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Sample records for titration calorimetry measurements

  1. Isothermal Titration Calorimetry in the Student Laboratory

    Science.gov (United States)

    Wadso, Lars; Li, Yujing; Li, Xi

    2011-01-01

    Isothermal titration calorimetry (ITC) is the measurement of the heat produced by the stepwise addition of one substance to another. It is a common experimental technique, for example, in pharmaceutical science, to measure equilibrium constants and reaction enthalpies. We describe a stirring device and an injection pump that can be used with a…

  2. On the Physical Meaning of the Isothermal Titration Calorimetry Measurements in Calorimeters with Full Cells

    Science.gov (United States)

    Grolier, Jean-Pierre E.; del Río, Jose Manuel

    2009-01-01

    We have performed a detailed study of the thermodynamics of the titration process in an isothermal titration calorimeter with full cells. We show that the relationship between the enthalpy and the heat measured is better described in terms of the equation Δ H = Winj + Q (where Winj is the work necessary to carry out the titration) than in terms of ΔH = Q. Moreover, we show that the heat of interaction between two components is related to the partial enthalpy of interaction at infinite dilution of the titrant component, as well as to its partial volume of interaction at infinite dilution. PMID:20054472

  3. Differential Binding Models for Direct and Reverse Isothermal Titration Calorimetry.

    Science.gov (United States)

    Herrera, Isaac; Winnik, Mitchell A

    2016-03-10

    Isothermal titration calorimetry (ITC) is a technique to measure the stoichiometry and thermodynamics from binding experiments. Identifying an appropriate mathematical model to evaluate titration curves of receptors with multiple sites is challenging, particularly when the stoichiometry or binding mechanism is not available. In a recent theoretical study, we presented a differential binding model (DBM) to study calorimetry titrations independently of the interaction among the binding sites (Herrera, I.; Winnik, M. A. J. Phys. Chem. B 2013, 117, 8659-8672). Here, we build upon our DBM and show its practical application to evaluate calorimetry titrations of receptors with multiple sites independently of the titration direction. Specifically, we present a set of ordinary differential equations (ODEs) with the general form d[S]/dV that can be integrated numerically to calculate the equilibrium concentrations of free and bound species S at every injection step and, subsequently, to evaluate the volume-normalized heat signal (δQ(V) = δq/dV) of direct and reverse calorimetry titrations. Additionally, we identify factors that influence the shape of the titration curve and can be used to optimize the initial concentrations of titrant and analyte. We demonstrate the flexibility of our updated DBM by applying these differentials and a global regression analysis to direct and reverse calorimetric titrations of gadolinium ions with multidentate ligands of increasing denticity, namely, diglycolic acid (DGA), citric acid (CIT), and nitrilotriacetic acid (NTA), and use statistical tests to validate the stoichiometries for the metal-ligand pairs studied.

  4. Isothermal titration calorimetry for drug design: Precision of the enthalpy and binding constant measurements and comparison of the instruments.

    Science.gov (United States)

    Linkuvienė, Vaida; Krainer, Georg; Chen, Wen-Yih; Matulis, Daumantas

    2016-12-15

    Isothermal titration calorimetry (ITC) is one of the most robust label- and immobilization-free techniques used to measure protein - small molecule interactions in drug design for the simultaneous determination of the binding affinity (ΔG) and the enthalpy (ΔH), both of which are important parameters for structure-thermodynamics correlations. It is important to evaluate the precision of the method and of various ITC instrument models by performing a single well-characterized reaction. The binding between carbonic anhydrase II and acetazolamide was measured by four ITC instruments - PEAQ-ITC, iTC200, VP-ITC, and MCS-ITC and the standard deviation of ΔG and ΔH was determined. Furthermore, the limit of an approach to reduce the protein concentration was studied for a high-affinity reaction (K d  = 0.3 nM), too tight to be measured by direct (non-displacement) ITC. Chemical validation of the enthalpy measurements is discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  5. Measurement of Nanomolar Dissociation Constants by Titration Calorimetry and Thermal Shift Assay – Radicicol Binding to Hsp90 and Ethoxzolamide Binding to CAII

    Directory of Open Access Journals (Sweden)

    Vilma Michailovienė

    2009-06-01

    Full Text Available The analysis of tight protein-ligand binding reactions by isothermal titration calorimetry (ITC and thermal shift assay (TSA is presented. The binding of radicicol to the N-terminal domain of human heat shock protein 90 (Hsp90aN and the binding of ethoxzolamide to human carbonic anhydrase (hCAII were too strong to be measured accurately by direct ITC titration and therefore were measured by displacement ITC and by observing the temperature-denaturation transitions of ligand-free and ligand-bound protein. Stabilization of both proteins by their ligands was profound, increasing the melting temperature by more than 10 ºC, depending on ligand concentration. Analysis of the melting temperature dependence on the protein and ligand concentrations yielded dissociation constants equal to 1 nM and 2 nM for Hsp90aN-radicicol and hCAII-ethoxzolamide, respectively. The ligand-free and ligand-bound protein fractions melt separately, and two melting transitions are observed. This phenomenon is especially pronounced when the ligand concentration is equal to about half the protein concentration. The analysis compares ITC and TSA data, accounts for two transitions and yields the ligand binding constant and the parameters of protein stability, including the Gibbs free energy and the enthalpy of unfolding.

  6. Biophysical characterization of antibodies with isothermal titration calorimetry

    Directory of Open Access Journals (Sweden)

    Verna Frasca

    2016-07-01

    Full Text Available Antibodies play a key role in the immune response. Since antibodies bind antigens with high specificity and tight affinity, antibodies are an important reagent in experimental biology, assay development, biomedical research and diagnostics. Monoclonal antibodies are therapeutic drugs and used for vaccine development. Antibody engineering, biophysical characterization, and structural data have provided a deeper understanding of how antibodies function, and how to make better drugs. Isothermal titration calorimetry (ITC is a label-free binding assay, which measures affinity, stoichiometry, and binding thermodynamics for biomolecular interactions. When thermodynamic data are used together with structural and kinetic data from other assays, a complete structure-activity-thermodynamics profile can be constructed. This review article describes ITC, and discusses several applications on how data from ITC provides insights into how antibodies function, guide antibody engineering, and aid design of new therapeutic drugs.

  7. Isothermal Titration Calorimetry Can Provide Critical Thinking Opportunities

    Science.gov (United States)

    Moore, Dale E.; Goode, David R.; Seney, Caryn S.; Boatwright, Jennifer M.

    2016-01-01

    College chemistry faculties might not have considered including isothermal titration calorimetry (ITC) in their majors' curriculum because experimental data from this instrumental method are often analyzed via automation (software). However, the software-based data analysis can be replaced with a spreadsheet-based analysis that is readily…

  8. Integration and global analysis of isothermal titration calorimetry data for studying macromolecular interactions.

    Science.gov (United States)

    Brautigam, Chad A; Zhao, Huaying; Vargas, Carolyn; Keller, Sandro; Schuck, Peter

    2016-05-01

    Isothermal titration calorimetry (ITC) is a powerful and widely used method to measure the energetics of macromolecular interactions by recording a thermogram of differential heating power during a titration. However, traditional ITC analysis is limited by stochastic thermogram noise and by the limited information content of a single titration experiment. Here we present a protocol for bias-free thermogram integration based on automated shape analysis of the injection peaks, followed by combination of isotherms from different calorimetric titration experiments into a global analysis, statistical analysis of binding parameters and graphical presentation of the results. This is performed using the integrated public-domain software packages NITPIC, SEDPHAT and GUSSI. The recently developed low-noise thermogram integration approach and global analysis allow for more precise parameter estimates and more reliable quantification of multisite and multicomponent cooperative and competitive interactions. Titration experiments typically take 1-2.5 h each, and global analysis usually takes 10-20 min.

  9. Thermodynamic investigations of protein's behaviour with ionic liquids in aqueous medium studied by isothermal titration calorimetry.

    Science.gov (United States)

    Bharmoria, Pankaj; Kumar, Arvind

    2016-05-01

    While a number of reports appear on ionic liquids-proteins interactions, their thermodynamic behaviour using suitable technique like isothermal titration calorimetry is not systematically presented. Isothermal titration calorimetry (ITC) is a key technique which can directly measure the thermodynamic contribution of IL binding to protein, particularly the enthalpy, heat capacities and binding stoichiometry. Ionic liquids (ILs), owing to their unique and tunable physicochemical properties have been the central area of scientific research besides graphene in the last decade, and growing unabated. Their encounter with proteins in the biological system is inevitable considering their environmental discharge though most of them are recyclable for a number of cycles. In this article we will cover the thermodynamics of proteins upon interaction with ILs as osmolyte and surfactant. The up to date literature survey of IL-protein interactions using isothermal titration calorimetry will be discussed and parallel comparison with the results obtained for such studies with other techniques will be highlighted to demonstrate the accuracy of ITC technique. Net stability of proteins can be obtained from the difference in the free energy (ΔG) of the native (folded) and denatured (unfolded) state using the Gibbs-Helmholtz equation (ΔG=ΔH-TΔS). Isothermal titration calorimetry can directly measure the heat changes upon IL-protein interactions. Calculation of other thermodynamic parameters such as entropy, binding constant and free energy depends upon the proper fitting of the binding isotherms using various fitting models. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Enzyme-catalyzed and binding reaction kinetics determined by titration calorimetry.

    Science.gov (United States)

    Hansen, Lee D; Transtrum, Mark K; Quinn, Colette; Demarse, Neil

    2016-05-01

    Isothermal calorimetry allows monitoring of reaction rates via direct measurement of the rate of heat produced by the reaction. Calorimetry is one of very few techniques that can be used to measure rates without taking a derivative of the primary data. Because heat is a universal indicator of chemical reactions, calorimetry can be used to measure kinetics in opaque solutions, suspensions, and multiple phase systems and does not require chemical labeling. The only significant limitation of calorimetry for kinetic measurements is that the time constant of the reaction must be greater than the time constant of the calorimeter which can range from a few seconds to a few minutes. Calorimetry has the unique ability to provide both kinetic and thermodynamic data. This article describes the calorimetric methodology for determining reaction kinetics and reviews examples from recent literature that demonstrate applications of titration calorimetry to determine kinetics of enzyme-catalyzed and ligand binding reactions. A complete model for the temperature dependence of enzyme activity is presented. A previous method commonly used for blank corrections in determinations of equilibrium constants and enthalpy changes for binding reactions is shown to be subject to significant systematic error. Methods for determination of the kinetics of enzyme-catalyzed reactions and for simultaneous determination of thermodynamics and kinetics of ligand binding reactions are reviewed. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Synthesis of a ruthenium(II) bipyridyl complex coordinated by a functionalized Schiff base ligand: characterization, spectroscopic and isothermal titration calorimetry measurements of M2+ binding and sensing (M2+=Ca2+, Mg2+).

    Science.gov (United States)

    Dixit, Namrata; Mishra, Lallan; Mustafi, Sourajit M; Chary, Kandala V R; Houjou, Hirohiko

    2009-07-01

    Bis-[methylsalicylidine-4'benzoic acid]-ethylene (LH2) complexed with cis-Ru(bpy)2Cl(2).2H2O provides a complex of composition [Ru(bpy)2L].2NH4PF6 (1), which has been characterized spectroscopically. Its binding behaviour towards Mg2+ and Ca2+ ions is monitored using 1H NMR titration, isothermal titration calorimetry (ITC) and luminescence microscopy. The luminescent ruthenium complex binds Ca2+ in a more selective manner as compared to Mg2+.

  12. Determination of the aggregation number for micelles by isothermal titration calorimetry

    DEFF Research Database (Denmark)

    Olesen, Niels Erik; Holm, Rene; Westh, Peter

    2014-01-01

    Isothermal titration calorimetry (ITC) has previously been applied to estimate the aggregation number (n), Gibbs free energy (ΔG), enthalpy (ΔH) and entropy (ΔS) of micellization. However, some difficulties of micelle characterization by ITC still remain; most micelles have aggregation numbers...... insight into optimal design of titration protocols for micelle characterization. By applying the new method, the aggregation number of sodium dodecyl sulphate and glycochenodeoxycholate was determined at concentrations around their critical micelle concentration (CMC)...

  13. Efficient Isothermal Titration Calorimetry Technique Identifies Direct Interaction of Small Molecule Inhibitors with the Target Protein.

    Science.gov (United States)

    Gal, Maayan; Bloch, Itai; Shechter, Nelia; Romanenko, Olga; Shir, Ofer M

    2016-01-01

    Protein-protein interactions (PPI) play a critical role in regulating many cellular processes. Finding novel PPI inhibitors that interfere with specific binding of two proteins is considered a great challenge, mainly due to the complexity involved in characterizing multi-molecular systems and limited understanding of the physical principles governing PPIs. Here we show that the combination of virtual screening techniques, which are capable of filtering a large library of potential small molecule inhibitors, and a unique secondary screening by isothermal titration calorimetry, a label-free method capable of observing direct interactions, is an efficient tool for finding such an inhibitor. In this study we applied this strategy in a search for a small molecule capable of interfering with the interaction of the tumor-suppressor p53 and the E3-ligase MDM2. We virtually screened a library of 15 million small molecules that were filtered to a final set of 80 virtual hits. Our in vitro experimental assay, designed to validate the activity of mixtures of compounds by isothermal titration calorimetry, was used to identify an active molecule against MDM2. At the end of the process the small molecule (4S,7R)-4-(4-chlorophenyl)-5-hydroxy-2,7-dimethyl-N-(6-methylpyridin-2-yl)-4,6,7,8 tetrahydrIoquinoline-3-carboxamide was found to bind MDM2 with a dissociation constant of ~2 µM. Following the identification of this single bioactive compound, spectroscopic measurements were used to further characterize the interaction of the small molecule with the target protein. 2D NMR spectroscopy was used to map the binding region of the small molecule, and fluorescence polarization measurement confirmed that it indeed competes with p53.

  14. Isothermal Titration Calorimetry and Macromolecular Visualization for the Interaction of Lysozyme and Its Inhibitors

    Science.gov (United States)

    Wei, Chin-Chuan; Jensen, Drake; Boyle, Tiffany; O'Brien, Leah C.; De Meo, Cristina; Shabestary, Nahid; Eder, Douglas J.

    2015-01-01

    To provide a research-like experience to upper-division undergraduate students in a biochemistry teaching laboratory, isothermal titration calorimetry (ITC) is employed to determine the binding constants of lysozyme and its inhibitors, N-acetyl glucosamine trimer (NAG[subscript 3]) and monomer (NAG). The extremely weak binding of lysozyme/NAG is…

  15. Thermodynamic profiling of Peptide membrane interactions by isothermal titration calorimetry: a search for pores and micelles

    DEFF Research Database (Denmark)

    Henriksen, Jonas Rosager; Andresen, Thomas Lars

    2011-01-01

    in mixed peptide-lipid micelles. We have investigated the mode of action of the antimicrobial peptide mastoparan-X using isothermal titration calorimetry (ITC) and cryo-transmission electron microscopy (cryo-TEM). The results show that mastoparan-X induces a range of structural transitions of POPC/POPG (3...

  16. Subsite binding energies of an exo-polygalacturonase using isothermal titration calorimetry

    Science.gov (United States)

    Thermodynamic parameters for binding of a series of galacturonic acid oligomers to an exo-polygalacturonase, RPG16 from Rhizopus oryzae, were determined by isothermal titration calorimetry. Binding of oligomers varying in chain length from two to five galacturonic acid residues is an exothermic proc...

  17. Interaction between Humic Acid and Lysozyme, Studied by Dynamic Light Scattering and Isothermal Titration Calorimetry

    NARCIS (Netherlands)

    Tan, Wen Feng; Koopal, Luuk K.; Norde, Willem

    2009-01-01

    Interactions of purified Aldrich humic acid (PAHA) with the protein lysozyme (LSZ) are studied with dynamic light scattering and isothermal titration calorimetry by mixing LSZ and PAHA at various mass ratios. In solution LSZ is positive and PAHA is negative at the investigated pH values. Up to

  18. Heat of supersaturation-limited amyloid burst directly monitored by isothermal titration calorimetry.

    Science.gov (United States)

    Ikenoue, Tatsuya; Lee, Young-Ho; Kardos, József; Yagi, Hisashi; Ikegami, Takahisa; Naiki, Hironobu; Goto, Yuji

    2014-05-06

    Amyloid fibrils form in supersaturated solutions via a nucleation and growth mechanism. Although the structural features of amyloid fibrils have become increasingly clearer, knowledge on the thermodynamics of fibrillation is limited. Furthermore, protein aggregation is not a target of calorimetry, one of the most powerful approaches used to study proteins. Here, with β2-microglobulin, a protein responsible for dialysis-related amyloidosis, we show direct heat measurements of the formation of amyloid fibrils using isothermal titration calorimetry (ITC). The spontaneous fibrillation after a lag phase was accompanied by exothermic heat. The thermodynamic parameters of fibrillation obtained under various protein concentrations and temperatures were consistent with the main-chain dominated structural model of fibrils, in which overall packing was less than that of the native structures. We also characterized the thermodynamics of amorphous aggregation, enabling the comparison of protein folding, amyloid fibrillation, and amorphous aggregation. These results indicate that ITC will become a promising approach for clarifying comprehensively the thermodynamics of protein folding and misfolding.

  19. A survey of the year 2007 literature on applications of isothermal titration calorimetry

    OpenAIRE

    Bjelic, S; Jelesarov, I

    2008-01-01

    Elucidation of the energetic principles of binding affinity and specificity is a central task in many branches of current sciences: biology, medicine, pharmacology, chemistry, material sciences, etc. In biomedical research, integral approaches combining structural information with in-solution biophysical data have proved to be a powerful way toward understanding the physical basis of vital cellular phenomena. Isothermal titration calorimetry (ITC) is a valuable experimental tool facilitating ...

  20. Monitoring of an RNA Multistep Folding Pathway by Isothermal Titration Calorimetry

    OpenAIRE

    Reymond, Cédric; Bisaillon, Martin; Perreault, Jean-Pierre

    2009-01-01

    Isothermal titration calorimetry was used to monitor the energetic landscape of a catalytic RNA, specifically that of the hepatitis delta virus ribozyme. Using mutants that isolated various tertiary interactions, the thermodynamic parameters of several ribozyme-substrate intermediates were determined. The results shed light on the impact of several tertiary interactions on the global structure of the ribozyme. In addition, the data indicate that the formation of the P1.1 pseudoknot is the lim...

  1. Interaction of diethyl aniline methylphosphonate with DNA: Spectroscopic and isothermal titration calorimetry

    International Nuclear Information System (INIS)

    Lu Yan; Xu Meihua; Wang Gongke; Zheng Yun

    2011-01-01

    In this study the diethyl aniline methylphosphonate (DAM) was synthesized, the interaction of DAM with ct-DNA has been investigated by fluorescence spectra, UV spectra, molecular modeling and isothermal titration calorimetry (ITC). The binding constant of DAM to ct-DNA calculated from both isothermal titration calorimetry and fluorescence spectra were found to be in the 10 4 M -1 range. According to the ethidium bromide displacement studies, UV spectra and isothermal titration calorimetry experimental results, it can be concluded that DAM is an intercalator that can slide into the G-C rich region of ct-DNA. Furthermore, the results obtained from molecular modeling corroborated the experimental results obtanied from spectroscopic and ITC investigations. At the same time, fluorescence spectra suggested that the mechanism of the interaction of DAM to ct-DNA was a static enhancing type. ITC data showed that ct-DNA/DAM binding is enthalpy controlled. - Research highlights: → The interaction of DAM with ct-DNA is a static enhancing type. → DAM can slide into the G-C rich region of ct-DNA. → The binding of DAM to ct-DNA is enthalpy controlled. → The hydrogen bonding forces play an essential role in the binding process.

  2. Uptake and release protocol for assessing membrane binding and permeation by way of isothermal titration calorimetry.

    Science.gov (United States)

    Tsamaloukas, Alekos D; Keller, Sandro; Heerklotz, Heiko

    2007-01-01

    The activity of many biomolecules and drugs crucially depends on whether they bind to biological membranes and whether they translocate to the opposite lipid leaflet and trans aqueous compartment. A general strategy to measure membrane binding and permeation is the uptake and release assay, which compares two apparent equilibrium situations established either by the addition or by the extraction of the solute of interest. Only solutes that permeate the membrane sufficiently fast do not show any dependence on the history of sample preparation. This strategy can be pursued for virtually all membrane-binding solutes, using any method suitable for detecting binding. Here, we present in detail one example that is particularly well developed, namely the nonspecific membrane partitioning and flip-flop of small, nonionic solutes as characterized by isothermal titration calorimetry. A complete set of experiments, including all sample preparation procedures, can typically be accomplished within 2 days. Analogous protocols for studying charged solutes, virtually water-insoluble, hydrophobic compounds or specific ligands are also considered.

  3. Single-experiment displacement assay for quantifying high-affinity binding by isothermal titration calorimetry.

    Science.gov (United States)

    Krainer, Georg; Keller, Sandro

    2015-04-01

    Isothermal titration calorimetry (ITC) is the gold standard for dissecting the thermodynamics of a biomolecular binding process within a single experiment. However, reliable determination of the dissociation constant (KD) from a single titration is typically limited to the range 100 μM>KD>1 nM. Interactions characterized by a lower KD can be assessed indirectly by so-called competition or displacement assays, provided that a suitable competitive ligand is available whose KD falls within the directly accessible window. However, this protocol is limited by the fact that it necessitates at least two titrations to characterize one high-affinity inhibitor, resulting in considerable consumption of both sample material and time. Here, we introduce a fast and efficient ITC displacement assay that allows for the simultaneous characterization of both a high-affinity ligand and a moderate-affinity ligand competing for the same binding site on a receptor within a single experiment. The protocol is based on a titration of the high-affinity ligand into a solution containing the moderate-affinity ligand bound to the receptor present in excess. The resulting biphasic binding isotherm enables accurate and precise determination of KD values and binding enthalpies (ΔH) of both ligands. We discuss the theoretical background underlying the approach, demonstrate its practical application to metal ion chelation, explore its potential and limitations with the aid of simulations and statistical analyses, and elaborate on potential applications to protein-inhibitor interactions. Copyright © 2014 Elsevier Inc. All rights reserved.

  4. Binding of Cu(II) ions to peptides studied by fluorescence spectroscopy and isothermal titration calorimetry

    Science.gov (United States)

    Makowska, Joanna; Żamojć, Krzysztof; Wyrzykowski, Dariusz; Uber, Dorota; Wierzbicka, Małgorzata; Wiczk, Wiesław; Chmurzyński, Lech

    2016-01-01

    Steady-state and time-resolved fluorescence quenching measurements supported by Isothermal Titration Calorimetry (ITC) were used to study the interactions of Cu2 + with four peptides. Two of them were taken from the N-terminal part of the FBP28 protein (formin binding protein) WW domain: Tyr-Lys-Thr-Ala-Asp-Gly-Lys-Thr-Tyr-NH2 (D9) and its mutant Tyr-Lys-Thr-Ala-Asn-Gly-Lys-Thr-Tyr-NH2 (D9_M) as well as two mutated peptides from the B3 domain of the immunoglobulin binding protein G derived from Streptococcus: Asp-Val-Ala-Thr-Tyr-Thr-NH2 (J1) and Glu-Val-Ala-Thr-Tyr-Thr-NH2 (J2). The measurements were carried out at 298.15 K in 20 mM 2-(N-morpholino)ethanesulfonic acid (MES) buffer solution with a pH of 6. The fluorescence of all peptides was quenched by Cu2 + ions. The stoichiometry, conditional stability constants and thermodynamic parameters for the interactions of the Cu2 + ions with D9 and D9_M were determined from the calorimetric data. The values of the conditional stability constants were additionally determined from fluorescence quenching measurements and compared with those obtained from calorimetric studies. There was a good correlation between data obtained from the two techniques. On the other hand, the studies revealed that J1 and J2 do not exhibit an affinity towards metal ions. The obtained results prove that fluorescence quenching experiments may be successfully used in order to determine stability constants of complexes with fluorescent ligands. Finally, based on the obtained results, the coordinating properties of the peptides towards the Cu2 + ions are discussed.

