioactive natural products. PMID:22414181

  8. Preparation, characterization and feasibility study of dialdehyde carboxymethyl cellulose as a novel crosslinking reagent.

    PubMed

    Jiang, Xiaolei; Yang, Zhao; Peng, Yanfei; Han, Baoqin; Li, Zhuoyue; Li, Xiuhua; Liu, Wanshun

    2016-02-10

    The natural biopolymers usually need to be chemically modified by crosslinking reagents to improve their mechanical properties. In the present research, the feasibility of using the dialdehyde carboxymethyl cellulose (DCMC) as a crosslinking reagent was systematically studied. DCMC was prepared by oxidizing carboxymethyl cellulose using sodium periodate. The formation of dialdehyde groups was confirmed by FTIR and the degree of oxidation was determined. The biocompatibility of DCMC was investigated by evaluating its cytotoxicity to L929 fibroblasts and histocompatibility in rat model via intramuscular and subcutaneous injection. DCMC-crosslinked carboxymethyl chitosan (DCMC-CMCTS) was prepared and characterized using the glutaraldehyde-crosslinked CMCTS (GA-CMCTS) as control. The result demonstrated that DCMC was non-cytotoxic, biodegradable and biocompatible. The DCMC-CMCTS displayed significantly better thermostability, swelling capacity and cyto-compatibility compared with GA-CMCTS. Our data provided experimental basis for the future application of DCMC as a novel crosslinking reagent.

  9. Reactive Derivatives of Nucleic Acids and Their Components as Affinity Reagents

    NASA Astrophysics Data System (ADS)

    Knorre, Dmitrii G.; Vlasov, Valentin V.

    1985-09-01

    The review is devoted to derivatives of nucleic acids and their components — nucleotides, nucleoside triphosphates, and oligonucleotides carrying reactive groups. Such derivatives are important tools for the investigation of protein-nucleic acid interactions and the functional topography of complex protein and nucleoprotein structures and can give rise to the prospect of being able to influence in a highly selective manner living organisms, including the nucleic acids and the nucleoproteins of the genetic apparatus. The review considers the principal groups of such reagents, the methods of their synthesis, and their properties which determine the possibility of their use for the selective (affinity) modification of biopolymers. The general principles of the construction of affinity reagents and their applications are analysed in relation to nucleotide affinity reagents. The bibliography includes 121 references.

  10. [Evaluating the Stability of Loop-Mediated Isothermal Amplification Reagents at Irregular Storage Temperatures for On-Site Diagnosis].

    PubMed

    Inoshima, Yasuo; Ishiguro, Naotaka

    2015-01-01

    Temperature-stability of loop-mediated isothermal amplification (LAMP) reagents was determined for their use in on-site diagnosis, such as in farms/pastures. Bst and Csa DNA polymerases and the reagents that were stored at different temperatures (4 or 25°C) for 1, 2, or 4 days were used for the LAMP assay to detect orf virus DNA as a model. After storage at 4 and 25°C for 2 days, the enzymes and reagents were found to retain sufficient activity to carry out successful DNA amplification. Visual diagnosis was also possible with the reagents (Loopamp Fluorescent Detection Reagent or hydroxy naphthol blue, as well as DNA amplification checker, D-Quick) that were stored for 2 days at different temperatures. Although the time taken to obtain the positive/negative results were delayed, the enzymes and reagents, stored at 25°C for 4 days, were active and had the ability to efficiently amplify DNA in less than 50 min. These results indicate that LAMP assay can be successfully utilized for the diagnosis of infectious diseases under non-clinical settings such as for on-site diagnosis in farms/pastures, owing to the fact that the relevant enzymes and reagents does not require restricted temperature storage.

  11. Chlorpromazine as permeabilizer and reagent for detection of microbial peroxidase and peroxidaselike activities.

    PubMed Central

    Galeazzi, L; Turchetti, G; Grilli, G; Groppa, G; Giunta, S

    1986-01-01

    Chlorpromazine was used to perform a test for the detection of microbial peroxidase activities. The compound acts as both a cell permeabilizer and a reagent in the procedure developed which allows the detection of peroxidase and peroxidase like reactions both semiquantitatively in whole cell determinations and quantitatively in cell-free supernatants. PMID:3539020

  12. Life cycle management of critical ligand-binding reagents.

    PubMed

    O'Hara, Denise M; Theobald, Valerie

    2013-11-01

    Bioanalytical laboratories develop and validate ligand-binding assays (LBA) used to quantify the concentration of analytes of interest in various buffers and relevant biological matrices. The building blocks of LBA are reagents that recognize molecular and structural motifs on ligands, which are combined in various LBA formats to minimize biological matrix interferences and specifically detect and quantify the analyte of interest. The use of these LBA-requiring critical reagents, can span decades as programs mature to commercialization. Since critical reagents are generated mostly from biological systems, attention to their life cycle management, quality, characterization and sustainability are vital to the success of bioanalytical laboratories. Integrating de novo reagent generation, reagent biophysical characterization, LBA development, validation, and use, with reagent resupply processes leverages interdisciplinary activities and ensures smooth operations of a bioanalytical laboratory.