  5. Isothermal titration calorimetry uncovers substrate promiscuity of bicupin oxalate oxidase from Ceriporiopsis subvermispora

    Directory of Open Access Journals (Sweden)

    Hassan Rana

    2016-03-01

    Full Text Available Isothermal titration calorimetry (ITC may be used to determine the kinetic parameters of enzyme-catalyzed reactions when neither products nor reactants are spectrophotometrically visible and when the reaction products are unknown. We report here the use of the multiple injection method of ITC to characterize the catalytic properties of oxalate oxidase (OxOx from Ceriporiopsis subvermispora (CsOxOx, a manganese dependent enzyme that catalyzes the oxygen-dependent oxidation of oxalate to carbon dioxide in a reaction coupled with the formation of hydrogen peroxide. CsOxOx is the first bicupin enzyme identified that catalyzes this reaction. The multiple injection ITC method of measuring OxOx activity involves continuous, real-time detection of the amount of heat generated (dQ during catalysis, which is equal to the number of moles of product produced times the enthalpy of the reaction (ΔHapp. Steady-state kinetic constants using oxalate as the substrate determined by multiple injection ITC are comparable to those obtained by a continuous spectrophotometric assay in which H2O2 production is coupled to the horseradish peroxidase-catalyzed oxidation of 2,2′-azinobis-(3-ethylbenzthiazoline-6-sulfonic acid and by membrane inlet mass spectrometry. Additionally, we used multiple injection ITC to identify mesoxalate as a substrate for the CsOxOx-catalyzed reaction, with a kinetic parameters comparable to that of oxalate, and to identify a number of small molecule carboxylic acid compounds that also serve as substrates for the enzyme.

  6. Titration calorimetry of surfactant–drug interactions: Micelle formation and saturation studies

    International Nuclear Information System (INIS)

    Waters, Laura J.; Hussain, Talib; Parkes, Gareth M.B.

    2012-01-01

    Highlights: ► Isothermal titration calorimetry can be used to monitor the saturation of micelles with pharmaceutical compounds. ► The number of drug molecules per micelle varies depending on the drug used and the temperature of the calorimeter. ► The change in enthalpy for the saturation of micelles with drugs can be endothermic or exothermic. ► The critical micellar concentration of an anionic surfactant (SDS) does not appear to vary in the presence of drugs. - Abstract: Isothermal titration calorimetry (ITC) was employed to monitor the addition of five model drugs to anionic surfactant based micelles, composed of sodium dodecyl sulfate (SDS), through to the point at which they were saturated with drug. Analysis of the resultant data using this newly developed method has confirmed the suitability of the technique to acquire such data with saturation limits established in all cases. Values for the point at which saturation occurred ranged from 17 molecules of theophylline per micelle at T = 298 K up to 63 molecules of caffeine per micelle at 310 K. Micellar systems can be disrupted by the presence of additional chemicals, such as the drugs used in this study, therefore a separate investigation was undertaken to determine the critical micellar concentration (CMC) for SDS in the presence of each drug at T = 298 K and 310 K using ITC. In the majority of cases, there was no appreciable alteration to the CMC of SDS with drug present.

  7. Combined use of titration calorimetry and spectrofluorimetry for the screening of the acidity of solid catalysts in different liquids

    International Nuclear Information System (INIS)

    Gervasini, Antonella; Auroux, Aline

    2013-01-01

    Graphical abstract: Measurements of acidity of oxides of catalytic importance in various liquids open the possibility to know their effective acidity, which is related with their activity in liquid-heterogeneous catalysis. Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. - Highlights: • Measurements of acidity of oxides of catalytic importance in various liquids. • Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. • Effective acidities are expressed by given sample in various liquids. • Nb-containing samples are able to maintain acidity in protic liquids. - Abstract: The effective acid and base surface properties of selected acidic and basic samples of catalytic interest (alumina, titania, zirconia, silica–alumina, niobium oxide, niobium phosphate, boron nitride, and hydrotalcite) were measured by titration with basic and acidic molecular probes (aniline, 2-phenylethylamine, and phenol) in various liquids (cyclohexane, 1,4-dioxane, isopropanol, n-decane, and toluene) with different polar and protic characteristics. The combined use of a reaction calorimeter and a spectrofluorimeter has been performed. The set-up of the coupled technique and the most interesting results are shown here. The study confirmed that the acid–base properties of solids are deeply affected by the nature and properties of the liquid surrounding the samples. Few oxides are able to maintain their surface acidity in highly polar and protic solvents, in particular whose containing niobium. In general, the solvating and coordinative ability of the most polar and protic liquids caused remarkable loss of acidity/basicity of the oxide surfaces

  8. Combined use of titration calorimetry and spectrofluorimetry for the screening of the acidity of solid catalysts in different liquids

    Energy Technology Data Exchange (ETDEWEB)

    Gervasini, Antonella, E-mail: antonella.gervasini@unimi.it [Dipartimento di Chimica, Università degli Studi di Milano, via Camillo Golgi, 19, 20133 Milano (Italy); Auroux, Aline, E-mail: aline.auroux@ircelyon.univ-lyon1.fr [Université Lyon 1, CNRS, UMR 5256, Institut de Recherches sur la Catalyse et l‘Environnement de Lyon (IRCELYON), 2 Avenue A. Einstein, 69626 Villeurbanne (France)

    2013-09-10

    Graphical abstract: Measurements of acidity of oxides of catalytic importance in various liquids open the possibility to know their effective acidity, which is related with their activity in liquid-heterogeneous catalysis. Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. - Highlights: • Measurements of acidity of oxides of catalytic importance in various liquids. • Titration-calorimetry alone or in connection with spectrofluorimetry is efficient for this scope. • Effective acidities are expressed by given sample in various liquids. • Nb-containing samples are able to maintain acidity in protic liquids. - Abstract: The effective acid and base surface properties of selected acidic and basic samples of catalytic interest (alumina, titania, zirconia, silica–alumina, niobium oxide, niobium phosphate, boron nitride, and hydrotalcite) were measured by titration with basic and acidic molecular probes (aniline, 2-phenylethylamine, and phenol) in various liquids (cyclohexane, 1,4-dioxane, isopropanol, n-decane, and toluene) with different polar and protic characteristics. The combined use of a reaction calorimeter and a spectrofluorimeter has been performed. The set-up of the coupled technique and the most interesting results are shown here. The study confirmed that the acid–base properties of solids are deeply affected by the nature and properties of the liquid surrounding the samples. Few oxides are able to maintain their surface acidity in highly polar and protic solvents, in particular whose containing niobium. In general, the solvating and coordinative ability of the most polar and protic liquids caused remarkable loss of acidity/basicity of the oxide surfaces.

  9. Automated back titration method to measure phosphate

    International Nuclear Information System (INIS)

    Comer, J.; Tehrani, M.; Avdeef, A.; Ross, J. Jr.

    1987-01-01

    Phosphate was measured in soda drinks and as an additive in flour, by a back titration method in which phosphate was precipitated with lanthanum, and the excess lanthanum was titrated with fluoride. All measurements were performed using the Orion fluoride electrode and the Orion 960 Autochemistry System. In most commercial automatic titrators, the inflection point of the titration curve, calculated from the first derivative of the curve, is used to find the equivalence polar of the titration. The inflection technique is compared with a technique based on Gran functions, which uses data collected after the end point and predicts the equivalence point accordingly

  10. Titration of fatty acids solubilized in cationic and anionic micelles. Calorimetry and thermodynamic modeling.

    Science.gov (United States)

    Söderman, Olle; Jönsson, Bengt; Olofsson, Gerd

    2006-02-23

    The electrostatic properties of charged surfactant micelles are investigated through titrations of fatty acid probes solubilized in the micelles. The titration process is followed by means of calorimetric measurements and by determining the pH values as a function of added base. This approach yields a complete thermodynamic description of the titration process. In particular, we find that the process is endothermic at 298 K. This is contrary to the titration of carboxylic acids in water, where DeltaH is approximately 0. To identify the main effect underlying the difference in DeltaH between titration in a micelle and water, a thermodynamic model has been developed which focuses on the transfer properties of charged and uncharged species from bulk water to the surface of a micelle and which incorporates a dielectric discontinuity at the micellar surface. The model relies on the use of the Poisson-Boltzmann equation which is solved using a finite element method. Experimental results and the model calculations imply that the dielectric discontinuity at (or near) the micellar surface plays a major role and hence must be included when analyzing the titration behavior of an acid functionality at the surface of a charged micelle.

  11. Use of isothermal titration calorimetry to study the interaction of short-chain alcohols with lipid membranes

    DEFF Research Database (Denmark)

    Trandum, Christa; Westh-Andersen, Peter; Jørgensen, Kent

    1999-01-01

    of short-chain alcohols on Lipid bilayers. isothermal titration calorimetry (ITC) has been used to determine the energy involved in the association of the alcohols with lipid bilayers. Pure unilamellar DMPC liposomes and DMPC liposomes incorporated with different amounts of cholesterol, sphingomyelin...... dependent on the lipid bilayer composition. In the presence of high concentrations of cholesterol, the binding enthalpy of ethanol is decreased, whereas the presence of ceramides enhances the enthalpic response of the lipid bilayer to ethanol. Isothermal titration calorimetry offers a new methodology...

  12. Isothermal titration calorimetry and surface plasmon resonance allow quantifying substrate binding to different binding sites of Bacillus subtilis xylanase

    DEFF Research Database (Denmark)

    Cuyvers, Sven; Dornez, Emmie; Abou Hachem, Maher

    2012-01-01

    Isothermal titration calorimetry and surface plasmon resonance were tested for their ability to study substrate binding to the active site (AS) and to the secondary binding site (SBS) of Bacillus subtilis xylanase A separately. To this end, three enzyme variants were compared. The first was a cat......Isothermal titration calorimetry and surface plasmon resonance were tested for their ability to study substrate binding to the active site (AS) and to the secondary binding site (SBS) of Bacillus subtilis xylanase A separately. To this end, three enzyme variants were compared. The first...

  13. Ln(III)-malate complexation studies using TRLFS and micro titration calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Taube, F.; Drobot, B. [Technische Univ. Dresden (Germany). Professorship Radiochemistry; Acker, M.; Taut, S. [Technische Univ. Dresden (Germany). Central Radionuclide Laboratory; Stumpf, Thorsten [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Inst. of Resource Ecology

    2017-06-01

    The complexation of trivalent lanthanides was studied using Time-Resolved Laser-Induced Fluorescence Spectroscopy (TRLFS) and Isothermal Titration Calorimetry (ITC). Formation constants, complexation enthalpies and fluorescence lifetimes are determined over a wide pH range at I = 0.5 m NaCl. This subject has the following background: Concrete is widely used as engineering barrier and for waste conditioning in waste repositories. Its binding agent is cement. Organic cement additives, which are used to improve the workability of fresh concrete, are complexation agents for radionuclides after they have been released during the concretes degradation. Thus, these additives might have an impact on the aqueous geochemistry of actinides. Here, the α-hydroxydicarboxylic acid or malic acid is examined. It is used in water-reducers or retarders in cement.

  14. The use of isothermal titration calorimetry to assess the solubility enhancement of simvastatin by a range of surfactants

    International Nuclear Information System (INIS)

    Patel, Rajesh; Buckton, Graham; Gaisford, Simon

    2007-01-01

    Surfactants are commonly used to increase the solubility of poorly water soluble drugs but the interactions between drug and surfactant can be complex and quantitative relationships can be hard to derive. One approach is to quantify the thermodynamics of interaction and relate these parameters to known solubility or dissolution rate enhancement data. Isothermal titration calorimetry (ITC) was used to measure the enthalpy and free energy of transfer of a model drug (simvastatin) to a number of surfactant (SDS, HTAB, SDCH and Brij 35) micelles. These data were then compared with the solubility enhancements determined for each surfactant using HPLC assays. As expected, there was correlation between the free energy of transfer for the drug to each surfactant and the solubility enhancement of that surfactant. Although the data set is limited, the results suggest that ITC screening of a range of surfactants against a poorly water soluble drug may allow the selection of the best potential solubilising surfactants

  15. Kinetic properties of two Rhizopus exo-polygalacturonase enzymes hydrolyzing galacturonic acid oligomers using isothermal titration calorimetry

    Science.gov (United States)

    The kinetic characteristics of two Rhizopus oryzae exo-polygalacturonases acting on galacturonic acid oligomers (GalpA) were determined using isothermal titration calorimetry (ITC). RPG15 hydrolyzing (GalpA)2 demonstrated a Km of 55 uM and kcat of 10.3 s^-1^ while RPG16 was shown to have greater af...

  16. Determination of thermodynamic potentials and the aggregation number for micelles with the mass-action model by isothermal titration calorimetry

    DEFF Research Database (Denmark)

    Olesen, Niels Erik; Westh, Peter; Holm, René

    2015-01-01

    The aggregation number (n), thermodynamic potentials (ΔG, ΔH, ΔS) and critical micelle concentration (CMC) for 6 natural bile salts were determined on the basis of both original and previously published isothermal titration calorimetry (ITC) data. Different procedures to estimate parameters...

  17. Quantifying high-affinity binding of hydrophobic ligands by isothermal titration calorimetry.

    Science.gov (United States)

    Krainer, Georg; Broecker, Jana; Vargas, Carolyn; Fanghänel, Jörg; Keller, Sandro

    2012-12-18

    A fast and reliable quantification of the binding thermodynamics of hydrophobic high-affinity ligands employing a new calorimetric competition experiment is described. Although isothermal titration calorimetry is the method of choice for a quantitative characterization of intermolecular interactions in solution, a reliable determination of a dissociation constant (K(D)) is typically limited to the range 100 μM > K(D) > 1 nM. Interactions displaying higher or lower K(D) values can be assessed indirectly, provided that a suitable competing ligand is available whose K(D) falls within the directly accessible affinity window. This established displacement assay, however, requires the high-affinity ligand to be soluble at high concentrations in aqueous buffer and, consequently, poses serious problems in the study of protein binding involving small-molecule ligands dissolved in organic solvents--a familiar case in many drug-discovery projects relying on compound libraries. The calorimetric competition assay introduced here overcomes this limitation, thus allowing for a detailed thermodynamic description of high-affinity receptor-ligand interactions involving poorly water-soluble compounds. Based on a single titration of receptor into a dilute mixture of the two competing ligands, this competition assay provides accurate and precise values for the dissociation constants and binding enthalpies of both high- and moderate-affinity ligands. We discuss the theoretical background underlying the approach, demonstrate its practical application to metal ion chelation and high-affinity protein-inhibitor interactions, and explore its potential and limitations with the aid of simulations and statistical analyses.

  18. Phosphate sorption by three potential filter materials as assessed by isothermal titration calorimetry.

    Science.gov (United States)

    Lyngsie, Gry; Penn, Chad J; Hansen, Hans C B; Borggaard, Ole K

    2014-10-01

    Phosphorus eutrophication of lakes and streams, coming from drained farmlands, is a serious problem in areas with intensive agriculture. Installation of phosphate (P) sorbing filters at drain outlets may be a solution. The aim of this study was to improve the understanding of reactions involved in P sorption by three commercial P sorbing materials, i.e. Ca/Mg oxide-based Filtralite-P, Fe oxide-based CFH-12 and Limestone in two particle sizes (2-1 mm and 1-0.5 mm), by means of isothermal titration calorimetry (ITC), sorption isotherms, sequential extractions and SEM-EDS. The results indicate that P retention by CFH is due to surface complexation by rapid formation of strong Fe-P bonds. In contrast, retention of P by Filtralite-P and Limestone strongly depends on pH and time and is interpreted due to formation of calcium phosphate precipitate(s). Consequently, CFH can unambiguously be recommended as P retention filter material in drain outlets, whereas the use of Filtralite-P and Limestone has certain (serious) limitations. Thus, Filtralite-P has high capacity to retain P but only at alkaline pH (pH ≥ 10) and P retention by Limestone requires long-time contact and a high ratio between sorbent and sorbate. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. A survey of the year 2007 literature on applications of isothermal titration calorimetry.

    Science.gov (United States)

    Bjelić, Sasa; Jelesarov, Ilian

    2008-01-01

    Elucidation of the energetic principles of binding affinity and specificity is a central task in many branches of current sciences: biology, medicine, pharmacology, chemistry, material sciences, etc. In biomedical research, integral approaches combining structural information with in-solution biophysical data have proved to be a powerful way toward understanding the physical basis of vital cellular phenomena. Isothermal titration calorimetry (ITC) is a valuable experimental tool facilitating quantification of the thermodynamic parameters that characterize recognition processes involving biomacromolecules. The method provides access to all relevant thermodynamic information by performing a few experiments. In particular, ITC experiments allow to by-pass tedious and (rarely precise) procedures aimed at determining the changes in enthalpy and entropy upon binding by van't Hoff analysis. Notwithstanding limitations, ITC has now the reputation of being the "gold standard" and ITC data are widely used to validate theoretical predictions of thermodynamic parameters, as well as to benchmark the results of novel binding assays. In this paper, we discuss several publications from 2007 reporting ITC results. The focus is on applications in biologically oriented fields. We do not intend a comprehensive coverage of all newly accumulated information. Rather, we emphasize work which has captured our attention with originality and far-reaching analysis, or else has provided ideas for expanding the potential of the method. Copyright (c) 2008 John Wiley & Sons, Ltd.

  20. A Universal Method for Fishing Target Proteins from Mixtures of Biomolecules using Isothermal Titration Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, X.; Sun, Q; Kini, R; Sivaraman, J

    2008-01-01

    The most challenging tasks in biology include the identification of (1) the orphan receptor for a ligand, (2) the ligand for an orphan receptor protein, and (3) the target protein(s) for a given drug or a lead compound that are critical for the pharmacological or side effects. At present, several approaches are available, including cell- or animal-based assays, affinity labeling, solid-phase binding assays, surface plasmon resonance, and nuclear magnetic resonance. Most of these techniques are not easy to apply when the target protein is unknown and the compound is not amenable to labeling, chemical modification, or immobilization. Here we demonstrate a new universal method for fishing orphan target proteins from a complex mixture of biomolecules using isothermal titration calorimetry (ITC) as a tracking tool. We took snake venom, a crude mixture of several hundred proteins/peptides, as a model to demonstrate our proposed ITC method in tracking the isolation and purification of two distinct target proteins, a major component and a minor component. Identities of fished out target proteins were confirmed by amino acid sequencing and inhibition assays. This method has the potential to make a significant advancement in the area of identifying orphan target proteins and inhibitor screening in drug discovery and characterization.

  1. Subsite binding energies of an exo-polygalacturonase using isothermal titration calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Mertens, Jeffrey A., E-mail: Jeffrey.Mertens@ars.usda.gov [Bioenergy Research Unit, National Center for Agricultural Utilization Research, Agricultural Research Service, U.S. Department of Agriculture, 1815 North University Street, Peoria, IL 61604 (United States); Hector, Ronald E.; Bowman, Michael J. [Bioenergy Research Unit, National Center for Agricultural Utilization Research, Agricultural Research Service, U.S. Department of Agriculture, 1815 North University Street, Peoria, IL 61604 (United States)

    2012-01-10

    Highlights: Black-Right-Pointing-Pointer Thermodynamics of (GalpA){sub n} oligomers binding to an exo-polygalacturonase. Black-Right-Pointing-Pointer Energetics of binding (GalpA){sub n} were determined by ITC. Black-Right-Pointing-Pointer Thermodynamic parameters attributable to individual subsites were determined. - Abstract: Thermodynamic parameters for binding of a series of galacturonic acid oligomers to an exo-polygalacturonase, RPG16 from Rhizopus oryzae, were determined by isothermal titration calorimetry. Binding of oligomers varying in chain length from two to five galacturonic acid residues is an exothermic process that is enthalpically driven and results in extremely tight binding of the substrate to RPG16. Binding energies in combination with prior biochemical data suggests that RPG16 has the potential for five subsites, -1 to +4, with the greatest contribution to binding energies arising from subsite -1/+1. While the enthalpic contribution to binding decreases substantially for subsites +2 to +4, beneficial entropic effects occur in subsites +3 and +4 leading to increased total free energy as the length of oligomer increases. This information will be useful for additional studies in determining the binding contributions of specific amino acids with mutant enzymes.

  2. Misuse of thermodynamics in the interpretation of isothermal titration calorimetry data for ligand binding to proteins.

    Science.gov (United States)

    Pethica, Brian A

    2015-03-01

    Isothermal titration calorimetry (ITC) has given a mass of data on the binding of small molecules to proteins and other biopolymers, with particular interest in drug binding to proteins chosen as therapeutic indicators. Interpretation of the enthalpy data usually follows an unsound protocol that uses thermodynamic relations in circumstances where they do not apply. Errors of interpretation include incomplete definitions of ligand binding and equilibrium constants and neglect of the non-ideality of the solutions under study, leading to unreliable estimates of standard free energies and entropies of binding. The mass of reported thermodynamic functions for ligand binding to proteins estimated from ITC enthalpies alone is consequently of uncertain thermodynamic significance and utility. ITC and related experiments to test the protocol assumptions are indicated. A thermodynamic procedure avoiding equilibrium constants or other reaction models and not requiring protein activities is given. The discussion draws attention to the fundamental but neglected relation between the thermodynamic activity and bioactivity of drugs and to the generally unknown thermodynamic status of ligand solutions, which for drugs relates directly to effective therapeutic dosimetry. Copyright © 2014 Elsevier Inc. All rights reserved.

  3. Calorimetry

    International Nuclear Information System (INIS)

    Anon.

    1982-01-01

    We have divided this study of calorimetry at the SLC into five topics: physics with calorimeters, readout geometries, performance of existing detectors, calorimeter technologies, and new calorimeter designs. The first topic is a review of the Z 0 physics in which calorimetry would be important. We discuss the Monte Carlo model and the general features of the events which it generates. We consider how the physics affects the design of the electromagnetic and hadron calorimeters in energy resolution, segmentation, solid angle coverage, and general performance. The two ways of reading out a calorimeter, strips and towers, are the basis of the second topic. We discuss a model which makes quantitative comparisons of these two schemes, with particular reference to electromagnetic calorimeters. These programs should be useful in other studies of calorimeter performance as well. There are six detectors at PEP and SPEAR with calorimetric elements. The third topic is a review of their performance at present energies and an evaluation of the problems which would arise at SLC energies. The new technologies which may be mature enough for use in an SLC detector are considered as the fourth topic. Some are now being built into anti pp detectors, others are in test beam stages, and others are still bright ideas. We review ten techniques and include references for further pursuit. The last section combines the physics goals, readout schemes, and present and future techniques into sensible calorimeter designs which sharpen the issues. Six models resulted. We discuss their strengths, weaknesses, feasibility, and rough costs

  4. Thermodynamics of ion binding to phosphatidic acid bilayers. Titration calorimetry of the heat of dissociation of DMPA.

    Science.gov (United States)

    Blume, A; Tuchtenhagen, J

    1992-05-19

    The heat of dissociation of the second proton of 1,2-dimyristoylphosphatidic acid (DMPA) was studied as a function of temperature using titration calorimetry. The dissociation of the second proton of DMPA was induced by addition of NaOH. From the calorimetric titration experiment, the intrinsic pK0 for the dissociation reaction could be determined by applying the Gouy-Chapman theory. pK0 decreases with temperature from ca. 6.2 at 11 degrees C to 5.4 at 54 degrees C. From the total heat of reaction, the dissociation enthalpy, delta Hdiss, was determined by subtracting the heat of neutralization of water and the heat of dilution of NaOH. In the temperature range between 2 and 23 degrees C, delta Hdiss is endothermic with an average value of ca. 2.5 kcal.mol-1 and shows no clear-cut temperature dependence. In the temperature range between 23 and 52 degrees C, delta Hdiss calculated after subtraction of the heat of neutralization and dilution is not the true dissociation enthalpy but includes contributions from the phase transition enthalpy, delta Htrans, as the pH jump induces a transition from the gel to the liquid-crystalline phase. The delta Cp for the reaction enthalpy observed in this temperature range is positive. Above 53 degrees C, the pH jump induces again only the dissociation of the second proton, and the bilayers stay in the liquid-crystalline phase. In this temperature range, delta Hdiss seems to decrease with temperature. The thermodynamic data from titration calorimetry and differential scanning calorimetry as a function of pH can be combined to construct a complete enthalpy-temperature diagram of DMPA in its two ionization states.

  5. Characteristics and thermodynamics of the interaction of 6-shogaol with human serum albumin as studied by isothermal titration calorimetry

    Directory of Open Access Journals (Sweden)

    Shevin Rizal Feroz

    Full Text Available ABSTRACT The interaction between 6-shogaol, a pharmacologically active ginger constituent, and human serum albumin (HSA, the main in vivo drug transporter, was investigated using isothermal titration calorimetry (ITC. The value of the binding constant, Ka (5.02 ± 1.37 × 104 M−1 obtained for the 6-shogaol-HSA system suggested intermediate affinity. Analysis of the ITC data revealed feasibility of the binding reaction due to favorable enthalpy and entropy changes. The values of the thermodynamic parameters suggested involvement of van der Waals forces, hydrogen bonds and hydrophobic interactions in the 6-shogaol-HSA complex formation.

  6. Calorimetry energy measurement in particle physics

    CERN Document Server

    Wigmans, Richard

    2017-01-01

    Particle physics is the science that pursues the age-old quest for the innermost structure of matter and the fundamental interactions between its constituents. Modern experiments in this field rely increasingly on calorimetry, a detection technique in which the particles of interest are absorbed in the detector. Calorimeters are very intricate instruments. Their performance characteristics depend on subtle, sometimes counter-intuitive design details. This book, written by one of the world's foremost experts, is the first comprehensive text on this topic. It provides a fundamental and systematic introduction to calorimetry. It describes the state of the art in terms of both the fundamental understanding of calorimetric particle detection, and the actual detectors that have been or are being built and operated in experiments. The last chapter discusses landmark scientific discoveries in which calorimetry has played an important role. This book summarizes and puts into perspective the work described in some 900...

  7. Binding between bixin and whey protein at pH 7.4 studied by spectroscopy and isothermal titration calorimetry.

    Science.gov (United States)

    Zhang, Yue; Zhong, Qixin

    2012-02-22

    Bixin is the major coloring component of annatto used in manufacturing colored cheeses, but its presence in liquid whey causes undesirable quality of the recovered whey protein ingredients. The objective of this work was to study molecular binding between bixin and three major whey proteins (β-lactoglobulin, α-lactalbumin, and bovine serum albumin) at pH 7.4 using UV-vis absorption spectroscopy, fluorescence spectroscopy, isothermal titration calorimetry, and circular dichroism. These complementary techniques illustrated that the binding is a spontaneous complexation process mainly driven by hydrophobic interactions. The complexation is favored at a lower temperature and a higher ionic strength. At a lower temperature, the binding is entropy-driven, while it changes to an enthalpy-driven process at higher temperatures. The binding also increases the percentage of unordered secondary structures of proteins. Findings from this work can be used to develop whey protein recovery processes for minimizing residual annatto content in whey protein ingredients.

  8. Interaction of phenazinium dyes with double-stranded poly(A): spectroscopy and isothermal titration calorimetry studies.

    Science.gov (United States)

    Khan, Asma Yasmeen; Saha, Baishakhi; Kumar, Gopinatha Suresh

    2014-10-15

    A comprehensive study on the binding of phenazinium dyes viz. janus green B, indoine blue, safranine O and phenosafranine with double stranded poly(A) using various spectroscopic and calorimetric techniques is presented. A higher binding of janus green B and indoine blue over safranine O and phenosafranine to poly(A) was observed from all experiments. Intercalative mode of binding of the dyes was inferred from fluorescence polarization anisotropy, iodide quenching and viscosity experiments. Circular dichroism study revealed significant perturbation of the secondary structure of poly(A) on binding of these dyes. Results from isothermal titration calorimetry experiments suggested that the binding was predominantly entropy driven with a minor contribution of enthalpy to the standard molar Gibbs energy. The results presented here may open new opportunities in the application of these dyes as RNA targeted therapeutic agents. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of thermodynamic and kinetic parameters of aminopolycarbonate complexes of cobalt(II) and nickel(II) based on isothermal titration calorimetry data.

    Science.gov (United States)

    Tesmar, Aleksandra; Wyrzykowski, Dariusz; Muñoz, Eva; Pilarski, Bogusław; Pranczk, Joanna; Jacewicz, Dagmara; Chmurzyński, Lech

    2017-04-01

    The influence of the different side chain residues on the thermodynamic and kinetic parameters for complexation reactions of the Co 2 + and Ni 2 + ions has been investigated by using the isothermal titration calorimetry (ITC) technique supported by potentiometric titration data. The study was concerned with the 2 common tripodal aminocarboxylate ligands, namely, nitrilotriacetic acid and N-(2-hydroxyethyl) iminodiacetic acid. Calorimetric measurements (ITC) were run in the 2-(N-morpholino)ethanesulfonic acid hydrate (2-(N-morpholino) ethanesulfonic acid), piperazine-N,N'-bis(2-ethanesulfonic acid), and dimethylarsenic acid buffers (0.1 mol L -1 , pH 6) at 298.15 K. The quantification of the metal-buffer interactions and their incorporation into the ITC data analysis enabled to obtain the pH-independent and buffer-independent thermodynamic parameters (K, ΔG, ΔH, and ΔS) for the reactions under study. Furthermore, the kinITC method was applied to obtain kinetic information on complexation reactions from the ITC data. Correlations, based on kinetic and thermodynamic data, between the kinetics of formation of Co 2 + and Ni 2 + complexes and their thermodynamic stabilities are discussed. Copyright © 2016 John Wiley & Sons, Ltd.

  10. Isoperibolic Titration Calorimetry as a Tool for the Prediction of Thermodynamic Properties of Cyclodextrins

    Directory of Open Access Journals (Sweden)

    Liliana Giraldo

    2008-10-01

    Full Text Available The interaction of guest molecules ranging from pentan-1-ol to octan-1-ol with α-cyclodextrin (α-CD in water of has been studied calorimetrically at 283.15, 288.15, 293.15, 298.15 and 308.15 K with an isoperibolic titration calorimeter designed in our laboratory. The calorimetric method employed allows the determination of the thermodynamic parameters characterizing the binding process, ΔG°m, ΔH°m, ΔS°mand ΔCp°, namely free energy, enthalpy, and calorific capacity. These results show that in the temperature range investigated, the entropy change increased with chain length. This is in line with what is expected for a hydrophobic dehydration process. However, that effect is not expected to lead to the more pronounced negative CH2-increment observed for nc > 5 or 6. As for many other ligand binding processes, we can observe a significant enthalpy - entropy compensation for this system, both with respect to temperature and structure.

  11. Isoperibolic titration calorimetry as a tool for the prediction of thermodynamic properties of cyclodextrins

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Pirajan, J. C. [Universidad de los Andes, Bogota, Grupo de investigacion en solidos porosos y calorimetria, Departamento de Quimica, Facultad de Ciencias / Carrera 1 No.18 A10, Bogota (Colombia); Giraldo, L. [Universidad Nacional de Colombia, Facultad de Ciencias, Departamento de Quimica / Ciudad Universitaria, Bogota (Colombia)

    2008-07-01

    The interaction of guest molecules ranging from pentan-1-ol to octan-1-ol with {alpha}-cyclodextrin ({alpha}-CD) in water of has been studied calorimetrically at 283.15, 288.15, 293.15, 298.15 and 308.15 K with an isoperibolic titration calorimeter designed in our laboratory. The calorimetric method employed allows the determination of the thermodynamic parameters characterizing the binding process, {delta}G {sup o}{sub m}, {delta}H {sup o}{sub m}, {delta}S {sup o}{sub m} and {delta}Cp {sup o}, namely free energy, enthalpy, and calorific capacity. These results show that in the temperature range investigated, the entropy change increased with chain length. This is in line with what is expected for a hydrophobic dehydration process. However, that effect is not expected to lead to the more pronounced negative CH{sub 2}-increment observed for n{sub c} > 5 or 6. As for many other ligand binding processes, we can observe a significant enthalpy - entropy compensation for this system, both with respect to temperature and structure. (author)

  12. Thermodynamics of Ligand Binding to Acyl-Coenzyme A Binding Protein Studied by Titration Calorimetry

    DEFF Research Database (Denmark)

    Færgeman, Nils Joakim; Sigurskjold, Bent Walther; Kragelund, Birthe B.

    1996-01-01

    Ligand binding to recombinant bovine acyl-CoA binding protein (ACBP) was examined using isothermal microcalorimetry. Microcalorimetric measurements confirm that the binding affinity of acyl-CoA esters for ACBP is strongly dependent on the length of the acyl chain with a clear preference for acyl-...

  13. Thermodynamics of ligand binding to acyl-coenzyme A binding protein studied by titration calorimetry

    DEFF Research Database (Denmark)

    Færgeman, Nils J.; Sigurskjold, B W; Kragelund, B B

    1996-01-01

    Ligand binding to recombinant bovine acyl-CoA binding protein (ACBP) was examined using isothermal microcalorimetry. Microcalorimetric measurements confirm that the binding affinity of acyl-CoA esters for ACBP is strongly dependent on the length of the acyl chain with a clear preference for acyl-...

  14. Characterization of the kinetic and thermodynamic landscape of RNA folding using a novel application of isothermal titration calorimetry

    Science.gov (United States)

    Vander Meulen, Kirk A.; Butcher, Samuel E.

    2012-01-01

    A novel isothermal titration calorimetry (ITC) method was applied to investigate RNA helical packing driven by the GAAA tetraloop–receptor interaction in magnesium and potassium solutions. Both the kinetics and thermodynamics were obtained in individual ITC experiments, and analysis of the kinetic data over a range of temperatures provided Arrhenius activation energies (ΔH‡) and Eyring transition state entropies (ΔS‡). The resulting rich dataset reveals strongly contrasting kinetic and thermodynamic profiles for this RNA folding system when stabilized by potassium versus magnesium. In potassium, association is highly exothermic (ΔH25°C = −41.6 ± 1.2 kcal/mol in 150 mM KCl) and the transition state is enthalpically barrierless (ΔH‡ = −0.6 ± 0.5). These parameters are sigificantly positively shifted in magnesium (ΔH25°C = −20.5 ± 2.1 kcal/mol, ΔH‡ = 7.3 ± 2.2 kcal/mol in 0.5 mM MgCl2). Mixed salt solutions approximating physiological conditions exhibit an intermediate thermodynamic character. The cation-dependent thermodynamic landscape may reflect either a salt-dependent unbound receptor conformation, or alternatively and more generally, it may reflect a small per-cation enthalpic penalty associated with folding-coupled magnesium uptake. PMID:22058128

  15. New applications of corrosion measurements by titration (CMT)

    DEFF Research Database (Denmark)

    Bech-Nielsen, Gregers

    1998-01-01

    . It is shown that when aluminium dissolves in alkali, CMT measurements can also be applied, but in this case requiring titration with alkali. Titration with alkali is also required in a special situation, where corrosion of nickel in an acid solution and subsequent formation of a nickel complex results...

  16. Thermodynamic insights into drug-surfactant interactions: Study of the interactions of naporxen, diclofenac sodium, neomycin, and lincomycin with hexadecytrimethylammonium bromide by using isothermal titration calorimetry.

    Science.gov (United States)

    Choudhary, Sinjan; Talele, Paurnima; Kishore, Nand

    2015-08-01

    The success of drug delivery depends on the efficiency of the route of administration, which in turn relies on properties of the drug and its transport vehicle. A quantitative knowledge of association of drugs with transport vehicles is lacking when the latter are in the category of self assembled structures. The work reported in this manuscript addresses the mechanism of partitioning of naproxen, diclofenac sodium, neomycin and lincomycin in the micelles of hexadecytrimethylammonium bromide and that is quantitatively based on the measurement of thermodynamic parameters of interactions by using isothermal titration calorimetry. The addressed mechanism of partitioning is based on the identification of the type of interactions of these drugs with the surfactant micelles and monomers, along with the effect of the former on the micellization properties of the surfactant. The conclusions are based on the interpretation of the values of partitioning constant, standard molar enthalpy change, standard molar entropy change and the stoichiometry of the interaction. The results of this study have implications for deriving guidelines for the target oriented synthesis of new drugs that are to be used for effective delivery via micellar media. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Carbon dioxide titration method for soil respiration measurements

    OpenAIRE

    Martín Rubio, Luis

    2017-01-01

    This thesis was commissioned by Tampere University of Applied Sciences, which was interested in studying and developing a titration measurement method for soil respiration and biodegradability. Some experiments were carried out measuring soil respiration for testing the method and others adding some biodegradable material like polylactic acid compressed material and 100% biodegradable plastic bags to test its biodegradability and the possibility to measure it via titration. The thesi...

  18. Characterization of the 1st and 2nd EF-hands of NADPH oxidase 5 by fluorescence, isothermal titration calorimetry, and circular dichroism

    Directory of Open Access Journals (Sweden)

    Wei Chin-Chuan

    2012-04-01

    Full Text Available Abstract Background Superoxide generated by non-phagocytic NADPH oxidases (NOXs is of growing importance for physiology and pathobiology. The calcium binding domain (CaBD of NOX5 contains four EF-hands, each binding one calcium ion. To better understand the metal binding properties of the 1st and 2nd EF-hands, we characterized the N-terminal half of CaBD (NCaBD and its calcium-binding knockout mutants. Results The isothermal titration calorimetry measurement for NCaBD reveals that the calcium binding of two EF-hands are loosely associated with each other and can be treated as independent binding events. However, the Ca2+ binding studies on NCaBD(E31Q and NCaBD(E63Q showed their binding constants to be 6.5 × 105 and 5.0 × 102 M-1 with ΔHs of -14 and -4 kJ/mol, respectively, suggesting that intrinsic calcium binding for the 1st non-canonical EF-hand is largely enhanced by the binding of Ca2+ to the 2nd canonical EF-hand. The fluorescence quenching and CD spectra support a conformational change upon Ca2+ binding, which changes Trp residues toward a more non-polar and exposed environment and also increases its α-helix secondary structure content. All measurements exclude Mg2+-binding in NCaBD. Conclusions We demonstrated that the 1st non-canonical EF-hand of NOX5 has very weak Ca2+ binding affinity compared with the 2nd canonical EF-hand. Both EF-hands interact with each other in a cooperative manner to enhance their Ca2+ binding affinity. Our characterization reveals that the two EF-hands in the N-terminal NOX5 are Ca2+ specific. Graphical abstract

  19. Isothermal Titration Calorimetry and Fluorescence Spectroscopy Study Of Asphaltene Self-Association In Toluene And Interaction With A Model Resin

    DEFF Research Database (Denmark)

    Garcia, Daniel Merino; Andersen, Simon Ivar

    2002-01-01

    This article collects the work performed by Isothermal Titration Caloritnetry (ITC) in the study of the self-association of asphaltenes in toluene solutions. Calorimetric experiments show that asphaltenes, start self-associating at very low concentrations and that the existence of a Critical...... with the results of the titration of three model molecules: nonylphenol, which associates by means of hydrogen bond formation, and coronene and pyrene, which associates by stacking. The results obtained leave open the question about the model-stacking molecules, as it was not possible to elucidate whether they do...

  20. Exploring variation in binding of Protein A and Protein G to immunoglobulin type G by isothermal titration calorimetry

    DEFF Research Database (Denmark)

    Lund, L. N.; Christensen, T.; Toone, E.

    2011-01-01

    ligands and for the establishment of generic processes for the purification of various antibodies. In this paper, the interactions between the two IgG-binding proteins and IgG of two different subclasses, IgG1 and IgG4, as well as their analogous Fc fragments have been studied by isothermal titration...

  1. Application of a new method for data analysis of isothermal titration calorimetry in the interaction between human serum albumin and Ni2+

    International Nuclear Information System (INIS)

    Saboury, Ali Akbar.

    2003-01-01

    The interaction of human serum albumin (HAS) with divalent nickel ion was studied by isothermal titration calorimetry (ITC) in 30 mM Tris buffer, pH 7.0. There is a set of eight identical and independent binding sites for nickel ions on the protein at the temperature of 300 K. A new calorimetric data analysis allows the determination of the complete set of thermodynamic parameters. The binding isotherm for nickel-HSA interaction is easily obtained by carrying out two different ITC experiments. In the first experiment, the enthalpy of binding for one mole of nickel ion to one mole of binding site on HSA (ΔH=-36.5 kJ) is obtained, and is used in a second experiment to determine the binding isotherm and to find the number of binding sites (g=8) and the equilibrium constant (K=0.57 μM -1 )

  2. Thermodynamics of biphasic lanthanide extraction by tripodal diglycolamide: a solution calorimetry study

    NARCIS (Netherlands)

    Ansari, S.A.; Mohapatra, P.K.; Verboom, Willem; Rao, L.

    2016-01-01

    Isothermal titration calorimetry was employed for the direct measurement of the enthalpy of extraction (ΔHextr) of Eu(NO3)3 by using a tripodal diglycolamide (T-DGA) ligand dissolved in n-dodecane containing 5% (v/v) 2-decanol. The enthalpy of extraction obtained by titration calorimetry was in good

  3. Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime Using Controlled Calorimetry

    International Nuclear Information System (INIS)

    Don W. Miller; Andrew Kauffmann; Eric Kreidler; Dongxu Li; Hanying Liu; Daniel Mills; Thomas D. Radcliff; Joseph Talnagi

    2001-01-01

    A comprehensive description of the accomplishments of the DOE grant titled, ''Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime using Controlled Calorimetry''

  4. Mechanism of melatonin protection against copper-ascorbate-induced oxidative damage in vitro through isothermal titration calorimetry.

    Science.gov (United States)

    Ghosh, Arnab K; Naaz, Shamreen; Bhattacharjee, Bharati; Ghosal, Nirajan; Chattopadhyay, Aindrila; Roy, Souvik; Reiter, Russel J; Bandyopadhyay, Debasish

    2017-07-01

    Involvement of oxidative stress in cardiovascular diseases is well established. Melatonin's role as an antioxidant and free radical scavenger via its receptor dependent and receptor independent pathways is well known. The aim of this study is to identify and elaborate upon a third mechanism by which melatonin is able to abrogate oxidative stress. Oxidative stress was induced in vitro, by copper (0.2mM)-ascorbate (1mM) in isolated goat heart mitochondria, cytosol and peroxisomes and they were co-incubated with graded doses of melatonin. Similar experiments in a cell-free chemical system involving two pure antioxidant enzymes, Cu-Zn superoxide dismutase and catalase was also carried out. Biochemical changes in activity of these antioxidant enzymes were analysed. Isothermal titration calorimetric studies with pure Cu-Zn superoxide dismutase and catalase were also carried out. Incubation with copper-ascorbate led to alteration in activity of Cu-Zn superoxide dismutase and catalase which were found to be protected upon co-incubation with melatonin (80μM for catalase and 1μM for others). Results of isothermal titration calorimetric studies with pure Cu-Zn superoxide dismutase and catalase along with different combinations of copper chloride, ascorbic acid and melatonin suggest that when melatonin is present in the reaction medium along with copper-ascorbate, it restrains the copper-ascorbate molecules by binding with them physically along with scavenging the free radicals generated by them. The present study suggests that possibly, binding of melatonin with antioxidant enzymes masks the vulnerable sites of these antioxidant enzymes, thus preventing oxidative damage by copper-ascorbate molecules. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. Cell titration assay for measuring blastogenesis of bovine lymphocytes.

    Science.gov (United States)

    Baldwin, C L; Antczak, D F; Winter, A J

    1985-08-01

    The blastogenic response of bovine peripheral blood lymphocytes to phytohemagglutinin (PHA) and to microbial antigens was measured using a lymphocyte titration assay. Culture conditions, including lymphocyte concentrations, incubation periods and medium formulation, were established which produced linear or nearly linear responses over a range of cell concentrations. These conditions were established by testing lymphocytes from unimmunized cattle and from heifers infected with Brucella abortus with PHA and a B. abortus extract. Four cell concentrations in 2-fold increments were selected for measuring responses to PHA (3.125 X 10(3) to 2.5 X 10(4) cells/well) and to antigens (5.0 X 10(4) to 4.0 X 10(5) cells/well). The strength of response varied among animals and also over time for individual animals, but the titration assay allowed exponential proliferation to be distinguished from decline, which may have been due to overcrowding of microtiter wells, exhaustion of nutrients or induction of regulatory events. This assay provided a more reliable and discriminating method of evaluating lymphocyte proliferation responses than that achieved by single point assays. The displacement of the titration curves could be used to estimate the relative frequency of lymphocytes responding to antigens or mitogens.

  6. The Critical Micelle Concentration of Asphaltenes as Measured by Calorimetry

    DEFF Research Database (Denmark)

    Andersen, Simon Ivar; Christensen, S. D.

    2000-01-01

    Micellization of asphaltenes in solution has been investigated using a micro calorimetric titration procedure (Andersen, S. I.; Birdi, K. S. J Colloid Interface Sci. 1991, 142, 497). The method uses the analysis of heat of dissociation and dilution of asphaltene micelles when a pure solvent (or...... solvent mixture) is titrated with a solution of asphaltene in the same solvent. The asphaltene concentration of the injected solution is at a level above the critical micelle concentration (CMC). In the present paper the procedure is applied in investigation of asphaltenes as well as subfractions...

  7. Laser-Driven Calorimetry Measurements of Petroleum and Biodiesel Fuels.

    Science.gov (United States)

    Presser, Cary; Nazarian, Ashot; Millo, Amit

    2018-02-01

    Thermochemical characteristics were determined for several National Institute of Standards and Technology standard-reference-material petroleum and biodiesel fuels, using a novel laser-heating calorimetry technique. Measurements focused on the sample thermal behavior, specific heat release rate, and total specific heat release. The experimental apparatus consists of a copper sphere-shaped reactor mounted within a chamber, along with laser-beam-steering optical components, gas-supply manifold, and a computer-controlled data-acquisition system. At the center of the reactor, liquid sample is injected onto a copper pan substrate that rests and is in contact with a fine-wire thermocouple. A second thermocouple is in contact with the inner reactor sphere surface. The reactor is heated from opposing sides by a continuous-wave, near-infrared laser to achieve nearly uniform sample temperature. The change in temperature with time (thermogram) is recorded for both thermocouples, and compared to a baseline thermogram (without liquid in the pan). The thermograms are then processed (using an equation for thermal energy conservation) for the thermochemical information of interest. The results indicated that the energy reaching the pan is dominated by radiative heat transfer processes, while the dominant thermal process for the reactor sphere is the stored (internal) thermal energy within the sphere material. Sufficient laser power is necessary to detect the fuel thermal-related characteristics, and the required power can differ from one fuel to another. With sufficient laser power, one can detect the preferential vaporization of the lighter and heavier fuel fractions. The total specific heat release obtained for the different conventional and biodiesel fuels used in this investigation were similar to the expected values available in the literature.