  13. Shelf-stable electrophilic trifluoromethylating reagents: A brief historical perspective

    PubMed Central

    Matsnev, Andrej

    2010-01-01

    Summary Since the discovery by Yagupolskii and co-workers that S-trifluoromethyl diarylsulfonium salts are effective for the trifluoromethylation of thiophenolates, the design and synthesis of electrophilic trifluoromethylating reagents have been extensively researched in both academia and industry, due to the significant unique features that trifluoromethylated compounds have in pharmaceuticals, agricultural chemicals, and functional materials. Several effective reagents have been developed by the groups of Yagupolskii, Umemoto, Shreeve, Adachi, Magnier, Togni and Shibata. Due to the high stability and reactivity of these reagents, a series of Umemoto reagents, Togni reagent and Shibata reagent are now commercially available. In this review, we wish to briefly provide a historical perspective of the development of so-called “shelf-stable electrophilic trifluoromethylating reagents”, although this field is in constant development. PMID:20703379

  14. The Reagent-sorption Technology of Water Treatment

    NASA Astrophysics Data System (ADS)

    Kurchatov, I. M.; Laguntsov, N. I.; Neschimenko, Y. P.; Feklistov, D. Y.

    The main purpose of this work is to intensify and to improve the efficiency of water treatment processes as well as to combine optimally modern techniques and technological devices in water treatment processes. Offered comprehensive hybrid water treatment developing technology of different origin is based on the combination of the treatment by reagent and membrane electro dialysis. In offered technology, of water treatment as a reagent is proposed to use alumino-silicic reagent, which simultaneously is coagulant, flocculant and adsorbent.

  15. 21 CFR 866.3360 - Lymphocytic choriomeningitis virus serological reagents.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents... cerebral meningitis (inflammation of membranes that envelop the brain) and occasionally a mild...

  16. 21 CFR 866.3360 - Lymphocytic choriomeningitis virus serological reagents.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents... cerebral meningitis (inflammation of membranes that envelop the brain) and occasionally a mild...

  17. 21 CFR 866.3360 - Lymphocytic choriomeningitis virus serological reagents.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents... cerebral meningitis (inflammation of membranes that envelop the brain) and occasionally a mild...

  18. 21 CFR 866.3360 - Lymphocytic choriomeningitis virus serological reagents.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents... cerebral meningitis (inflammation of membranes that envelop the brain) and occasionally a mild...

  19. 21 CFR 866.3360 - Lymphocytic choriomeningitis virus serological reagents.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... HUMAN SERVICES (CONTINUED) MEDICAL DEVICES IMMUNOLOGY AND MICROBIOLOGY DEVICES Serological Reagents... cerebral meningitis (inflammation of membranes that envelop the brain) and occasionally a mild...

  20. On-Line Monitoring for Control and Safeguarding of Radiochemical Streams at Spent Fuel Reprocessing Plant

    SciTech Connect

    Bryan, Samuel A.; Levitskaia, Tatiana G.; Casella, Amanda J.; Peterson, James M.; Lines, Amanda M.; Jordan, Elizabeth A.; Verdugo, Dawn E.; Skomurski, Frances N.

    2011-07-19

    There is a renewed interest worldwide to promote the use of nuclear power and close the nuclear fuel cycle. The long term successful use of nuclear power is critically dependent upon adequate and safe processing and disposition of the spent nuclear fuel Liquid-liquid extraction is a separation technique commonly employed for the processing of the dissolved spent nuclear fuel. Our approach is based on prerequisite that real time monitoring of the solvent extraction flowsheets provides unique capability to quickly detect unwanted manipulations with fissile isotopes present in the radiochemical streams during reprocessing activities. The instrumentation used to monitor these processes must be robust, require little or no maintenance, and be able to withstand harsh environments such as high radiation fields and aggressive chemical matrices. In addition, the ability for continuous on-line monitoring allows for numerous benefits. Our team experimentally assessed the potential of Raman and vis-NIR spectrophotometric techniques for on-line real-time monitoring of the U(VI)/nitrate ion/nitric acid and Pu(IV)/Np(V)/Nd(III), respectively, in solutions relevant to spent fuel reprocessing. Both techniques demonstrated robust performance in the repetitive batch measurements of each analyte in a wide concentration range using simulant and commercial dissolved spent fuel solutions. Static spectroscopic measurements served as training sets for the multivariate data analysis to obtain partial least squares predictive models, which were validated using on-line centrifugal contactor extraction tests. The corresponding spectrometers used under the laboratory conditions are easily convertible to the process-friendly configurations allowing remote measurements under the flow conditions. A fiber optic Raman probe allows monitoring of the high concentration species encountered in both aqueous and organic phases within the PUREX suite of flowsheets, including metal oxide ions, such as