  8. Effect of pH on the complexation of kaempferol-4'-glucoside with three β-cyclodextrin derivatives: isothermal titration calorimetry and spectroscopy study.

    Science.gov (United States)

    Zheng, Yan; Dong, Li-Na; Liu, Min; Chen, Aiju; Feng, Shangcai; Wang, Bingquan; Sun, Dezhi

    2014-01-08

    The utilization of kaempferol and its glycosides in food and pharmaceutical industries could be improved by the formation of inclusion complexes with cyclodextrins at different pH. This study explores the complexation of kaempferol-4'-glucoside with sulfobutyl ether-β-cyclodextrin (SBE-β-CD), hydroxypropyl-β-cyclodextrin (HP-β-CD), and methylated-β-cyclodextrin (M-β-CD) in phosphate buffer solutions of different pH using isothermal titration calorimetry, UV-vis absorption and proton nuclear magnetic resonance spectroscopy at 298.2 K. Experimental results showed that kaempferol-4'-glucoside binds with the three β- cyclodextrins in the same 1:1 stoichiometry. The rank order of stability constants is SBE-β-CD > HP-β-CD > M-β-CD at the same pH level and pH 6.0 > pH 7.4 > pH 9.0 for the same cyclodextrin. The binding of kaempferol-4'-glucoside with the three β-cyclodextrin derivatives is synergistically driven by enthalpy and entropy at pH 6.0 and enthalpy-driven at pH 7.4 and 9.0. The possible inclusion mode was that in the cavity of β-CD is included the planar benzopyranic-4-one part of the kaempferol-4'-glucoside.

  9. Analysis of the interactions between human serum albumin/amphiphilic penicillin in different aqueous media: an isothermal titration calorimetry and dynamic light scattering study

    International Nuclear Information System (INIS)

    Barbosa, Silvia; Taboada, Pablo; Mosquera, Victor

    2005-01-01

    The complexation process of the amphiphilic penicillins sodium cloxacillin and sodium dicloxacillin with the protein human serum albumin (HSA) in aqueous buffered solutions of pH 4.5 and 7.4 at 25 o C was investigated through isothermal titration calorimetry (ITC) and dynamic light scattering. ITC experiments were carried out in the very dilute regime and showed that although hydrophobic interactions are the leading forces for complexation, electrostatic interactions also play an important role. The possibility of the formation of hydrogen bonds is also deduced from experimental data. The thermodynamic quantities of the binding mechanism, i.e, the enthalpy, ΔHITCi, entropy, ΔSITCi, Gibbs energy, ΔGITCi, binding constant, KITCi and the number of binding sites, n i , were obtained. The binding was saturable and is characterised by Langmuir adsorption isotherms. From ITC data and following a theoretical model, the number of bound and free penicillin molecules was calculated. From Scatchard plots, KITCi and n i were obtained and compared with those from ITC data. The interaction potential between the HSA-penicillin complexes and their stability were determined at pH 7.4 from the dependence of the diffusion coefficients on protein concentration by application of the DLVO colloidal stability theory. The results indicate decreasing stability of the colloidal dispersion of the drug-protein complexes with increase in the concentration of added drug

  10. Application of prediction of equilibrium to servo-controlled calorimetry measurements

    International Nuclear Information System (INIS)

    Mayer, R.L. II

    1987-01-01

    Research was performed to develop an endpoint prediction algorithm for use with calorimeters operating in the digital servo-controlled mode. The purpose of this work was to reduce calorimetry measurement times while maintaining the high degree of precision and low bias expected from calorimetry measurements. Data from routine operation of two calorimeters were used to test predictive models at each stage of development against time savings, precision, and robustness criteria. The results of the study indicated that calorimetry measurement times can be significantly reduced using this technique. The time savings is, however, dependent on parameters in the digital servo-control algorithm and on packaging characteristics of measured items

  11. Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime Using Controlled Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Don W. Miller; Andrew Kauffmann; Eric Kreidler; Dongxu Li; Hanying Liu; Daniel Mills; Thomas D. Radcliff; Joseph Talnagi

    2001-12-31

    A comprehensive description of the accomplishments of the DOE grant titled, ''Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime using Controlled Calorimetry''.

  12. Molecular interaction studies of acetylcholinesterase with potential acetylcholinesterase inhibitors from the root of Rhodiola crenulata using molecular docking and isothermal titration calorimetry methods.

    Science.gov (United States)

    Li, Fa-Jie; Liu, Yuan; Yuan, Yuan; Yang, Bin; Liu, Zhen-Ming; Huang, Lu-Qi

    2017-11-01

    (-)-Epicatechin gallate ((-)-ECG), 1,2,3,4,6-O-pentagalloylglucose (PGG), rhodionin, herbacetin and rhodiosin isolated from the root of Rhodiola crenulata exhibited potent, dose-dependent inhibitory effects on acetylcholinesterase (AChE) with IC 50 ranged from 57.50±5.83 to 2.43±0.34μg/mL. With the aim of explaining the differences in activity of these active ingredients and clarifying how they inhibit AChE, the AChE-inhibitor interactions were further explored using molecular docking and isothermal titration calorimetry (ITC) methods in the present study. Molecular docking studies revealed that all compounds except PGG showed binding energy values ranging from -10.30 to -8.00kcal/mol while the binding energy of galantamine, a known AChE inhibitor, was -9.53kcal/mol; they inhibited the AChE by binding into the ligand pocket with the similar binding pattern to that of galantamine by interacting with Glu199 of AChE. Inhibition constant of these active ingredients had a positive correlation with binding energy. The interaction between AChE and PGG was further evaluated with the ITC method and the results indicated that the PGG-AChE interaction was relevant to AChE concentration. The results revealed a possible mechanism for the AChE inhibition activity of these bioactive ingredients, which may provide some help in lead compounds optimization in the future. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Dual-Readout Calorimetry for High-Quality Energy Measurements

    CERN Document Server

    Wigmans, R

    2010-01-01

    During the past seven years, the DREAM Collaboration has systematically investigated all factors that determine and limit the precision with which the properties of hadrons and jets can be measured in calorimeters. Using simultaneous detection of the deposited energy and the Cerenkov light produced in hadronic shower development (dual readout), the fluctuations in the electromagnetic shower fraction could be measured event by event and their effects on signal linearity, response function and energy resolution eliminated. Detailed measurement of the time structure of the signals made it possible to measure the contributions of nuclear evaporation to the signals and thus reduce the effects of fluctuations in “invisible energy”. We are now embarking on the construction of a full-scale calorimeter which incorporates all these elements and which should make it possible to measure the four-vectors of both electrons, hadrons and jets with very high precision, in an instrument that can be simply calibrated with e...

  14. Indirect calorimetry

    NARCIS (Netherlands)

    Gerrits, W.J.J.; Labussière, E.

    2015-01-01

    The use of indirect calorimetry to measure the heat production of men and animals has increased rapidly since the pioneering work of Lavoisier. Measurement of the consumption of oxygen and production of carbon dioxide are the basis for the measurement of heat production. Today, applications of

  15. Attributes measurements by calorimetry in 15 to 30 minutes

    International Nuclear Information System (INIS)

    Fiarman, S.; Perry, R.B.

    1987-01-01

    An analysis of the early portion of the power-history data collected with both of the IAEA's air-cooled bulk calorimeters has demonstrated that such calorimeters can measure the power from preheated containers of plutonium oxide with an accuracy of 2 to 5% in 15 to 30 minutes. Material accountancy at plutonium facilities has a need for such a capability for measurement of Pu scrap. Also, the International Atomic Energy Agency (IAEA) could use just two calorimeters and a gamma-ray assay system for reliable variables and attributes measurements of plutonium mass during a two-day physical-inventory verification (PIV) at a mixed-oxide (MOX) fuel-fabrication facility. The assay results would be free of the concerns about sample moisture, impurities, and geometry that previously have limited the accuracy of assays based on neutron measurements

  16. Periods found in heat measurements obtained by calorimetry

    International Nuclear Information System (INIS)

    Jordan, K.C.

    1984-01-01

    During a span of 640 days, a periodicity of 1.5158 +- 0.0008 days was discovered in successive heater equilibria on Calorimeter No. 127. Measurements were taken at 12-h intervals, with occasional changes of exactly 3 or 6 h in the schedule of measurements. This schedule eliminated all other possible periods except a period of 0.150156 days. Periods of 1.519125 and 1.511283 days were discovered in data on the excess length of day as obtained by the US Naval Observatory over a period of 24 y. These two periods could equally well represent periods of 0.150189 and 0.150112 days, since measurements were obtained only once every 24 h. It is suggested that periods observed in sensitive calorimeters and in length of day data may be related. 1 reference, 6 figures, 5 tables

  17. Measurement of Fiber Saturation Point of Wood Using Differential Scanning Calorimetry: Measurement Fundamentals and Experimental Results

    Directory of Open Access Journals (Sweden)

    asghar tarmian

    2017-02-01

    Full Text Available In this research, the measurement fundamentals of fiber saturation point (FSP using differential scanning calorimetry (DSC method were explained. This method is based on the assumption that free water is frozen but bound water remains unfrozen in low temperatures. Thus, the FSP can be calculated by measuring the enthalpy of melting of frozen wet samples. This method measures the amount of energy absorbed or released by a sample when it is heated or cooled. Results showed that the DSC method may yield a higher FSP value compared to the widely accepted value of 30%, depending on the wood species. Both thermal and chemical (acetylation modification methods reduced the FSP but in the acetylation method, there was no linear correlation between the weight gain percentage (WPG and FSP.

  18. IMPEDANCE METHOD OF MEASURING OF THE TITRATABLE ACIDITY OF YOGURT

    Directory of Open Access Journals (Sweden)

    Miroslav Vasilev

    2016-10-01

    Full Text Available In the present work are analyzed studies related to changes in the active impedance component of the dairy environment caused by the flow of lactic fermentation and coagulation of casein in milk. The aim of this work was to determine the relationship between the relative change of titratable acidity and the relative change of active impedance component of the dairy environment with lactic fermentation, causing coagulation of the casein in milk. . The data were interpolated with cubic spline, visualizing how when the fat content increases, the electrical resistance increases too. All data, collected during the tests would complement and be used for solving the optimization problem to determine the time of completion of the coagulation in future work.

  19. Potentiometric Measurement of Transition Ranges and Titration Errors for Acid/Base Indicators

    Science.gov (United States)

    Flowers, Paul A.

    1997-07-01

    Sophomore analytical chemistry courses typically devote a substantial amount of lecture time to acid/base equilibrium theory, and usually include at least one laboratory project employing potentiometric titrations. In an effort to provide students a laboratory experience that more directly supports their classroom discussions on this important topic, an experiment involving potentiometric measurement of transition ranges and titration errors for common acid/base indicators has been developed. The pH and visually-assessed color of a millimolar strong acid/base system are monitored as a function of added titrant volume, and the resultant data plotted to permit determination of the indicator's transition range and associated titration error. Student response is typically quite positive, and the measured quantities correlate reasonably well to literature values.

  20. Design and first measurements of an alternative calorimetry chamber for the HZB quadrupole resonator

    CERN Document Server

    Keckert, Sebastian; Knobloch, Jens; Kugeler, Oliver

    2015-01-01

    The systematic research on superconducting thin films requires dedicated testing equipment. The Quadrupole Resonator (QPR) is a specialized tool to characterize the superconducting RF properties of circular planar samples. A calorimetric measurement of the RF surface losses allows the surface resistance to be measured with sub nano-ohm resolution. This measurement can be performed over a wide temperature and magnetic field range, at frequencies of 433, 866 and 1300 MHz. The system at Helmholtz-Zentrum Berlin (HZB) is based on a resonator built at CERN and has been optimized to lower peak electric fields and an improved resolution. In this paper the design of an alternative calorimetry chamber is presented, providing flat samples for coating which are easy changeable. All parts are connected by screwing connections and no electron beam welding is required. Furthermore this design enables exchangeability of samples between the resonators at HZB and CERN. First measurements with the new design show ambiguous r...

  1. Null-point titration measurements of free magnesium in stored erythrocytes

    International Nuclear Information System (INIS)

    Bock, J.L.; Yusuf, Y.; Puntillo, E.

    1987-01-01

    Free intracellular magnesium concentration (Mg/sub i/) was measured in stored human erythrocytes, using null-point titration with ionophore A23187. For cells stored 31 P NMR spectroscopy, which showed a decrease in Mg/sub i/ with storage. However, the NMR measurements are performed with no pretreatment of the cells, while the null-point method requires an initial washing step, which alters pH/sub i/ and may also alter Mg/sub i/. The titration-measured Mg/sub i/ values are still surprisingly low for long-stored cells, considering that depletion of ATP and 2,3-DPG should release bound Mg. Using the titration-measured Mg/sub i/ values along with measurements of total Mg, ATP, and 2,3-DPG, they estimate that an additional buffer contains about 47% of total Mg in cells stored 21 days. Mg/sub i/ determinations by both 31 P NMR and null-point titration thus indicate that erythrocyte Mg is largely bound to a high-capacity, low-affinity buffer whose relative importance increases during cell storage. Discrepancies between the methods require further investigation

  2. Thermal expansivities of peptides, polypeptides and proteins as measured by pressure perturbation calorimetry.

    Science.gov (United States)

    Pandharipande, Pranav P; Makhatadze, George I

    2015-04-01

    The main goal of this work was to provide direct experimental evidence that the expansivity of peptides, polypeptides and proteins as measured by pressure perturbation calorimetry (PPC), can serve as a proxy to characterize relative compactness of proteins, especially the denatured state ensemble. This is very important as currently only small angle X-ray scattering (SAXS), intrinsic viscosity and, to a lesser degree, fluorescence resonance transfer (FRET) experiments are capable of reporting on the compactness of denatured state ensembles. We combined the expansivity measurements with other biophysical methods (far-UV circular dichroism spectroscopy, differential scanning calorimetry, and small angle X-ray scattering). Three case studies of the effects of conformational changes on the expansivity of polypeptides in solution are presented. We have shown that expansivity appears to be insensitive to the helix-coil transition, and appears to reflect the changes in hydration of the side-chains. We also observed that the expansivity is sensitive to the global conformation of the polypeptide chain and thus can be potentially used to probe hydration of different collapsed states of denatured or even intrinsically disordered proteins. Copyright © 2015 Elsevier Inc. All rights reserved.

  3. Electron beam water calorimetry measurements to obtain beam quality conversion factors.

    Science.gov (United States)

    Muir, Bryan R; Cojocaru, Claudiu D; McEwen, Malcolm R; Ross, Carl K

    2017-10-01

    To provide results of water calorimetry and ion chamber measurements in high-energy electron beams carried out at the National Research Council Canada (NRC). There are three main aspects to this work: (a) investigation of the behavior of ionization chambers in electron beams of different energies with focus on long-term stability, (b) water calorimetry measurements to determine absorbed dose to water in high-energy beams for direct calibration of ion chambers, and (c) using measurements of chamber response relative to reference ion chambers, determination of beam quality conversion factors, k Q , for several ion chamber types. Measurements are made in electron beams with energies between 8 MeV and 22 MeV from the NRC Elekta Precise clinical linear accelerator. Ion chamber measurements are made as a function of depth for cylindrical and plane-parallel ion chambers over a period of five years to investigate the stability of ion chamber response and for indirect calibration. Water calorimetry measurements are made in 18 MeV and 22 MeV beams. An insulated enclosure with fine temperature control is used to maintain a constant temperature (drifts less than 0.1 mK/min) of the calorimeter phantom at 4°C to minimize effects from convection. Two vessels of different designs are used with calibrated thermistor probes to measure radiation induced temperature rise. The vessels are filled with high-purity water and saturated with H 2 or N 2 gas to minimize the effect of radiochemical reactions on the measured temperature rise. A set of secondary standard ion chambers are calibrated directly against the calorimeter. Finally, several other ion chambers are calibrated in the NRC 60 Co reference field and then cross-calibrated against the secondary standard chambers in electron beams to realize k Q factors. The long-term stability of the cylindrical ion chambers in electron beams is better (always <0.15%) than plane-parallel chambers (0.2% to 0.4%). Calorimetry measurements

  4. The formation of amino acid and dipeptide complexes with α-cyclodextrin and cucurbit[6]uril in aqueous solutions studied by titration calorimetry

    International Nuclear Information System (INIS)

    Buschmann, H.-J.; Schollmeyer, E.; Mutihac, L.

    2003-01-01

    The complex stabilities and the thermodynamic data for the complexation of α-cyclodextrin and cucurbit[6]uril with some amino acids (glycine, L-alanine, L-valine, L-phenylalanine, 6-amino hexanoic acid, 8-amino octanoic acid, 11-amino undecanoic acid) and dipeptides (glycyl-glycine, glycyl-L-valine, glycyl-L-leucine and glycyl-L-phenylalanine) have been determined in aqueous solution by calorimetric titrations. The complex formation with α-cyclodextrin is mainly favoured by entropic contributions due to the release of water molecules from the cavity of the ligand. The values of the reaction enthalpies are small with the exception of 11-amino undecanoic acid. In case of the ligand cucurbit[6]uril, ion-dipole interactions between the protonated amino groups of the amino acids and the carbonyl groups take place. By steric reasons these interactions are lowered for native amino acids because the polar carboxylic groups are always located outside the hydrophobic cavity of cucurbit[6]uril. The complexes of both ligands with dipeptides in water are characterised by hydrophobic interactions and in case of cucurbit[6]uril by additional ion-dipole interactions

  5. The active titration method for measuring local hydroxyl radical concentration

    Science.gov (United States)

    Sprengnether, Michele; Prinn, Ronald G.

    1994-01-01

    We are developing a method for measuring ambient OH by monitoring its rate of reaction with a chemical species. Our technique involves the local, instantaneous release of a mixture of saturated cyclic hydrocarbons (titrants) and perfluorocarbons (dispersants). These species must not normally be present in ambient air above the part per trillion concentration. We then track the mixture downwind using a real-time portable ECD tracer instrument. We collect air samples in canisters every few minutes for roughly one hour. We then return to the laboratory and analyze our air samples to determine the ratios of the titrant to dispersant concentrations. The trends in these ratios give us the ambient OH concentration from the relation: dlnR/dt = -k(OH). A successful measurement of OH requires that the trends in these ratios be measureable. We must not perturb ambient OH concentrations. The titrant to dispersant ratio must be spatially invariant. Finally, heterogeneous reactions of our titrant and dispersant species must be negligible relative to the titrant reaction with OH. We have conducted laboratory studies of our ability to measure the titrant to dispersant ratios as a function of concentration down to the few part per trillion concentration. We have subsequently used these results in a gaussian puff model to estimate our expected uncertainty in a field measurement of OH. Our results indicate that under a range of atmospheric conditions we expect to be able to measure OH with a sensitivity of 3x10(exp 5) cm(exp -3). In our most optimistic scenarios, we obtain a sensitivity of 1x10(exp 5) cm(exp -3). These sensitivity values reflect our anticipated ability to measure the ratio trends. However, because we are also using a rate constant to obtain our (OH) from this ratio trend, our accuracy cannot be better than that of the rate constant, which we expect to be about 20 percent.

  6. Determination of thermodynamic parameters for complexation of calcium and magnesium with chondroitin sulfate isomers using isothermal titration calorimetry: Implications for calcium kidney-stone research

    Science.gov (United States)

    Rodgers, Allen L.; Jackson, Graham E.

    2017-04-01

    Chondroitin sulfate (CS) occurs in human urine. It has several potential binding sites for calcium and as such may play an inhibitory role in calcium oxalate and calcium phosphate (kidney stone disease by reducing the supersaturation (SS) and crystallization of these salts. Urinary magnesium is also a role player in determining speciation in stone forming processes. This study was undertaken to determine the thermodynamic parameters for binding of the disaccharide unit of two different CS isomers with calcium and magnesium. These included the binding constant K. Experiments were performed using an isothermal titration calorimeter (ITC) at 3 different pH levels in the physiological range in human urine. Data showed that interactions between the CS isomers and calcium and magnesium occur via one binding site, thought to be sulfate, and that log K values are 1.17-1.93 and 1.77-1.80 for these two metals respectively. Binding was significantly stronger in Mg-CS than in Ca-CS complexes and was found to be dependent on pH in the latter but not in the former. Furthermore, binding in Ca-CS complexes was dependent on the location of the sulfate binding site. This was not the case in the Mg-CS complexes. Interactions were shown to be entropy driven and enthalpy unfavourable. These findings can be used in computational modeling studies to predict the effects of the calcium and magnesium CS complexes on the speciation of calcium and the SS of calcium salts in real urine samples.

  7. Measurement and Model Validation of Nanofluid Specific Heat Capacity with Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    Harry O'Hanley

    2012-01-01

    Full Text Available Nanofluids are being considered for heat transfer applications; therefore it is important to know their thermophysical properties accurately. In this paper we focused on nanofluid specific heat capacity. Currently, there exist two models to predict a nanofluid specific heat capacity as a function of nanoparticle concentration and material. Model I is a straight volume-weighted average; Model II is based on the assumption of thermal equilibrium between the particles and the surrounding fluid. These two models give significantly different predictions for a given system. Using differential scanning calorimetry (DSC, a robust experimental methodology for measuring the heat capacity of fluids, the specific heat capacities of water-based silica, alumina, and copper oxide nanofluids were measured. Nanoparticle concentrations were varied between 5 wt% and 50 wt%. Test results were found to be in excellent agreement with Model II, while the predictions of Model I deviated very significantly from the data. Therefore, Model II is recommended for nanofluids.

  8. Dual-Readout Calorimetry for High-Quality Energy Measurements. Final Report

    International Nuclear Information System (INIS)

    Wigmans, Richard; Nural, Akchurin

    2013-01-01

    This document constitutes the final report on the project Dual-Readout Calorimetry for High-Quality Energy Measurements. The project was carried out by a consortium of US and Italian physicists, led by Dr. Richard Wigmans (Texas tech University). This consortium built several particle detectors and tested these at the European Center for Nuclear Research (CERN) in Geneva, Switzerland. The idea arose to use scintillating crystals as dual-readout calorimeters. Such crystals were of course already known to provide excellent energy resolution for the detection of particles developing electromagnetic (em) showers. The efforts to separate the signals from scintillating crystals into scintillation and Cerenkov components led to four different methods by which this could be accomplished. These methods are based on a) the directionality, b) spectral differences, c) the time structure, and d) the polarization of the signals

  9. Calorimetry Minisensor for the Localised Measurement of Surface Heat Dissipated from the Human Body.

    Science.gov (United States)

    Socorro, Fabiola; Rodríguez de Rivera, Pedro Jesús; Rodríguez de Rivera, Manuel

    2016-11-06

    We have developed a calorimetry sensor that can perform a local measurement of the surface heat dissipated from the human body. The operating principle is based on the law of conductive heat transfer: heat dissipated by the human body passes across a thermopile located between the individual and a thermostat. Body heat power is calculated from the signals measured by the thermopile and the amount of power dissipated across the thermostat in order to maintain a constant temperature. The first prototype we built had a detection area measuring 6 × 6 cm², while the second prototype, which is described herein, had a 2 × 2 cm² detection area. This new design offers three advantages over the initial one: (1) greater resolution and three times greater thermal sensitivity; (2) a twice as fast response; and (3) it can take measurements from smaller areas of the body. The sensor has a 5 mW resolution, but the uncertainty is greater, up to 15 mW, due to the measurement and calculation procedure. The order of magnitude of measurements made in healthy subjects ranged from 60 to 300 mW at a thermostat temperature of 28 °C and an ambient room temperature of 21 °C. The values measured by the sensor depend on the ambient temperature and the thermostat's temperature, while the power dissipated depends on the individual's metabolism and any physical and/or emotional activity.

  10. HEAT OF HYDRATION OF SALTSTONE MIXES-MEASUREMENT BY ISOTHERMAL CALORIMETRY

    International Nuclear Information System (INIS)

    Harbour, J; Vickie Williams, V; Tommy Edwards, T

    2007-01-01

    This report provides initial results on the measurement of heat of hydration of Saltstone mixes using isothermal calorimetry. The results were obtained using a recently purchased TAM Air Model 3116 Isothermal Conduction Calorimeter. Heat of hydration is an important property of Saltstone mixes. Greater amounts of heat will increase the temperature of the curing mix in the vaults and limit the processing rate. The heat of hydration also reflects the extent of the hydraulic reactions that turn the fluid mixture into a ''stone like'' solid and consequently impacts performance properties such as permeability. Determining which factors control these reactions, as monitored by the heat of hydration, is an important goal of the variability study. Experiments with mixes of portland cement in water demonstrated that the heats measured by this technique over a seven day period match very well with the literature values of (1) seven day heats of hydration using the standard test method for heat of hydration of hydraulic cement, ASTM C 186-05 and (2) heats of hydration measured using isothermal calorimetry. The heats of hydration of portland cement or blast furnace slag in a Modular Caustic Side Solvent Extraction Unit (MCU) simulant revealed that if the cure temperature is maintained at 25 C, the amount of heat released over a seven day period is roughly 62% less than the heat released by portland cement in water. Furthermore, both the blast furnace slag and the portland cement were found to be equivalent in heat production over the seven day period in MCU. This equivalency is due to the activation of the slag by the greater than 1 Molar free hydroxide ion concentration in the simulant. Results using premix (a blend of 10% cement, 45% blast furnace slag, and 45% fly ash) in MCU, Deliquification, Dissolution and Adjustment (DDA) and Salt Waste Processing Facility (SWPF) simulants reveal that the fly ash had not significantly reacted (undergone hydration reactions) after seven

  11. Isothermal calorimetry: Impact of measurements error on heat of reaction and kinetic calculations

    International Nuclear Information System (INIS)

    Papadaki, Maria; Nawada, Hosadu P.; Gao, Jun; Fergusson-Rees, Andrew; Smith, Michael

    2007-01-01

    Heat flow and power compensation calorimetry measures the power generation of a reaction via an energy balance over an appropriately designed isothermal reactor. However, the measurement of the power generated by a reaction is a relative measurement, and calibrations are used to eliminate the contribution of a number of unknown factors. In this work the effect of the error in the measurement of temperature of electric power used in the calibrations and the heat transfer coefficient and baseline is assessed. It has been shown that the error in all aforementioned quantities reflects on the baseline and it can have a very serious impact on the accuracy of the measurement. The influence of the fluctuation of ambient temperature has been evaluated and a means of a correction that reduces its impact has been implemented. The temperature of dosed material is affected by the heat loses if reaction is performed at high temperature and low dosing rate. An experimental methodology is presented that can provide means of assessment of the actual temperature of the dosed material. Depending on the reacting system, the heat of evaporation could be included in the baseline, especially if non-condensable gases are produced during the course of the reaction

  12. MO-AB-BRA-03: Calorimetry-Based Absorbed Dose to Water Measurements Using Interferometry

    Energy Technology Data Exchange (ETDEWEB)

    Flores-Martinez, E; Malin, M; DeWerd, L [University of WI-Madison/ADCL, Madison, WI (United States)

    2015-06-15

    Purpose: Interferometry-based calorimetry is a novel technique to measure radiation-induced temperature changes allowing the measurement of absorbed dose to water (ADW). There are no mechanical components in the field. This technique also has the possibility of obtaining 2D dose distributions. The goal of this investigation is to calorimetrically-measure doses between 2.5 and 5 Gy over a single projection in a photon beam using interferometry and compare the results with doses calculated using the TG-51 linac calibration. Methods: ADW was determined by measuring radiation-induced phase shifts (PSs) of light passing through water irradiated with a 6 MV photon beam. A 9×9×9 cm{sup 3} glass phantom filled with water and placed in an arm of a Michelson interferometer was irradiated with 300, 400, 500 and 600 monitor units. The whole system was thermally insulated to achieve sufficient passive temperature control. The depth of measurement was 4.5 cm with a field size of 7×7 cm{sup 2}. The intensity of the fringe pattern was monitored with a photodiode and used to calculate the time-dependent PS curve. Data was acquired 60 s before and after the irradiation. The radiation-induced PS was calculated by taking the difference in the pre- and post-irradiation drifts extrapolated to the midpoint of the irradiation. Results were compared to computed doses. Results: Average comparison of calculated ADW values with interferometry-measured values showed an agreement to within 9.5%. k=1 uncertainties were 4.3% for calculations and 14.7% for measurements. The dominant source of uncertainty for the measurements was a temperature drift of about 30 µK/s caused by heat conduction from the interferometer’s surroundings. Conclusion: This work presented the first absolute ADW measurements using interferometry in the dose range of linac-based radiotherapy. Future work to improve measurements’ reproducibility includes the implementation of active thermal control techniques.

  13. Enhanced thermal property measurement of a silver zinc battery cell using isothermal calorimetry

    International Nuclear Information System (INIS)

    Ubelhor, Ryan; Ellison, Daniel; Pierce, Cecilia

    2015-01-01

    Highlights: • Design and construction of novel heat flow calorimeter for large battery cell. • Heat flow characterization of silver zinc battery under load. • Thermal efficiency determination of silver zinc battery under load. • Surface map of heat flow of silver zinc battery under load. - Abstract: The push for increased energy density of electrochemical cells highlights the need for novel electrochemical techniques as well as additional characterization methods for these cells in order to meet user needs and safety requirements. To achieve ever increasing energy densities and faster controlled release of that energy, all materials of construction must be constantly evaluated from electrode to casing and everything in-between. Increasing the energy density of the cell improves its utility, but it also increases the waste heat and maximum potential uncontrolled energy release. Design agents and system developers need new ways to monitor and classify the probability and severity of the catastrophic failures as well as the system characteristics during intended operation. To support optimization of these battery cells it is necessary to understand their thermal characteristics at rest as well as under prescribed charge and discharge cycles. One of the many calorimetric tools available to observe and record these characteristics is heat flow calorimetry. Typically, a heat flow calorimeter is operated isothermally and measures the sum heat released or consumed by a sample material inside of a calorimetric measuring cell. For this study an improved calorimetric measuring cell for a modified Hart 6209 precision temperature bath was designed and constructed to measure the heat flow of larger electrochemical cells (18 × 8 × 16 cm). This new calorimetric measuring cell is constructed to allow independent measurements of heat flow among each of the sample’s six sides in contrast to the typical one measurement of the average heat flow. Heat flows from 0.01 to 7

  14. Measuring titratable alkalinity by single versus double endpoint titration: An evaluation in two cyprinodont species and implications for characterizing net H+ flux in aquatic organisms.

    Science.gov (United States)

    Brix, Kevin V; Wood, Chris M; Grosell, Martin

    2013-01-01

    In this study, Na(+) uptake and acid-base balance in the euryhaline pupfish Cyprinodon variegatus variegatus were characterized when fish were exposed to pH 4.5 freshwater (7mM Na(+)). Similar to the related cyprinodont, Fundulus heteroclitus, Na(+) uptake was significantly inhibited when exposed to low pH water. However, it initially appeared that C. v. variegatus increased apparent net acid excretion at low pH relative to circumneutral pH. This result is opposite to previous observations for F. heteroclitus under similar conditions where fish were observed to switch from apparent net H(+) excretion at circumneutral pH to apparent net H(+) uptake at low pH. Further investigation revealed disparate observations between these studies were the result of using double endpoint titrations to measure titratable alkalinity fluxes in the current study, while the earlier study utilized single endpoint titrations to measure these fluxes (i.e.,. Cyprinodon acid-base transport is qualitatively similar to Fundulus when characterized using single endpoint titrations). This led to a comparative investigation of these two methods. We hypothesized that either the single endpoint methodology was being influenced by a change in the buffer capacity of the water (e.g., mucus being released by the fish) at low pH, or the double endpoint methodology was not properly accounting for ammonia flux by the fish. A series of follow-up experiments indicated that buffer capacity of the water did not change significantly, that excretion of protein (a surrogate for mucus) was actually reduced at low pH, and that the double endpoint methodology does not properly account for NH(3) excretion by fish under low pH conditions. As a result, it overestimates net H(+) excretion during low pH exposure. After applying the maximum possible correction for this error (i.e., assuming that all ammonia is excreted as NH(3)), the double endpoint methodology indicates that net H(+) transport was reduced to

  15. Direct measurement of electron beam quality conversion factors using water calorimetry.

    Science.gov (United States)

    Renaud, James; Sarfehnia, Arman; Marchant, Kristin; McEwen, Malcolm; Ross, Carl; Seuntjens, Jan

    2015-11-01

    electron energy dependence of the PTW Roos data measured in this work and a recent MC-based study are also shown. This is the first time that water calorimetry has been successfully used to measure electron beam quality conversion factors for energies as low as 6 MeV (R50=2.25 cm).

  16. Karl Fischer titration and coulometry for measurement of water content in small cartilage specimens.

    Science.gov (United States)

    Spahn, Gunter; Plettenberg, Holger; Nagel, Horst; Kahl, Enrico; Klinger, Hans Michael; Günther, Manfred; Mückley, Thomas; Hofmann, Gunther O

    2006-12-01

    This study evaluated the efficiency of Karl Fischer titration and coulometry for measurement of water content in small intact and defective cartilage specimens. Cartilage from the main weight-bearing zone of the medial condyle of 38 fresh sheep knees was used. Of these, 20 condyles had an intact cartilage, while defects (14 grade I and 4 grade II) were found in the rest. The mechanical hardness was determined as Shore A. Cartilage specimens of approximately 5 mg were analyzed in special devices for moisture measurement and then continuously heated up to 105 degrees C. The actual measurement was performed in an electric cell (coulometry). An electrode was laminated with hygroscopic phosphorus pentoxide. In the electrochemical reaction, H and O are liberated from the electrode. The requirement for electric energy correlates with the amount of water in the specimen. The water content in intact cartilage was 66.9%. Grade I (72.6%) and grade II (77.8%) defects had significantly higher water content. Significantly higher and faster spontaneous evaporation was observed in cartilage defects at room temperature. The water content and spontaneous water evaporation correlated with significantly lower mechanical hardness. The experimental design (combined method of thermogravimetry, Karl Fischer titration, and coulometry) was sufficient for evaluating the water content in small cartilage specimens. It is also possible to measure the temperature-dependent water liberation from cartilage specimens.

  17. Indirect Calorimetry Measurement of Energy Expenditure Related to Body Position Changes in Healthy Adults.

    Science.gov (United States)

    Obata, Kengo; Yumoto, Tetsuya; Fuke, Soichiro; Tsukahara, Kohei; Naito, Hiromichi; Iida, Atsuyoshi; Takahashi, Tetsuya; Ujike, Yoshihito; Nakao, Atsunori

    2017-12-01

    Early mobilization is advocated to prevent intensive care unit-acquired physical weakness, but the patient's workload and its changes in response to body position changes have not been established. We used indirect calorimetry to determine the energy expenditure (EE) in response to body position changes, and we assessed EE's correlation with respiratory parameters in healthy volunteers: 8 males and 8 females, mean age 23.4±1.3 years. The subjects started in the resting supine position followed by a 30° head-up position, a 60° head-up position, an upright sitting position, a standing position, and the resting supine position. EE was determined in real time by indirect calorimetry monitoring the subject's respiratory rate, tidal volume (VT), and minute volume (MV). The highest values were observed immediately after the subjects transitioned from standing to supine, and this was significantly higher compared to the original supine position (1,450±285 vs. 2,004±519 kcal/day, p<0.01). Moderate correlations were observed between VT and EE (r=0.609, p<0.001) and between MV and EE (r=0.576, p<0.001). Increasing VT or MV indicates an increasing patient workload during mobilization. Monitoring these parameters may contribute to safe rehabilitation. Further studies should assess EE in critically ill patients.

  18. Thermodynamics of self-assembling of mixture of a cationic gemini surfactant and sodium dodecylsulfate in aqueous solution: Calorimetry, conductivity and surface pressure measurements

    International Nuclear Information System (INIS)

    Bai, Guangyue; Wang, Yujie; Ding, Yanhong; Zhuo, Kelei; Wang, Jianji; Bastos, Margarida

    2016-01-01

    Highlights: • ITC provided thermodynamic characterization of self-association of oppositely charged gemini/SDS surfactants. • Phase transitions and corresponding enthalpies were obtained by ITC. • The transitions reflect a change in morphology, supported by Cryo-TEM images. • Conductivity and ITC results show very good agreement. • An asymmetric distribution of surfactants in the aggregates is supported by results. - Abstract: The thermodynamics and phase behavior of mixtures of cationic gemini surfactant decanediyl-α,ω-bis(dodecyldimethylammonium bromide) (12-10-12) and sodium dodecylsulfate (SDS) were studied in the dilute SDS-rich region. The enthalpy of interaction between both surfactant monomers before the critical micelle concentration for the mixture (cmc mix ) was determined by isothermal titration calorimetry (ITC). After the cmc mix , ITC results exhibited a first process associated with a large endothermic enthalpy change followed by a second one with a very small exothermic enthalpy change. In the same regions, the conductivity curves show an increase in slope after the break, followed by a plateau region, respectively for the two processes. The combined results from the various methodologies used lead us to propose that the first process reflects the formation of non-spherical micelles and the second one the vesicle formation. The area per catanionic complex was obtained through surface pressure measurements, leading to an apparent packing parameter ⩾1. The observed behavior may be rationalized on the basis of the hypothesis that both surfactants distribute asymmetrically in the vesicle bilayers and unevenly in the non-spherical micelle. In order to get structural information Cryo-TEM experiments were performed, which provided images that support this interpretation. From all the information gathered a phase diagram was mapped, including three one-phase regions of spherical micelles, non-spherical micelles and vesicles.

  19. Constructing a proton titration curve from ion-step measurements, applied to a membrane with adsorbed protein

    NARCIS (Netherlands)

    Eijkel, Jan C.T.; Bosch, Coen; Olthuis, Wouter; Bergveld, Piet

    1997-01-01

    A new measuring method is described for obtaining a proton titration curve. The curve is obtained from a microporous composite membrane, consisting of polystyrene beads in an agarose matrix, with lysozyme molecules adsorbed to the bead surface. The membrane is incorporated into a sensor system by

  20. Titration and Spectroscopic Measurements of Poultry Litter pH Buffering Capacity.

    Science.gov (United States)

    Cassity-Duffey, Kate; Cabrera, Miguel; Mowrer, Jake; Kissel, David

    2015-07-01

    The pH value of poultry litter is affected by nitrification, mineralization, and the addition of acidifying chemicals, all acting on the poultry litter pH buffering capacity (pHBC). Increased understanding of poultry litter pHBC will aid in modeling NH volatilization from surface-applied poultry litter as well as estimating rates of alum applications. Our objectives were to (i) determine the pHBC of a wide range of poultry litters; (ii) assess the accuracy of near-infrared reflectance spectroscopy (NIRS) for determining poultry litter pHBC; and (iii) demonstrate the use of poultry litter pHBC to increase the accuracy of alum additions. Litter pHBC was determined by titration and calculated from linear and sigmoidal curves. For the 37 litters measured, linear pHBC ranged from 187 to 537 mmol (pH unit) kg dry litter. The linear and sigmoidal curves provided accurate predictions of pHBC, with most > 0.90. Results from NIRS analysis showed that the linear pHBC expressed on an "as is" water content basis had a NIRS coefficient of calibration (developed using a modified partial least squares procedure) of 0.90 for the 37 poultry litters measured. Using the litter pHBC, an empirical model was derived to determine the amount of alum needed to create a target pH. The model performed well in the range of pH 6.5 to 7.5 (RMSE = 0.07) but underpredicted the amount of alum needed to reach pH litter, which prevented its hydrolysis. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  1. Titration Curves: Fact and Fiction.

    Science.gov (United States)

    Chamberlain, John

    1997-01-01

    Discusses ways in which datalogging equipment can enable titration curves to be measured accurately and how computing power can be used to predict the shape of curves. Highlights include sources of error, use of spreadsheets to generate titration curves, titration of a weak acid with a strong alkali, dibasic acids, weak acid and weak base, and…

  2. Review of Nuclear Heating Measurement by Calorimetry in France and USA

    Science.gov (United States)

    Reynard-Carette, C.; Kohse, G.; Brun, J.; Carette, M.; Volte, A.; Lyoussi, A.

    2018-01-01

    This paper gives a short review of sensors dedicated to measuring nuclear heating rate inside fission reactors in France and USA and especially inside Material Testing Reactors. These sensors correspond to heat flow calorimeters composed of a single calorimetric cell or of two calorimetric cells at least with a reference cell to obtain a differential calorimeter. The aim of this paper is to present the common running principle of these sensors and their own special characteristics through their design, calibration methods, and in-pile measurement techniques, and to describe multi-sensor probes including calorimeters.

  3. A technique for accurate measurements of temperature variations in solution calorimetry and osmometry of actinide complexes

    International Nuclear Information System (INIS)

    Ponkshe, M.R.; Samuel, J.K.

    1982-01-01

    The temperature variations of the order of 10 3- to 10 -4 C are measured by means of matched pair of thermistors and constant current techniques. The factors deciding the sensitivity and accuracy are fully discussed. Also the factors which put restrictions on the practical detection limits are also described. (author)

  4. Enthalpy measurement of lithium meta-titanate by drop calorimetry and its derived heat capacity

    International Nuclear Information System (INIS)

    Ishioka, Rika; Mukai, Keisuke; Terai, Takayuki; Suzuki, Akihiro

    2013-01-01

    Highlights: • Li 2 TiO 3 was synthesized by a neutralizing method. • Enthalpy of Li 2 TiO 3 was measured by a drop calorimeter. • Heat capacity of Li 2 TiO 3 was derived as a function of temperature. -- Abstract: Enthalpy of Li 2 TiO 3 , which was synthesized by a neutralizing method and its Li/Ti ratio was determined to be Li/Ti ratio (mol/mol) = 1.97, was measured by a drop calorimeter, and its heat capacity was derived as a function of temperature. XRD (X-ray diffraction) analysis of the sample before and after the enthalpy measurement indicated no phase change during the measurement and a single phase of Li 2 TiO 3 was observed. The enthalpy data were expressed as H(T) − H(323.17) (J/g) = 2.2 × 10 −5 ·T 2 + 1.4·T + 2.7 × 10 4 /T − 5.6 × 10 2 (373–1273 K), where T is temperature in K. The heat capacity was calculated as C p (J/g K) = 2.2 × 2 × 10 −5 ·T + 1.4–2.7 × 10 4 /T 2 by differentiating the equation by temperature. These equations have accuracy of 3%

  5. Nuclear heating measurements by in-pile calorimetry: prospective works for a microsensor design

    Energy Technology Data Exchange (ETDEWEB)

    Reynard-Carette, C.; Carette, M.; Aguir, K.; Bendahan, M.; Fiorido, T. [Aix Marseille Universite, CNRS, Universite de Toulon, IM2NP UMR 7334, 13397, Marseille (France); Lyoussi, A.; Fourmentel, D.; Villard, J.F. [CEA, DEN, DER, Instrumentation Sensors and Dosimetry Laboratory, Cadarache, F-13108 (France); Barthes, M.; Lanzetta, F.; Layes, G.; Vives, S. [FEMTO-ST, UMR 6174, Departement ENERGIE, Universite de Franche-Comte, 90000, Belfort (France)

    2015-07-01

    Since 2009 works have been performed in the framework of joint research programs between CEA and Aix-Marseille University. The main aim of these programs is to design and develop in-pile instrumentations, advanced calibration procedure and accurate measurement methods in particular for the new Material Testing Reactor (MTR) under construction in the South of France: Jules Horowitz Reactor (JHR). One major sensor is a specific radiometric calorimeter, which was studied out-of-pile from a thermal point of view and in-pile during irradiation campaigns. This sensor type is dedicated to measurements of nuclear heating (energy deposition rate per mass unit induced by interactions between nuclear rays and matter) inside experimental channels of MTRs. This kind of in-pile calorimeter corresponds to heat flux calorimeter exchanging with the external cooling fluid. This thermal running mode allows the establishment of steady thermal conditions inside the sensor to carry out online continuous measurements inside the reactor (core or reflector). Two main types of calorimeters exist. The first type consists of a single cell calorimeter. It is divided into a sample of material to be tested and a jacket instrumented with two thermocouples or a single thermocouple (Gamma Thermometer). The second, called a differential calorimeter, is composed of two superposed twin cells (a measurement cell containing a sample of material, and a reference cell to remove the heating of the cell body) instrumented with four thermocouples and two electrical heaters. Contrary to a single-cell calorimeter, a differential calorimeter allows the compensation of the parasite nuclear heating of the sensor body or jacket. Moreover, it possesses interesting advantages: thanks to the heaters embedded in the cells, three different measurement methods can be applied during irradiations to quantify nuclear heating. The first one is based on the use of out-of-pile calibration curves obtained by generating a heat

  6. Precision tracking and electromagnetic calorimetry towards a measurement of the pion polarisabilities at COMPASS

    Energy Technology Data Exchange (ETDEWEB)

    Dinkelbach, Anna-Maria Elisabeth

    2010-07-20

    In 2004 the COMPASS experiment at CERN SPS measured soft reactions with a beam of negatively charged pions on various nuclear targets. For this measurement, a silicon micro-strip telescope was installed in the target region. For the first time 5 silicon detector stations were operated simultaneously in the COMPASS experiment. A novel method of time calibration, with a clustering algorithm accordingly adapted, and refined alignment corrections were implemented in the analysis software. The spatial resolution of a silicon detector was determined to be 5 - 14 {mu}m and the time resolution 2 - 3 ns. Combining the time information of all stations, a track time resolution of 530 ps from the silicon telescope could be reached. One of the key points of this experiment was the observation of Primakoff events, namely pions scattering off quasi-real photons in the Coulomb field of a heavy nucleus. The production of real photons corresponds to pion Compton scattering in inverse kinematics which is sensitive to the pion polarisabilities {alpha}{sub {pi}} and {beta}{sub {pi}}. Key ingredient for such measurements is a precise knowledge of the performance of the electromagnetic calorimeter. This includes a study of the instabilities of calorimeter cells and an improved reconstruction algorithm. A data-driven shower model was developed, which was used for a timedependent recalibration of the calorimeter. A new cluster refitting method was used to recover position and energy of clusters containing passive or saturated cells and detects double-hit clusters. The latter are important, as the main background to the Primakoff Compton events stems from neutral pions misinterpreted as single-photon hits. The physics analysis comprised the selection of Primakoff events and the necessary steps to obtain the pionic polarisabilities. The measurement was limited by systematic effects of the apparatus also determined within this thesis. (orig.)

  7. Enthalpies of sublimation of ferrocene and nickelocene measured by calorimetry and the method of Langmuir

    Energy Technology Data Exchange (ETDEWEB)

    Rojas, Aaron, E-mail: arojas@cinvestav.mx [Departamento de Quimica del Centro de Investigacion y de Estudios Avanzados del IPN, Av. Instituto Politecnico Nacional 2508, C.P. 07360, Mexico D.F. (Mexico); Vieyra-Eusebio, Maria Teresa [Departamento de Quimica del Centro de Investigacion y de Estudios Avanzados del IPN, Av. Instituto Politecnico Nacional 2508, C.P. 07360, Mexico D.F. (Mexico)

    2011-11-15

    Highlights: > Calorimetric enthalpies of sublimation of ferrocene and nickelocene are supplied. > Sublimation enthalpies of both metallocenes were also obtained by indirect Langmuir's method. > Calorimetric and indirect enthalpies of sublimation are comparable in accuracy and dispersion. > Sublimation enthalpies are congruent with both compounds being monoclinic and isostructural. - Abstract: A quick and accurate methodology that is based on Langmuir's equation and that is developed by utilising a DSC7 device is proposed for the measurement of the enthalpies of sublimation of substances characterised by vapour pressures of approximately 1.0 Pa at room temperature. The procedure was applied to ferrocene and nickelocene; the accuracy and uncertainty associated with the experimental results show that the reliability of the developed indirect method is comparable to the direct calorimetric measurements also performed in this work. Furthermore, the melting data and crystal-phase heat capacities for both metallocenes were calorimetrically measured, whereas the gas-phase heat capacity for each metallic bis(cyclopentadienyl) was theoretically estimated by DFT calculations.

  8. Enthalpies of sublimation of ferrocene and nickelocene measured by calorimetry and the method of Langmuir

    International Nuclear Information System (INIS)

    Rojas, Aaron; Vieyra-Eusebio, Maria Teresa

    2011-01-01

    Highlights: → Calorimetric enthalpies of sublimation of ferrocene and nickelocene are supplied. → Sublimation enthalpies of both metallocenes were also obtained by indirect Langmuir's method. → Calorimetric and indirect enthalpies of sublimation are comparable in accuracy and dispersion. → Sublimation enthalpies are congruent with both compounds being monoclinic and isostructural. - Abstract: A quick and accurate methodology that is based on Langmuir's equation and that is developed by utilising a DSC7 device is proposed for the measurement of the enthalpies of sublimation of substances characterised by vapour pressures of approximately 1.0 Pa at room temperature. The procedure was applied to ferrocene and nickelocene; the accuracy and uncertainty associated with the experimental results show that the reliability of the developed indirect method is comparable to the direct calorimetric measurements also performed in this work. Furthermore, the melting data and crystal-phase heat capacities for both metallocenes were calorimetrically measured, whereas the gas-phase heat capacity for each metallic bis(cyclopentadienyl) was theoretically estimated by DFT calculations.

  9. Mathematical Model for Localised and Surface Heat Flux of the Human Body Obtained from Measurements Performed with a Calorimetry Minisensor

    Science.gov (United States)

    Socorro, Fabiola; Rodríguez de Rivera, Pedro Jesús; Rodríguez de Rivera, Miriam

    2017-01-01

    The accuracy of the direct and local measurements of the heat power dissipated by the surface of the human body, using a calorimetry minisensor, is directly related to the calibration rigor of the sensor and the correct interpretation of the experimental results. For this, it is necessary to know the characteristics of the body’s local heat dissipation. When the sensor is placed on the surface of the human body, the body reacts until a steady state is reached. We propose a mathematical model that represents the rate of heat flow at a given location on the surface of a human body by the sum of a series of exponentials: W(t) = A0 + ∑Aiexp(−t/τi). In this way, transient and steady states of heat dissipation can be interpreted. This hypothesis has been tested by simulating the operation of the sensor. At the steady state, the power detected in the measurement area (4 cm2) varies depending on the sensor’s thermostat temperature, as well as the physical state of the subject. For instance, for a thermostat temperature of 24 °C, this power can vary between 100–250 mW in a healthy adult. In the transient state, two exponentials are sufficient to represent this dissipation, with 3 and 70 s being the mean values of its time constants. PMID:29182567

  10. Mathematical Model for Localised and Surface Heat Flux of the Human Body Obtained from Measurements Performed with a Calorimetry Minisensor.

    Science.gov (United States)

    Socorro, Fabiola; Rodríguez de Rivera, Pedro Jesús; Rodríguez de Rivera, Miriam; Rodríguez de Rivera, Manuel

    2017-11-28

    The accuracy of the direct and local measurements of the heat power dissipated by the surface of the human body, using a calorimetry minisensor, is directly related to the calibration rigor of the sensor and the correct interpretation of the experimental results. For this, it is necessary to know the characteristics of the body's local heat dissipation. When the sensor is placed on the surface of the human body, the body reacts until a steady state is reached. We propose a mathematical model that represents the rate of heat flow at a given location on the surface of a human body by the sum of a series of exponentials: W ( t ) = A ₀ + ∑A i exp( -t / τ i ). In this way, transient and steady states of heat dissipation can be interpreted. This hypothesis has been tested by simulating the operation of the sensor. At the steady state, the power detected in the measurement area (4 cm²) varies depending on the sensor's thermostat temperature, as well as the physical state of the subject. For instance, for a thermostat temperature of 24 °C, this power can vary between 100-250 mW in a healthy adult. In the transient state, two exponentials are sufficient to represent this dissipation, with 3 and 70 s being the mean values of its time constants.

  11. Measuring Hadronic Jets at the ILC - From Particle Flow Calorimetry to the Higgs Self-Coupling

    CERN Document Server

    Hermberg, Benjamin

    2015-01-01

    This work deals with the development of a technical prototype of a highly segmented hadron calorimeter for precision measurements at the future International Linear Col- lider (ILC). The precision measurements at the ILC pose special challenges for both the detector technology as well as for the reconstruction methods. In this thesis two aspects to hadronic final states are examined. The first part deals with a prototype of a highly segmented hadronic calorimeter and the second part with kinematic Fits for the deter- mination of the Higgs self-coupling in decays of the Higgs boson into b quarks. The challenge for the examined prototype of the hadronic calorimeter is the demon- stration of the technical feasibility of a real detector. The ILC is pursuing the Particle Flow concept, as a consequence, it follows for the calorimeter a high granularity and an integrated readout electronics. Two important aspects of the calorimeter prototype are the channel-wise adjustable trigger threshold and the power-pulsing fun...

  12. Measuring hadronic jets at the ILC. From particle flow calorimetry to the Higgs self-coupling

    International Nuclear Information System (INIS)

    Hermberg, Benjamin

    2015-10-01

    This work deals with the development of a technical prototype of a highly segmented hadron calorimeter for precision measurements at the future International Linear Collider (ILC). The precision measurements at the ILC pose special challenges for both the detector technology as well as for the reconstruction methods. In this thesis two aspects to hadronic final states are examined. The first part deals with a prototype of a highly segmented hadronic calorimeter and the second part with kinematic Fits for the determination of the Higgs self-coupling in decays of the Higgs boson into b quarks. The challenge for the examined prototype of the hadronic calorimeter is the demonstration of the technical feasibility of a real detector. The ILC is pursuing the Particle Flow concept, as a consequence, it follows for the calorimeter a high granularity and an integrated readout electronics. Two important aspects of the calorimeter prototype are the channel-wise adjustable trigger threshold and the power-pulsing functionality to minimize the power consumption. In this work it could be shown that with the current readout chip generation, the use of the channel-wise threshold adjustment leads to a shift of the global trigger threshold. Despite of the functionality of the power pulsing, the total current consumption is 30 times above the desired power consumption of 25 μW/channel. In the data of a test beam campaign at CERN 2012 the pedestal was determined, the stability analyzed and specific features of the pedestal identified. In order to achieve the accuracy for the measurement of the Higgs self-coupling, this work examines the applicability of kinematic fits within the framework of the Higgs self-coupling analysis. Basis of the analysis is the lepton channel ZHH→l anti lb anti bb anti b.It could be shown that the use of kinematic fits improves the mass resolution, thus the uncertainty of the cross section is reduced by 18%. The use of a modified fit processor improves the

  13. Direct Measurements of Half-Cycle Reaction Heats during Atomic Layer Deposition by Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Lownsbury, James M. [Department; Gladden, James A. [Department; Campbell, Charles T. [Department; Department; Kim, In Soo [Materials; Martinson, Alex B. F. [Materials

    2017-10-05

    We introduce a new high-temperature adsorption calorimeter that approaches the ideal limit of a heat detector whereby the signal at any time is proportional to the heat power being delivered to the sample and prove its sensitivity for measuring pulse-to-pulse heats of half-reactions during atomic layer deposition (ALD) at 400 K. The heat dynamics of amorphous Al2O3 growth via sequential self-limiting surface reaction of trimethylaluminum (TMA) and H2O is clearly resolved. Calibration enables quantitation of the exothermic TMA and H2O half-reactions with high precision, -343 kJ/mol TMA and -251 kJ/mol H2O, respectively. A time resolution better than 1 ms is demonstrated, allowing for the deconvolution of at least two distinct surface reactions during TMA microdosing. It is further demonstrated that this method can provide the heat of reaction versus extent of reaction during each precursors half-reaction, thus providing even richer mechanistic information on the surface processes involved. The broad applicability of this novel calorimeter is demonstrated through excellent signal-to-noise ratios of less exothermic ALD half-reactions to produce TiO2 and MnO.

  14. Effect of polyglycerol esters additive on palm oil crystallization using focused beam reflectance measurement and differential scanning calorimetry.

    Science.gov (United States)

    Saw, M H; Hishamuddin, E; Chong, C L; Yeoh, C B; Lim, W H

    2017-01-01

    The effect of 0.1-0.7% (w/w) of polyglycerol esters (PGEmix-8) on palm oil crystallization was studied using focused beam reflectance measurement (FBRM) to analyze the in-line changes of crystal size distribution during the crystallization. FBRM results show that 0.1-0.5% (w/w) of PGEmix-8 did not significantly affect nucleation but slightly retarded crystal growth. The use of 0.7% (w/w) additive showed greater heterogeneous nucleation compared to those with lower dosages of additive. Crystal growth was also greatly reduced when using 0.7% (w/w) dosage. The morphological study indicated that the palm oil crystals were smaller and more even in size than when more additive was added. Isothermal crystallization studies using differential scanning calorimetry (DSC) showed increased inhibitory effects on palm oil crystal growth with increasing concentration of PGEmix-8. These results imply that PGEmix-8 is a nucleation enhancing and crystal growth retarding additive in palm oil crystallization at 0.7% (w/w) dosage. Copyright © 2016 The Author(s). Published by Elsevier Ltd.. All rights reserved.

  15. base titration

    African Journals Online (AJOL)

    The pH and temperature in the titration cell were monitored using single junction electrodes and platinum resistance thermometers, respectively. A constant supply of nitrogen gas in the cell was used to maintain inert conditions. The whole set up was interfaced with a computer for easy data acquisition. It was observed that ...

  16. Automated uranium titration system

    International Nuclear Information System (INIS)

    Takahashi, M.; Kato, Y.

    1983-01-01

    An automated titration system based on the Davies-Gray method has been developed for accurate determination of uranium. The system consists of a potentiometric titrator with precise burettes, a sample changer, an electronic balance and a desk-top computer with a printer. Fifty-five titration vessels are loaded in the sample changer. The first three contain the standard solution for standardizing potassium dichromate titrant, and the next two and the last two contain the control samples for data quality assurance. The other forty-eight measurements are carried out for sixteen unknown samples. Sample solution containing about 100 mg uranium is taken in a titration vessel. At the pretreatment position, uranium (VI) is reduced to uranium (IV) by iron (II). After the valency adjustment, the vessel is transferred to the titration position. The rate of titrant addition is automatically controlled to be slower near the end-point. The last figure (0.01 mL) of the equivalent titrant volume for uranium is calculated from the potential change. The results obtained with this system on 100 mg uranium gave a precision of 0.2% (RSD,n=3) and an accuracy of better than 0.1%. Fifty-five titrations are accomplished in 10 hours. (author)

  17. A quantitative mechanistic description of Ni, Zn and Ca sorption on Na-Montmorillonite. Part I: Physico-chemical characterisation and titration measurements

    International Nuclear Information System (INIS)

    Baeyens, B.; Bradbury, M.H.

    1995-07-01

    The work presented in this report is primarily concerned with characterisation studies and titration measurements on conditioned Na-montmorillonite. The starting material, SWy-1 Na-montmorillonite (Crook County, Wyoming, USA), contains background metal impurities, soluble salts and sparingly soluble minerals which can influence titration and sorption measurements and thereby lead to difficulties in the interpretation of the data. A conditioning procedure is described which yielded a purified clay material in the homoionic sodium form with a particle size 4 . The reasons for choosing a batch method, coupled with back titration of the supernatant solutions, instead of a continuous procedure, are fully discussed. Chemical analyses data for the supernatant solutions are presented in detail. The influence of background impurities, not removed by the conditioning, and cation exchange processes on the form of the titration curves were investigates. Net Na-montmorillonite titration curves at two different ionic strengths were derived which are considered to reflect only the acid/base behaviour of ≡SOH type surface sites. The acid end point in the titration data was used to estimate an ≡SOH site capacity of 0.08 moles per kg conditioned Na-montmorillonite. (author) 8 figs., 19 tabs., refs

  18. Breath test measurements in combination with indirect calorimetry for estimation of 13C-leucine oxidation in mink (Mustela vison)

    DEFF Research Database (Denmark)

    Tauson, Anne-Helene; Ali, Abdalla; Kanska, Katarzyna

    2000-01-01

    Gas exchange measurements by means of indirect calorimetry can be used to calculate quantitative substrate oxidation. The results represents average net oxidation values (substrate disappearance rate), but they cannot describe the dynamics of the oxidation processes. Breath test measurements...... was significant (P=0.03), values generally being lower during fasting, indicating a lower rate of leucine oxidation. It was concluded that the present results clearly demonstrate differences in rate of oxidation of leucine between fed and fasted animals....... to feeding and fasting. Twelve 1-year-old male mink (Mustela vison) were measured in each five consecutive periods by means of indirect calorimetry and simultaneous breath test. In Periods 1, 3 and 5, each lasting 3 days, the animals were fed ad libitum and Periods 2 and 4 were fasting periods, each of 48 h...

  19. SU-E-T-410: Fringe Stability and Phase Shift Measurements in a Michelson Interferometer for Optical Calorimetry

    International Nuclear Information System (INIS)

    Flores-Martinez, E; Malin, M; DeWerd, L

    2014-01-01

    Purpose: To identify the variables limiting the resolution of a Michelson interferometer used to measure phase shifts (PS) in water as part of a radiometric calorimeter. Methods: We investigated the output stability of a He-Ne laser and a laser diode. The short and long term stability of the fringe pattern in a Michelson interferometer was tested with different types of lasers, thermal insulation arrangements, damping systems and optical mounts to optimize system performance. PS were induced by electrically heating water in a 1 cm quartz cuvette located in one of the interferometer arms. The PS was calculated from fringe intensity changes and compared to a calculated PS using thermocouple-measured temperature changes in the water. Results: The intensity of the laser diode is more stable, but the gas laser’s profile is more suitable for fringe analysis and has better temporal coherence. The laser requires a warm-up time of 4 hours before its output is stabilized (SNR>95). The fringe’s stability strongly depends on the thermal insulation. When the interferometer is exposed to ambient temperature swings of 0.7 K, it is not possible to stabilize the fringe pattern. Enclosing the system in a 2.5 cm-thick Styrofoam box improves the SNR, but further insulation will be needed to increase the SNR above 50. High frequency noise is significantly reduced by damping the system.Inducing a temperature rise in water, starting at 299 K, the average temperature increase for a 2π PS is 0.29 ± 0.02 K and the proportionality constant is -21.1 ± 0.8 radians/K. This is 5.8% lower than the calculated value using the thermocouple. Conclusion: Interferometric PS measurements of temperature may provide an alternative to thermistors for water calorimetry. The resolution of the current prototype is limited by ambient temperature stability. Calculated and measured thermally-induced PS in water agreed to within 5.8%

  20. Application of titration methods for measuring the contents of ammonium nitrogen and volatile fatty acids in agricultural biogas plants.

    Science.gov (United States)

    Piątek, Michał; Lisowski, Aleksander; Lisowska, Barbara

    2017-12-20

    The aim of our research was to assess a relatively new method of estimating ammonium nitrogen concentration in anaerobic digestion of plant substrates. We analysed our own data, received from the anaerobic digestion of maize silage (PM), as well as data published by Purser et al. (2014) who measured energy crops and slurry (ECS), and food waste (FW). In our study, the process was monitored for VFA content that was determined by gas chromatography, and for the content of ammonium nitrogen determined using the HACH LANGE LCK 303 cuvette test. We created polynomial regression models that bind the content of ammonium nitrogen with the volume of H 2 SO 4 used to titrate the sample from initial pH to pH 5. To estimate parameters of model, the PM dataset was used. The obtained models were positively validated using ECS and FW datasets. Our results confirmed the effectiveness of the Purser et al. method with an average absolute error of less than 223mgl -1 of the VFA concentration, which was approximately 20-times less than the level that caused inhibition. In conclusion, we can affirm the suitability of using titration methods to assess the ammonium nitrogen content of bioreactors with a stable composition. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Calorimetry at industrial electron accelerators

    DEFF Research Database (Denmark)

    Miller, Arne; Kovacs, A.

    1985-01-01

    Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials such as grap......Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials...

  2. Exploration of Energy Metabolism in the Mouse Using Indirect Calorimetry: Measurement of Daily Energy Expenditure (DEE) and Basal Metabolic Rate (BMR).

    Science.gov (United States)

    Meyer, Carola W; Reitmeir, Peter; Tschöp, Matthias H

    2015-09-01

    Current comprehensive mouse metabolic phenotyping involves studying energy balance in cohorts of mice via indirect calorimetry, which determines heat release from changes in respiratory air composition. Here, we describe the measurement of daily energy expenditure (DEE) and basal metabolic rate (BMR) in mice. These well-defined metabolic descriptors serve as meaningful first-line read-outs for metabolic phenotyping and should be reported when exploring energy expenditure in mice. For further guidance, the issue of appropriate sample sizes and the frequency of sampling of metabolic measurements is also discussed. Copyright © 2015 John Wiley & Sons, Inc.

  3. Isothermal titration calorimetry of sorption processes. A promising approach

    Energy Technology Data Exchange (ETDEWEB)

    Jordan, Norbert; Foerstendorf, Harald [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Surface Processes; Drobot, B. [Technische Univ. Dresden (Germany); Fahmy, Karim [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Biophysics; Reder, Christian

    2017-06-01

    As a consequence of nuclear waste disintegration heat, elevated temperatures in the near field may influence radionuclide retention significantly. However, there is a nearly complete lack of spectroscopic investigations of sorption processes at elevated temperatures. In addition, experimental data on free Gibbs energy (Δ{sub R}G), enthalpy (Δ{sub R}H) and entropy (Δ{sub R}S) of reactions of most radionuclides including fission products such as {sup 79}Se are sparse. Using the Se(IV)/hematite system, we show that microcalorimetry can provide these thermodynamic parameters with high accuracy and in a manner that allows studying various radionuclides.

  4. Iodine losses during Winkler titrations

    Science.gov (United States)

    Knapp, George P.; Stalcup, Marvel C.; Stanley, Robert J.

    1991-01-01

    An experiment designed to measure iodine loss during the aliquot version of the Winkler titration for dissolved oxygen in seawater shows that 0.01-0.03 ml l -1 equivalent oxygen is lost at typical oceanic concentrations in the method presently used. A standardization technique, which mimics that employed during the titration of seawater samples, compensates for this iodine loss throughout the oceanic range. This result, contradicting an earlier report by GREEN and CARRITT (1966, Analyst, 91, 207-208), demonstrates that the whole-bottle method of oxygen titration is not to be preferred over the aliquot method.

  5. The effect of feeding on CO2 production and energy expenditure in ponies measured by indirect calorimetry and the 13C-bicarbonate technique

    DEFF Research Database (Denmark)

    Jensen, Rasmus Bovbjerg; Kyrstein, T. D.; Junghans, P

    2015-01-01

    -labelled sodium bicarbonate (NaH(13)CO(3)). The ponies were fed haylage 3 h before (T(-3)), simultaneously with (T(0)) or 3 h after (T(+3)) administration of (13)C-bicarbonate. The CO(2) produced and O(2) consumed by the ponies were measured for 6 h with both administration routes of (13)C-bicarbonate......Energy expenditure (EE) can be estimated based on respiratory gas exchange measurements, traditionally done in respiration chambers by indirect calorimetry (IC). However, the (13)C-bicarbonate technique ((13)C-BT) might be an alternative minimal invasive method for estimation of CO(2) production......)) compared with when no feed was available (T -3) during measurements. In conclusion, this study showed that feeding time affects the RF and measurements of CO(2) production and EE. This should be considered when the (13)C-BT is used in the field. IV administration of (13)C-bicarbonate is recommended...

  6. Tracer-monitored flow titrations.

    Science.gov (United States)

    Sasaki, Milton K; Rocha, Diogo L; Rocha, Fábio R P; Zagatto, Elias A G

    2016-01-01

    The feasibility of implementing tracer-monitored titrations in a flow system is demonstrated. A dye tracer is used to estimate the instant sample and titrant volumetric fractions without the need for volume, mass or peak width measurements. The approach was applied to spectrophotometric flow titrations involving variations of sample and titrant flow-rates (i.e. triangle programmed technique) or concentration gradients established along the sample zone (i.e. flow injection system). Both strategies required simultaneous monitoring of two absorbing species, namely the titration indicator and the dye tracer. Mixing conditions were improved by placing a chamber with mechanical stirring in the analytical path aiming at to minimize diffusional effects. Unlike most of flow-based titrations, the innovation is considered as a true titration, as it does not require a calibration curve thus complying with IUPAC definition. As an application, acidity evaluation in vinegars involving titration with sodium hydroxide was selected. Phenolphthalein and brilliant blue FCF were used as indicator and dye tracer, respectively. Effects of sample volume, titrand/titrant concentrations and flow rates were investigated aiming at improved accuracy and precision. Results were reliable and in agreement with those obtained by a reference titration procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Automatic titrator for high precision plutonium assay

    International Nuclear Information System (INIS)

    Jackson, D.D.; Hollen, R.M.

    1986-01-01

    Highly precise assay of plutonium metal is required for accountability measurements. We have developed an automatic titrator for this determination which eliminates analyst bias and requires much less analyst time. The analyst is only required to enter sample data and start the titration. The automated instrument titrates the sample, locates the end point, and outputs the results as a paper tape printout. Precision of the titration is less than 0.03% relative standard deviation for a single determination at the 250-mg plutonium level. The titration time is less than 5 min

  8. Theory of calorimetry

    CERN Document Server

    Zielenkiewicz, Wojciech

    2004-01-01

    The purpose of this book is to give a comprehensive description of the theoretical fundamentals of calorimetry. The considerations are based on the relations deduced from the laws and general equations of heat exchange theory and steering theory.

  9. Calorimetry at industrial electron accelerators

    DEFF Research Database (Denmark)

    Miller, Arne; Kovacs, A.

    1985-01-01

    Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials such as grap......Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials...... such as graphite and aluminium have been used. These materials offer advantages of simpler construction and higher sensitivity. Dose estimates using these different types of calorimeters differ by ~5%, and the possible reasons for these discrepancies are discussed...

  10. Calorimetry for the SSC

    International Nuclear Information System (INIS)

    Gordon, H.A.; Grannis, P.D.

    1984-01-01

    The activities related to calorimetry at Snowmass took place in three main areas. These were: (1) The performance criteria for SSC calorimetry, including the requirements on hermeticity, shower containment, segmentation and time resolution. The use of calorimetric means of particle identification was studied. (2) The study of triggering methods using calorimeter energy, angle and timing information. (3) A review of a wide variety of calorimeter materials for absorber and sampling, as well as several means of obtaining the readout of the energy deposits. 48 references, 10 figures, 1 table

  11. Calorimetry for the SSC

    Energy Technology Data Exchange (ETDEWEB)

    Gordon, H.A.; Grannis, P.D.

    1984-01-01

    The activities related to calorimetry at Snowmass took place in three main areas. These were: (1) The performance criteria for SSC calorimetry, including the requirements on hermeticity, shower containment, segmentation and time resolution. The use of calorimetric means of particle identification was studied. (2) The study of triggering methods using calorimeter energy, angle and timing information. (3) A review of a wide variety of calorimeter materials for absorber and sampling, as well as several means of obtaining the readout of the energy deposits. 48 references, 10 figures, 1 table.

  12. Theoretical considerations and a simple method for measuring alkalinity and acidity in low-pH waters by gran titration

    Science.gov (United States)

    Barringer, J.L.; Johnsson, P.A.

    1996-01-01

    Titrations for alkalinity and acidity using the technique described by Gran (1952, Determination of the equivalence point in potentiometric titrations, Part II: The Analyst, v. 77, p. 661-671) have been employed in the analysis of low-pH natural waters. This report includes a synopsis of the theory and calculations associated with Gran's technique and presents a simple and inexpensive method for performing alkalinity and acidity determinations. However, potential sources of error introduced by the chemical character of some waters may limit the utility of Gran's technique. Therefore, the cost- and time-efficient method for performing alkalinity and acidity determinations described in this report is useful for exploring the suitability of Gran's technique in studies of water chemistry.

  13. Calorimetry at the SSC

    International Nuclear Information System (INIS)

    Wigmans, R.

    1988-01-01

    The state of the art, and the present understanding of the basic limitations in hadron calorimetry, are briefly described. The various options for SSC calorimeters are discussed, and the R ampersand D needed for the ones that look most promising is outlined. The most promising candidates are (1) lead/scintillating fibers and (2) lead (or uranium)/TMS (or other warm liquids)

  14. Calorimetry at the SSC

    International Nuclear Information System (INIS)

    Wigmans, R.

    1987-09-01

    The state of the art, and our present understanding of the basic limitations in hadron calorimetry, are briefly described. The various options for SSC calorimeters are discussed, and the R and D needed for the ones that look most promising is outlined. 13 refs.; 8 figs

  15. Seventy Years of Calorimetry

    Science.gov (United States)

    Wigmans, Richard

    2017-11-01

    In this opening talk of the CALOR 2016 conference, I briefly review some milestones in the history of calorimetry as a detection technique in particle physics. I also discuss common misconceptions, which are unfortunately widespread, and give you my personal outlook on the future.

  16. Calorimetry for dose measurement at electron accelerators in the 80-120 keV energy range

    DEFF Research Database (Denmark)

    Helt-Hansen, J.; Miller, A.; Duane, S.

    2005-01-01

    Calorimeters for dose measurement at low-energy electron accelerator energies (80-120 keV) are described. Three calorimeters with different characteristics were designed and their dose response and measurement uncertainties were characterized. The heated air between the beam exit window...... and the calorimeter absorber influences significantly the response of the calorimeter and a thermal model was applied to quantify this effect. All three calorimeters are capable of measuring absolute dose, and can thus be used for calibration of other dosimeters. (C) 2005 Elsevier Ltd. All rights reserved....

  17. Enthalpy measurement using calorimetry shows a significant difference in potential energy between the active and latent conformations of PAI-1.

    Science.gov (United States)

    Sherman, Westley A; Blouse, Grant E; Perron, Michel J; Tran, Timothy; Shore, Joseph D; Gafni, Ari

    2005-02-01

    A central feature of the serpin inhibition mechanism is insertion of the reactive center loop into the central beta-sheet (beta-sheet A). This insertion also occurs when the reactive center loop is cleaved without protease inhibition. Using this effect, we have measured the enthalpy (DeltaH) of loop cleavage and insertion for plasminogen activator inhibitor 1 (PAI-1) as -38 kcal/mol. Because loop insertion can be blocked by incorporating a peptide into the central beta-sheet, it was possible to assign -7 kcal/mol to loop cleavage and -31 kcal/mol to loop insertion. These values are lower than values reported for the serpins alpha 1 -proteinase inhibitor and antithrombin of -53 to -63 kcal/mol, respectively, for loop insertion with negligible enthalpy for loop cleavage. A free energy difference of -9 kcal/mol has been reported between the active and spontaneously loop inserted "latent forms" of PAI-1, which is significantly smaller in magnitude than the -31 kcal/mol of enthalpy we measured for loop insertion. Because the enthalpy should relate closely to those regions of PAI-1 that have moved to lower potential energy, a difference distance matrix is presented that identifies regions of PAI-1 that move during loop insertion.

  18. TH-CD-201-09: High Spatial Resolution Absorbed Dose to Water Measurements Using Optical Calorimetry in Megavoltage External Beam Therapy

    Energy Technology Data Exchange (ETDEWEB)

    Flores-Martinez, E; DeWerd, L [School of Medicine and Public Health, University of Wisconsin-Madison, Madison, WI (United States); Radtke, J [University of Wisconsin, Madison, WI (United States)

    2016-06-15

    Purpose: To develop and implement a high spatial resolution calorimeter methodology to measure absorbed dose to water (ADW) using phase shifts (PSs) of light passing through a water phantom and to compare measurements with theoretical calculations. Methods: Radiation-induced temperature changes were measured using the PSs of a He-Ne laser beam passing through a (10×10×10) cm{sup 3} water phantom. PSs were measured using a Michelson interferometer and recording the time-dependent fringe patterns on a CCD camera. The phantom was positioned at the center of the radiation field. A Varian 21EX was used to deliver 500 MU from a 9 MeV beam using a (6×6) cm{sup 2} cone. A 127cm SSD was used and the PSs were measured at depths ranging from of 1.90cm to 2.10cm in steps of 0.05cm by taking profiles at the corresponding rows across the image. PSs were computed by taking the difference between pre- and post-irradiation image frames and then measuring the amplitude of the resulting image profiles. An amplitude-to-PS calibration curve was generated using a piezoelectric transducer to mechanically induce PSs between 0.05 and 1.50 radians in steps of 0.05 radians. The temperature dependence of the refractive index of water at 632.8nm was used to convert PSs to ADW. Measured results were compared with ADW values calculated using the linac output calibration and commissioning data. Results: Milli-radian resolution in PS measurement was achieved using the described methodology. Measured radiation-induced PSs ranged from 0.10 ± 0.01 to 0.12 ± 0.01 radians at the investigated depths. After converting PSs to ADW, measured and calculated ADW values agreed within the measurement uncertainty. Conclusion: This work shows that interferometer-based calorimetry measurements are capable of achieving sub-millimeter resolution measuring 2D temperature/dose distributions, which are particularly useful for characterizing beams from modalities such as SRS, proton therapy, or microbeams.

  19. Measuring melting capacity with calorimetry

    OpenAIRE

    Betten, Linda

    2014-01-01

    Road salting is an important aspect of winter maintenance. There has been an increase in the usage of salt in later years to keep the road safe and accessible. It is a desire to reduce the amount of salt due to environmental aspects. To achieve better practices for winter maintenance it is necessary to obtain more knowledge about the different properties of salt. The motivation for this thesis is to develop a better method for determining the melting capacity for salt, which is an important p...

  20. Water calorimetry: The heat defect

    International Nuclear Information System (INIS)

    Klassen, N.V.; Ross, C.K.

    1997-01-01

    Domen developed a sealed water calorimeter at NIST to measure absorbed dose to water from ionizing radiation. This calorimeter exhibited anomalous behavior using water saturated with gas mixtures of H 2 O 2 . Using computer simulations of the radiolysis of water, the authors show that the observed behavior can be explained if, in the gas mixtures, the amount-of-substance of H 2 and of O 2 differed significantly from 50%. The authors also report the results of simulations for other dilute aqueous solutions that are used for water calorimetry--pure water, air-saturated water, and H 2 -saturated water. The production of H 2 O 2 was measured for these aqueous solutions and compared to simulations. The results indicate that water saturated with a gas mixture containing an amount-of-substance of H 2 of 50% and of O 2 of 50% is suitable for water calorimetry if the water is stirred and is in contact with a gas space of similar volume. H 2 -saturated water does not require a gas space but O 2 contamination must be guarded against. The lack of a scavenger for OH radicals in pure water means that, depending on the water purity, some pure water might require a large priming dose to remove reactive impurities. The experimental and theoretical problems associated with air-saturated water and O 2 -saturated water in water calorimeters are discussed

  1. Scintillating-fibre calorimetry

    International Nuclear Information System (INIS)

    Livan, M.; Vercesi, V.; Wigmans, R.

    1995-01-01

    In the past decade, calorimetry based on scintillating plastic fibres as active elements was developed from a conceptual idea to a mature detector technology, which is nowadays widely applied in particle physics experiments. This development and the performance characteristics of representative calorimeters, both for the detection of electromagnetic and hadronic showers, are reviewed. We also discuss new information on shower development processes in dense matter and its application to calorimetric principles that has emerged from some very thorough studies that were performed in the framework of this development. (orig.)

  2. Simple and Automated Coulometric Titration of Acid Using Nonisolated Electrodes

    Science.gov (United States)

    Kuntzleman, Thomas S.; Kenney, Joshua B.; Hasbrouck, Scott; Collins, Michael J.; Amend, John R.

    2011-01-01

    Coulometric titrations involve the quantification of analyte by measurements of current and time. In most coulometric titrations, the anode and cathode are placed in isolated cells that are connected by a salt bridge. By contrast, the experiments described here involve coulometric titrations (of acidic protons in solution) using a silver anode and…

  3. Thermodynamic signatures of fragment binding: Validation of direct versus displacement ITC titrations.

    Science.gov (United States)

    Rühmann, Eggert; Betz, Michael; Fricke, Marie; Heine, Andreas; Schäfer, Martina; Klebe, Gerhard

    2015-04-01

    Detailed characterization of the thermodynamic signature of weak binding fragments to proteins is essential to support the decision making process which fragments to take further for the hit-to-lead optimization. Isothermal titration calorimetry (ITC) is the method of choice to record thermodynamic data, however, weak binding ligands such as fragments require the development of meaningful and reliable measuring protocols as usually sigmoidal titration curves are hardly possible to record due to limited solubility. Fragments can be titrated either directly under low c-value conditions (no sigmoidal curve) or indirectly by use of a strong binding ligand displacing the pre-incubated weak fragment from the protein. The determination of Gibbs free energy is reliable and rather independent of the applied titration protocol. Even though the displacement method achieves higher accuracy, the obtained enthalpy-entropy profile depends on the properties of the used displacement ligand. The relative enthalpy differences across different displacement experiments reveal a constant signature and can serve as a thermodynamic fingerprint for fragments. Low c-value titrations are only reliable if the final concentration of the fragment in the sample cell exceeds 2-10 fold its K(D) value. Limited solubility often prevents this strategy. The present study suggests an applicable protocol to characterize the thermodynamic signature of protein-fragment binding. It shows however, that such measurements are limited by protein and fragment solubility. Deviating profiles obtained by use of different displacement ligands indicate that changes in the solvation pattern and protein dynamics most likely take influence on the resulting overall binding signature. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Characterization of dynamics in complex lyophilized formulations: I. Comparison of relaxation times measured by isothermal calorimetry with data estimated from the width of the glass transition temperature region.

    Science.gov (United States)

    Chieng, Norman; Mizuno, Masayasu; Pikal, Michael

    2013-10-01

    The purposes of this study are to characterize the relaxation dynamics in complex freeze dried formulations and to investigate the quantitative relationship between the structural relaxation time as measured by thermal activity monitor (TAM) and that estimated from the width of the glass transition temperature (ΔT(g)). The latter method has advantages over TAM because it is simple and quick. As part of this objective, we evaluate the accuracy in estimating relaxation time data at higher temperatures (50 °C and 60 °C) from TAM data at lower temperature (40 °C) and glass transition region width (ΔT(g)) data obtained by differential scanning calorimetry. Formulations studied here were hydroxyethyl starch (HES)-disaccharide, HES-polyol, and HES-disaccharide-polyol at various ratios. We also re-examine, using TAM derived relaxation times, the correlation between protein stability (human growth hormone, hGH) and relaxation times explored in a previous report, which employed relaxation time data obtained from ΔT(g). Results show that most of the freeze dried formulations exist in single amorphous phase, and structural relaxation times were successfully measured for these systems. We find a reasonably good correlation between TAM measured relaxation times and corresponding data obtained from estimates based on ΔT(g), but the agreement is only qualitative. The comparison plot showed that TAM data are directly proportional to the 1/3 power of ΔT(g) data, after correcting for an offset. Nevertheless, the correlation between hGH stability and relaxation time remained qualitatively the same as found with using ΔT(g) derived relaxation data, and it was found that the modest extrapolation of TAM data to higher temperatures using ΔT(g) method and TAM data at 40 °C resulted in quantitative agreement with TAM measurements made at 50 °C and 60 °C, provided the TAM experiment temperature, is well below the Tg of the sample. Copyright © 2013 Elsevier B.V. All rights

  5. Calorimetry at a Future Linear Collider

    CERN Document Server

    AUTHOR|(CDS)2090195; Marshall, John

    This thesis describes the optimisation of the calorimeter design for collider experiments at the future Compact LInear Collider (CLIC) and the International Linear Collider (ILC). The detector design of these experiments is built around high-granularity Particle Flow Calorimetry that, in contrast to traditional calorimetry, uses the energy measurements for charged particles from the tracking detectors. This can only be realised if calorimetric energy deposits from charged particles can be separated from those of neutral particles. This is made possible with fine granularity calorimeters and sophisticated pattern recognition software, which is provided by the PandoraPFA algorithm. This thesis presents results on Particle Flow calorimetry performance for a number of detector configurations. To obtain these results a new calibration procedure was developed and applied to the detector simulation and reconstruction to ensure optimal performance was achieved for each detector configuration considered. This thesis a...

  6. The use of calorimetry for plutonium assay

    International Nuclear Information System (INIS)

    Mason, J.A.

    1982-12-01

    Calorimetry is a technique for measuring the thermal power of heat-producing substances. The technique may be applied to the measurement of plutonium-bearing materials which evolve heat as a result of alpha and beta decay. A calorimetric measurement of the thermal power of a plutonium sample, combined with a knowledge or measurement of the plutonium isotopic mass ratios of the sample provides a convenient and accurate, non-destructive measure of the total plutonium mass of the sample. The present report provides a description, and an assessment of the calorimetry technique applied to the assay of plutonium-bearing materials. Types and characteristics of plutonium calorimeters are considered, as well as calibration and operating procedures. The instrumentation used with plutonium calorimeters is described and the use of computer control for calorimeter automation is discussed. A critical review and assessment of plutonium calorimetry literature since 1970 is presented. Both fuel element and plutonium-bearing material calorimeters are considered. The different types of plutonium calorimeters are evaluated and their relative merits are discussed. A combined calorimeter and gamma-ray measurement assay system is considered. The design principles of plutonium assay calorimeters are considered. An automatic, computer-based calorimeter control system is proposed in conjunction with a general plutonium assay calorimeter design. (author)

  7. Filtrates & Residues: Olfactory Titration.

    Science.gov (United States)

    Wood, John T.; Eddy, Roberta M.

    1996-01-01

    Presents an experiment that uses a unique acid-base indicator--the odor of raw onion--to indicate the end point of the titration of sodium hydroxide with hydrochloric acid. Allows the student to detect the completion of the neutralization reaction by olfaction rather than sight. (JRH)

  8. ''Titration'' polymerization of monovinylacetylene

    NARCIS (Netherlands)

    Mavinkurve, A; Visser, S; vandenBroek, W; Pennings, AJ

    1996-01-01

    A polymer consisting of a saturated carbon backbone with pendent acetylenic groups was prepared from monovinylacetylene. A titration was performed between the monomer and tertiary butyllithium, its lithiating agent. The charge transfer complex formed between the solvent THF and the tertiary

  9. Simultaneous estimation of a binary mixture of a weak acid and a strong acid by volumetric titration and pH measurement

    International Nuclear Information System (INIS)

    Karmakar, Sanat; Mallika, C.; Kamachi Mudali, U.

    2012-01-01

    High level liquid waste (HLLW) generated in the aqueous reprocessing of spent nuclear fuels for the separation of uranium and plutonium by PUREX process, comprises the fission and corrosion products in 4 M nitric acid. Reduction in waste volume is accomplished by destroying the acidity of the waste solution from 4 to less than 2 M by treating it with formaldehyde and subsequent concentration by evaporation. In the denitration by HCHO, nitric acid in the waste solution is reduced to NOx and water via nitrous acid as the intermediate product: whereas formaldehyde is oxidized to formic acid which is converted to CO 2 and H 2 O subsequently. The reaction is highly exothermic and the release of all gaseous products may lead to uncontrollable process conditions. Hence, for the safe operation, it is desirable to estimate the concentration of residual formic acid as well as nitric acid in the product stream as a function of time. The acidity in the feed solution is 4 M and the concentration of HNO 3 in the product solution is in the range 1- 4 M. Since the formic acid generated during the reaction will be consumed immediately, the concentration of residual acid will be in the range 0.05-0.5 M. A simultaneous titration method based on pH measurement and volumetric analysis has been developed in the present work for the quantitative determination of the weak acid (HCOOH)with known pKa value and the strong acid (HNO 3 ) in the binary mixture

  10. WA80 BGO calorimetry electronics

    International Nuclear Information System (INIS)

    Wintenberg, A.L.; Britton, C.L. Jr.; Ericson, M.N.; Maples, R.A.; Young, G.R.; Awes, T.C.

    1991-01-01

    This paper describes instrumentation designed for BGO scintillator-based calorimetry of particles covering a very wide range of energies (from less than 50 MeV to 50 GeV). The instrumentation was designed to have a measurement accuracy of 0.1% over as much of the energy range as possible so the energy resolution of BGO would be the limiting factor. Two 1.5-cm 2 photodiodes were used per 2.5 cm x 2.5 cm x 25 cm BGO crystal. Both a charge-sensitive preamplifier and a pulse processor were developed specifically for the needs of the WA80 experiment. The preamplifier was designed for high detector capacitance (100 to 700 pF), low integral and differential non-linearity and low power consumption (200 mW). The pulse processor is a time-invariant shaping amplifier with integral peak-detect-and-hold and automatic gain selection circuits. The amplifier use quasi-triangular shaping with 4 μs peaking time, and the hold circuit is gated with a fast first level trigger. The system has more than 20 bits of effective resolution when used with an external 12-bit ADC. Results from beam tests at CERN are presented. 6 refs., 5 figs., 1 tab

  11. Calorimetry end-point predictions

    International Nuclear Information System (INIS)

    Fox, M.A.

    1981-01-01

    This paper describes a portion of the work presently in progress at Rocky Flats in the field of calorimetry. In particular, calorimetry end-point predictions are outlined. The problems associated with end-point predictions and the progress made in overcoming these obstacles are discussed. The two major problems, noise and an accurate description of the heat function, are dealt with to obtain the most accurate results. Data are taken from an actual calorimeter and are processed by means of three different noise reduction techniques. The processed data are then utilized by one to four algorithms, depending on the accuracy desired to determined the end-point

  12. Plutonium titration by controlled potential coulometry

    International Nuclear Information System (INIS)

    Leguay, N.

    2011-01-01

    The LAMMAN (Nuclear Materials Metrology Laboratory) is the support laboratory of the CETAMA (Analytical Method Committee), whose two main activities are developing analytic methods, and making and characterizing reference materials. The LAMMAN chose to develop the controlled potential coulometry because it is a very accurate analytical technique which allows the connection between the quantity of element electrolysed to the quantity of electricity measured thanks to the Faraday's law: it does not require the use of a chemical standard. This method was first used for the plutonium titration and was developed in the Materials Analysis and Metrology Laboratory (LAMM), for upgrading its performances and developing it to the titration of other actinides. The equipment and the material used were developed to allow the work in confined atmosphere (in a glove box), with all the restrictions involved. Plutonium standard solutions are used to qualify the method, and in particular to do titrations with an uncertainty better than 0.1 %. The present study allowed making a bibliographic research about controlled potential coulometry applied to the actinides (plutonium, uranium, neptunium, americium and curium). A full procedure was written to set all the steps of plutonium titration, from the preparation of samples to equipments storage. A method validation was done to check the full procedure, and the experimental conditions: working range, uncertainty, performance... Coulometric titration of the plutonium from pure solution (without interfering elements) was developed to the coulometric titration of the plutonium in presence of uranium, which allows to do accurate analyses for the analyses of some parts of the reprocessing of the spent nuclear fuel. The possibility of developing this method to other actinides than plutonium was highlighted thanks to voltammetric studies, like the coulometric titration of uranium with a working carbon electrode in sulphuric medium. (author)

  13. Automated titration method for use on blended asphalts

    Science.gov (United States)

    Pauli, Adam T [Cheyenne, WY; Robertson, Raymond E [Laramie, WY; Branthaver, Jan F [Chatham, IL; Schabron, John F [Laramie, WY

    2012-08-07

    A system for determining parameters and compatibility of a substance such as an asphalt or other petroleum substance uses titration to highly accurately determine one or more flocculation occurrences and is especially applicable to the determination or use of Heithaus parameters and optimal mixing of various asphalt stocks. In a preferred embodiment, automated titration in an oxygen gas exclusive system and further using spectrophotometric analysis (2-8) of solution turbidity is presented. A reversible titration technique enabling in-situ titration measurement of various solution concentrations is also presented.

  14. Fiber optic calorimetry

    International Nuclear Information System (INIS)

    Rudy, C.; Bayliss, S.; Bracken, D.; Bush, J.; Davis, P.

    1998-01-01

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using fiber for heat-flow measurements of special nuclear material. This calorimeter uses piezoelectric-generated phase-carrier modulation with subsequent electronic signal processing to allow phase shifts as small as 1 microradian (μrad) to be measured. The sensing element consists of 21-m lengths of single-mode optical fiber wrapped around sample and reference chambers. The sensitivity of the calorimeter was determined to be 74 radians (rad) of phase shift per milliwatt of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  15. Fiber optic calorimetry

    International Nuclear Information System (INIS)

    Rudy, C.R.; Bayliss, S.C.; Bracken, D.S.; Bush, I.J.; Davis, P.G.

    1998-01-01

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using optical fibers for heat-flow measurements of special nuclear material. This calorimeter uses piezoelectric-generated phase-carrier modulation with subsequent electronic signal processing to allow phase shifts as small as 1 microrad to be measured. The sensing element consists of 21-m lengths of single-mode optical fiber wrapped around sample and reference chambers. The sensitivity of the calorimeter was determined to be 74 rad of phase shift per mW of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  16. Fiber Optic Calorimetry

    International Nuclear Information System (INIS)

    Rudy, C.; Bayliss, S.; Bracken, D.; Bush, J.; Davis, P.

    1997-01-01

    A twin-bridge calorimeter using optical fiber as the sensor element was constructed and tested. This system demonstrates the principle and capability of using optical fibers for heat-flow measurements of special nuclear material. This calorimeter uses piezoelectric-generated phase-carrier modulation with subsequent electronic signal processes to allow phase shifts as small as 1 microradian (microrad) to be measured. The sensing element consists of 21-m lengths of single-mode optical fiber wrapped around sample and reference chambers. The sensitivity of the calorimeter was determined to be 74 radians (rad) of phase shift per milliwatt of thermal power. One milliwatt of thermal power is equivalent to 400 mg of plutonium (6% 240 Pu). The system noise base was about 0.2 rad, equivalent to about 1 mg of plutonium

  17. Digital Hadron Calorimetry

    Science.gov (United States)

    Bilki, Burak

    2018-03-01

    The Particle Flow Algorithms attempt to measure each particle in a hadronic jet individually, using the detector providing the best energy/momentum resolution. Therefore, the spatial segmentation of the calorimeter plays a crucial role. In this context, the CALICE Collaboration developed the Digital Hadron Calorimeter. The Digital Hadron Calorimeter uses Resistive Plate Chambers as active media and has a 1-bit resolution (digital) readout of 1 × 1 cm2 pads. The calorimeter was tested with steel and tungsten absorber structures, as well as with no absorber structure, at the Fermilab and CERN test beam facilities over several years. In addition to conventional calorimetric measurements, the Digital Hadron Calorimeter offers detailed measurements of event shapes, rigorous tests of simulation models and various tools for improved performance due to its very high spatial granularity. Here we report on the results from the analysis of pion and positron events. Results of comparisons with the Monte Carlo simulations are also discussed. The analysis demonstrates the unique utilization of detailed event topologies.

  18. Thermodynamics of Surfactants, Block Copolymers and Their Mixtures in Water: The Role of the Isothermal Calorimetry

    Science.gov (United States)

    De Lisi, Rosario; Milioto, Stefania; Muratore, Nicola

    2009-01-01

    The thermodynamics of conventional surfactants, block copolymers and their mixtures in water was described to the light of the enthalpy function. The two methodologies, i.e. the van’t Hoff approach and the isothermal calorimetry, used to determine the enthalpy of micellization of pure surfactants and block copolymers were described. The van’t Hoff method was critically discussed. The aqueous copolymer+surfactant mixtures were analyzed by means of the isothermal titration calorimetry and the enthalpy of transfer of the copolymer from the water to the aqueous surfactant solutions. Thermodynamic models were presented to show the procedure to extract straightforward molecular insights from the bulk properties. PMID:19742173

  19. Potentiometric titration with polarized electrodes

    International Nuclear Information System (INIS)

    Chikryzova, E.G.

    1977-01-01

    Based on the analysis of the works carried out during 1911-75 consideration is given to the present state of the method of potentiometric titration with polarized electrodes. The material is generalized in the tabular form indicating the elments of interest, titration conditions and the objects to be analyzed. The list and classification of the potentiometric titration methods intended for determining organic and inorganic substances are presented

  20. AUTOMATION OF POTENTIOMETRIC TITRATION WITH A ...

    African Journals Online (AJOL)

    An IBM compatible interface card system with infrared source-detector data sampling was designed and tested for automation of potentiometric titrations with personal computers without continuous measurement of the volume of the titrant. The device with other appropriate apparatus and setup was tested for determination ...

  1. Experience with uranium-scintillator calorimetry

    International Nuclear Information System (INIS)

    Hasell, D.K.; Frisken, W.R.

    1990-01-01

    The ZEUS experiment on HERA will employ depleted uranium-scintillator calorimetry. Extensive studies have been made to optimize the calorimeter design. Test results and design aspects are discussed with a view to energy resolution, uniformity of response, mechanical assembly and calibration and monitoring. The energy resolution of four prototype calorimeter modules has been measured as 18%/v√E for electrons from 1 to 75 GeV and 35%/√E for pions from 1 to 100 GeV with an e/h ratio equal to one

  2. Calorimetry of non-reacting systems

    CERN Document Server

    McCullough, John P

    2013-01-01

    Experimental Thermodynamics, Volume 1: Calorimetry of Non-Reacting Systems covers the heat capacity determinations for chemical substances in the solid, liquid, solution, and vapor states, at temperatures ranging from near the absolute zero to the highest at which calorimetry is feasible.This book is divided into 14 chapters. The first four chapters provide background information and general principles applicable to all types of calorimetry of non-reacting systems. The remaining 10 chapters deal with specific types of calorimetry. Most of the types of calorimetry treated are developed over a c

  3. Corrosion Measurements by Titration, (CMT). Alone or Combined With Electrochemical Measurements(EC). Examples: Corrosion of Zinc, Nickel, Aluminium and Iron

    DEFF Research Database (Denmark)

    Bech-Nielsen, Gregers

    1998-01-01

    species or non-electrochemical dissolution reactions.A great number of examinations of corrosion has been made with the following metals: Zinc, nickel, aluminium and iron, as pure metals or alloys and also, with zinc, as post-treated electrodeposits.Limitations and restrictions in the use of CMT......At the corrosion potential the anodic dissolution of metal, Me = Me(z+) + z (e-), is accompanied by a cathodic reaction, z H(+) + z e(-) = z/2 H(2), for example. In order to maintain a constant pH-value addition of acid is needed, at a rate, which is equal to the rate of metal dissolution....... Measurement of the rate of addition of acid is then equivalent to a measurement of the rate of metal dissolution. By using a pH-stat and a simple PC-program the rate of corrosion can be measured continuously and very precisely; this is the basis for CMT measurements. Electrochemical measurements of corrosion...

  4. INSTRUMENTS AND METHODS OF INVESTIGATION: Electron-proton separation in calorimetry experiments directly measuring the composition and energy spectrum of cosmic rays

    Science.gov (United States)

    Voronov, Sergei A.; Borisov, Stanislav V.; Karelin, Aleksandr V.

    2009-09-01

    Calorimetric particle detectors that play an important role in high-energy cosmic-ray balloon and satellite experiments not only have the major task of measuring energy but also face the problem of identifying electrons and protons. This problem is usually solved by measuring the longitudinal and traverse shower profiles and the total energy release in the calorimeter, using the fact that electromagnetic and hadronic showers differ in their spatial and energy distributions. In this paper, electron and proton identification methods for different types of calorimeters used in cosmic-ray balloon- and satellite-borne experiments are discussed.

  5. Electromagnetic calorimeter and accurate measurement with the ATLAS detector of the LHC collider; Calorimetrie electromagnetique et mesures de precision avec le detecteur ATLAS aupres du collisionneur LHC

    Energy Technology Data Exchange (ETDEWEB)

    Pralavorio, P

    2007-06-15

    The main purpose of the ATLAS experiment is the understanding of the underlying mechanisms that drive the breaking of the electro-weak symmetry through the discovery of Higgs bosons. An important element to achieve this aim was the design of an electromagnetic calorimeter able to investigate the decay channels: H {yields} {gamma}{gamma} and H {yields} 4e. The high performance of the calorimeter will allow us to get a better accuracy on the measuring values of W and top masses which is essential to indirectly constrain the mass of the Higgs. In the same way, accurate measurements of top and W properties during the decays of top and tWb vertex will be necessary to question the standard model and to see beyond. The author has been working for 9 years in the ATLAS project, he has been involved in the design, construction, qualification and testing phases of the electromagnetic calorimeter of ATLAS. This document is a detailed presentation of the calorimeter, of its qualification and of its expectations when LHC is operating. This document is organized into 4 chapters: 1) assets and weaknesses of the standard model, 2) the ATLAS experiment, 3) the electromagnetic calorimeter, and 4) accurate measurements with ATLAS. This document presented before an academic board will allow its author to manage research works and particularly to tutor thesis students. (A.C.)

  6. Dissociation of weak acids during Gran plot free acidity titrations

    OpenAIRE

    Lindberg, Steven E:; Cole, Jan M.

    2011-01-01

    A comparison of weak and free acid concentrations measured by base titration and hydrogen ionactivities determined by direct pH measurement is described for several of our data sets for raincollected above and below a forest canopy in the eastern United States. These data illustrate theinfluence of weak acid dissociation during titration and the possible effect of activity coefficientson calculated free acid concentrations.DOI: 10.1111/j.1600-0889.1984.tb00240.x

  7. Amperometric, Bipotentiometric, and Coulometric Titration.

    Science.gov (United States)

    Stock, John T.

    1980-01-01

    Discusses recent review articles in various kinds of titration. Also discusses new research in apparatus and methodology, acid-base reactions, precipitation and complexing reactions, oxidation-reduction reactions, and nomenclature. Cites 338 references. (CS)

  8. Higher Order Inclusion Complexes and Secondary Interactions Studied by Global Analysis of Calorimetric Titrations

    DEFF Research Database (Denmark)

    Schönbeck, Jens Christian Sidney; Holm, René; Westh, Peter

    2012-01-01

    This paper investigates the use of isothermal titration calorimetry (ITC) as a tool for studying molecular systems in which weaker secondary interactions are present in addition to a dominant primary interaction. Such systems are challenging since the signal pertaining to the stronger primary......). The results are validated by a 13C NMR titration and negative controls with a bile salt with no secondary binding site (glycocholate) (K = 2.96 ± 0.01 × 103 M–1). The method proved useful for detailed analysis of ITC data and may strengthen its use as a tool for studying molecular systems by advanced binding...

  9. Development of Quartz Fiber Calorimetry

    CERN Multimedia

    2002-01-01

    % RD40 \\\\ \\\\ Very Forward Calorimeters (VFCs) in LHC detectors should cover the pseudorapidity range from $\\eta$~=~2.5 to at least $\\eta$~=~5 in order to compute missing transverse energy and for jet tagging. Operation at such high rapidity requires the use of a calorimetry technique that is very radiation resistant, fast and insensitive to radioactivity (especially to neutrons). This can be accomplished through the Quartz-Calorimeter~(Q-Cal) concept of embedding silica core fibers, that resist to the Gigarad radiation level, into an absorber. In this calorimeter the shower particles produce light through the Cherenkov effect generating a signal less than 10~ns in duration. Unique to this new technology the visible energy of hadronic showers has a transverse dimension nearly an order of magnitude smaller than that in conventional calorimeters, enabling precise spatial resolution, sharper isolation cuts and better jet recognition against the minimum bias events background. Last but not least, most radioactive ...

  10. Spectroscopy, calorimetry and molecular simulation studies on the interaction of catalase with copper ion.

    Science.gov (United States)

    Hao, Fang; Jing, Mingyang; Zhao, Xingchen; Liu, Rutao

    2015-02-01

    In this research, the binding mechanism of Cu(2+) to bovine liver catalase (BLC) was studied by fluorescence spectroscopy, ultraviolet-visible (UV-vis) absorption spectroscopy, circular dichroism (CD) spectroscopy, isothermal titration calorimetry (ITC) and molecular docking methods. The cellar experiment was firstly carried out to investigate the inhibition effect of catalase. During the fluorescence quenching study, after correcting the inner filter effect (IFE), the fluorescence of BLC was found to be quenched by Cu(2+). The quenching mechanism was determined by fluorescence lifetime measurement, and was confirmed to be the dynamic mode. The secondary structure content of BLC was changed by the addition of Cu(2+), as revealed by UV-vis absorption and CD spectra, which further induces the decrease in BLC activity. Molecular simulation study indicates that Cu(2+) is located between two β-sheets and two random coils of BLC near to the heme group, and interacts with His 74 and Ser 113 residues near a hydrophilic area. The decrease of α-helix and the binding of His 74 are considered to be the major reason for the inhibition of BLC activity caused by Cu(2+). The ITC results indicate that the binding stoichiometry of Cu(2+) to catalase is 11.4. Moreover, the binding of Cu(2+) to BLC destroyed H-bonds, which was confirmed by the CD result. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Silicon calorimetry for the SSC[ Superconducting Supercollider

    International Nuclear Information System (INIS)

    Bertrand, C.; Borchi, E.; Brau, J.E.

    1989-01-01

    SSC experiments will rely heavily on their calorimeters. Silicon calorimetry, which has been introduced in recent years as a useful technology, has many attractive characteristics which may make it a viable option for consideration. The many attractive properties of silicon detectors are reviewed. The relevant present day applications of large areas of silicon detectors are summarize to illustrate the emerging use. The troublesome issue of radiation damage in a high luminosity environment like the SSC is considered with a summary of much of the recent new measurements which help clarify this situation. A discussion of the electronics and a possible mechanical configuration is presented, followed by a summary of the outstanding R and D issues. 31 refs., 11 figs., 3 tabs

  12. Indirect calorimetry: assessing animal response to heat and cold stress

    NARCIS (Netherlands)

    Gaughan, J.B.; Heetkamp, M.J.W.; Hendriks, P.

    2015-01-01

    Calorimetric thermal stress studies where indirect calorimetry is used as a tool to estimate energy expenditure have been undertaken since this technique was developed. Some examples of these studies are presented in this chapter. The measurement of gas exchange by means of an open-circuit

  13. Study of asphaltene precipitation by Calorimetry

    DEFF Research Database (Denmark)

    Verdier, Sylvain Charles Roland; Plantier, Frédéric; Bessières, David

    2007-01-01

    Can calorimetry bring new input to the Current understanding of asphaltene precipitation? In this work, two types of precipitation were studied by means of calorimetry: addition of n-heptane into asphaltene solutions and temperature/pressure variations on a recombined live oil. The first series...

  14. Kinetic characteristics of polygalacturonase enzymes hydrolyzing galacturonic acid oligomers using isothermal titration calorimetry

    Science.gov (United States)

    Polygalacturonase enzymes hydrolyze the polygalacturonic acid chains found in pectin. Interest in polygalacturonase enzymes continues as they are useful in a number of industrial processes and conversely, detrimental, as they are involved in maceration of economically important crops. While a good...

  15. Synergy of molecular dynamics and isothermal titration calorimetry in studies of Allostery

    Czech Academy of Sciences Publication Activity Database

    Strawn, R.; Stockner, T.; Melicherčík, Milan; Jin, L.; Xue,, W. F.; Carey, J.; Ettrich, Rüdiger

    2011-01-01

    Roč. 492, - (2011), s. 151-188 ISSN 0076-6879 R&D Projects: GA MŠk(CZ) LC06010; GA ČR GAP207/10/1934 Institutional research plan: CEZ:AV0Z60870520 Keywords : hexameric arginine repressor * DNA-binding domain * escherichia-coli * ligand-binding * bacillus-stearothhermophilus * proteins * systems * model * simulations * operator Subject RIV: EH - Ecology, Behaviour Impact factor: 2.042, year: 2011

  16. Detection of conformational changes in immunoglobulin G using isothermal titration calorimetry with low molecular weight probes

    NARCIS (Netherlands)

    Rispens, T.; Lakemond, C.M.M.; Derksen, N.I.L.; Aalberse, R.C.

    2008-01-01

    Proteins for therapeutic use may contain small amounts of partially misfolded monomeric precursors to postproduction aggregation. To detect these misfolded proteins in the presence of an excess of properly folded protein, fluorescent probes such as 8-anilino-1-naphthalene sulfonate (ANS) are

  17. Measuring energy expenditure in the intensive care unit: a comparison of indirect calorimetry by E-sCOVX and Quark RMR with Deltatrac II in mechanically ventilated critically ill patients.

    Science.gov (United States)

    Rehal, Martin Sundström; Fiskaare, Erik; Tjäder, Inga; Norberg, Åke; Rooyackers, Olav; Wernerman, Jan

    2016-03-05

    Indirect calorimetry allows the determination of energy expenditure in critically ill patients by measuring oxygen consumption (VO2) and carbon dioxide production (VCO2). Recent studies have demonstrated variable performance of "breath-by-breath" instruments compared to mixing chamber technology. The aim of this study was to validate two modern devices (E-sCOVX and Quark RMR) against a reference method (Deltatrac II). Measurements of VO2/VCO2 with the test and reference devices were performed simultaneously over a 20-min period in mechanically ventilated adult intensive care unit patients. Accuracy and precision of instruments were analyzed using Bland-Altman plots. Forty-eight measurements in 22 patients were included for analysis. Both E-sCOVX and Quark RMR overestimated VO2 and VCO2 compared to Deltatrac II, corresponding to a 10% higher mean resting energy expenditure. Limits of agreement of resting energy expenditure within ± 2 standard deviations were ± 461 kcal/24 h (± 21% expressed as percentage error) for ΔE-sCOVX-Deltatrac II and ± 465 kcal/24 h (± 22%) for ΔQuark RMR-Deltatrac II. Both test devices overestimate VO2 and VCO2 compared to Deltatrac II. The observed limits of agreement are comparable to those commonly accepted in evaluations of circulatory monitoring, and significantly less than results from predictive equations. We hypothesize that the discrepancy between methods is due to patient/ventilator-related factors that affect the synchronization of gas and spirometry waveforms. Australian New Zealand Clinical Trials Registry, Trial ID ACTRN12615000205538. Date registered 3 March 2015.

  18. Ultra-Fast Hadronic Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Denisov, Dmitri [Fermilab; Lukić, Strahinja [VINCA Inst. Nucl. Sci., Belgrade; Mokhov, Nikolai [Fermilab; Striganov, Sergei [Fermilab; Ujić, Predrag [VINCA Inst. Nucl. Sci., Belgrade

    2017-12-18

    Calorimeters for particle physics experiments with integration time of a few ns will substantially improve the capability of the experiment to resolve event pileup and to reject backgrounds. In this paper time development of hadronic showers induced by 30 and 60 GeV positive pions and 120 GeV protons is studied using Monte Carlo simulation and beam tests with a prototype of a sampling steel-scintillator hadronic calorimeter. In the beam tests, scintillator signals induced by hadronic showers in steel are sampled with a period of 0.2 ns and precisely time-aligned in order to study the average signal waveform at various locations w.r.t. the beam particle impact. Simulations of the same setup are performed using the MARS15 code. Both simulation and test beam results suggest that energy deposition in steel calorimeters develop over a time shorter than 3 ns providing opportunity for ultra-fast calorimetry. Simulation results for an "ideal" calorimeter consisting exclusively of bulk tungsten or copper are presented to establish the lower limit of the signal integration window.

  19. Differential scanning calorimetry of bacteria.

    Science.gov (United States)

    Miles, C A; Mackey, B M; Parsons, S E

    1986-04-01

    Thermograms obtained by differential scanning calorimetry of a range of bacteria of different heat resistances were compared. Equations were derived to calculate the rate at which the numbers of viable organisms in a calorimeter decline as the temperature is raised at a constant rate. Vegetative bacteria scanned at 10 degrees C min-1 showed multi-peaked thermograms with four major peaks (denoted m, n, p and q) occurring in the regions 68-73, 77-84, 89-99 and 105-110 degrees C respectively. Exceptions were that peak m (the largest peak) occurred at 79-82 degrees C in Bacillus stearothermophilus and an additional peak, r, was detected in Escherichia coli at 119 degrees C. At temperatures below the main peak m there were major differences in thermograms between species. There was a direct relationship between the onset of thermal denaturation and the thermoresistance of different organisms. Heat-sensitive organisms displayed thermogram features which were absent in the more heat-resistant types. When samples were cooled to 5 degrees C and re-heated, a small endothermic peak, pr, was observed at the same temperature as p. Peaks p and pr were identified as the melting endotherms of DNA. In all vegetative organisms examined, maximum death rates, computed from published D and z values, occurred at temperatures above the onset of thermal denaturation, i.e. cell death and irreversible denaturation of cell components occurred within the same temperature range.

  20. What does calorimetry and thermodynamics of living cells tell us?

    Science.gov (United States)

    Maskow, Thomas; Paufler, Sven

    2015-04-01

    This article presents and compares several thermodynamic methods for the quantitative interpretation of data from calorimetric measurements. Heat generation and absorption are universal features of microbial growth and product formation as well as of cell cultures from animals, plants and insects. The heat production rate reflects metabolic changes in real time and is measurable on-line. The detection limit of commercially available calorimetric instruments can be low enough to measure the heat of 100,000 aerobically growing bacteria or of 100 myocardial cells. Heat can be monitored in reaction vessels ranging from a few nanoliters up to many cubic meters. Most important the heat flux measurement does not interfere with the biological process under investigation. The practical advantages of calorimetry include the waiver of labeling and reactants. It is further possible to assemble the thermal transducer in a protected way that reduces aging and thereby signal drifts. Calorimetry works with optically opaque solutions. All of these advantages make calorimetry an interesting method for many applications in medicine, environmental sciences, ecology, biochemistry and biotechnology, just to mention a few. However, in many cases the heat signal is merely used to monitor biological processes but only rarely to quantitatively interpret the data. Therefore, a significant proportion of the information potential of calorimetry remains unutilized. To fill this information gap and to motivate the reader using the full information potential of calorimetry, various methods for quantitative data interpretations are presented, evaluated and compared with each other. Possible errors of interpretation and limitations of quantitative data analysis are also discussed. Copyright © 2014 Elsevier Inc. All rights reserved.

  1. TAPIR: a device for automatic titration with incremental weighing of the titration reagent

    International Nuclear Information System (INIS)

    Ganivet, Michel

    TAPIR is a titration device enabling automatic analyses with weighting of the titration reagent. The titration method used can be based on potentiometry, amperometry, color indicator change... The reproducibility is about 3.10 -4 [fr

  2. Improving medication titration in heart failure by embedding a structured medication titration plan.

    Science.gov (United States)

    Hickey, Annabel; Suna, Jessica; Marquart, Louise; Denaro, Charles; Javorsky, George; Munns, Andrew; Mudge, Alison; Atherton, John J

    2016-12-01

    To improve up-titration of medications to target dose in heart failure patients by improving communication from hospital to primary care. This quality improvement project was undertaken within three heart failure disease management (HFDM) services in Queensland, Australia. A structured medication plan was collaboratively designed and implemented in an iterative manner, using methods including awareness raising and education, audit and feedback, integration into existing work practice, and incentive payments. Evaluation was undertaken using sequential audits, and included process measures (use of the titration plan, assignment of responsibility) and outcome measures (proportion of patients achieving target dose) in HFDM service patients with reduced left ventricular ejection fraction. Comparison of the three patient cohorts (pre-intervention cohort A n=96, intervention cohort B n=95, intervention cohort C n=89) showed increase use of the titration plan, a shift to greater primary care responsibility for titration, and an increase in the proportion of patients achieving target doses of angiotensin converting enzyme inhibitors/angiotensin receptor blockers (ACEI/ARB) (A 37% vs B 48% vs C 55%, p=0.051) and beta-blockers (A 38% vs B 33% vs C 51%, p=0.045). Combining all three cohorts, patients not on target doses when discharged from hospital were more likely to achieve target doses of ACEI/ARB (pplan. A medication titration plan was successfully implemented in three HFDM services and improved transitional communication and achievement of target doses of evidence-based therapies within six months of hospital discharge. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  3. Recent Work on Calorimetry at LANL

    Energy Technology Data Exchange (ETDEWEB)

    Santi, Peter A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Hauck, Danielle K. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2014-01-09

    This report is a briefing to collaborators at the Swedish Nuclear Fuel and Waste Management Company, Oskarshamn, Sweden, January 14, 2014. It describes the way in which calorimetry supports the safegurard mission.

  4. Calorimetry of ion beam damage in silicon

    International Nuclear Information System (INIS)

    Roorda, S.; Kajrys, G.; Graham, J.

    1994-01-01

    Annealing of ion-beam damage in crystalline Si has been characterized by differential scanning calorimetry and infrared absorption spectroscopy. Si discs of 100 μm thickness have been bombarded with 3.4 MeV protons. Scanning calorimetry reveals a sharp peak riding on a broad background signal. From infrared absorption, this peak is tentatively identified as heat release associated with divacancy annihilation. (orig.)

  5. Glass transition of anhydrous starch by fast scanning calorimetry.

    Science.gov (United States)

    Monnier, Xavier; Maigret, Jean-Eudes; Lourdin, Denis; Saiter, Allisson

    2017-10-01

    By means of fast scanning calorimetry, the glass transition of anhydrous amorphous starch has been measured. With a scanning rate of 2000Ks -1 , thermal degradation of starch prior to the glass transition has been inhibited. To certify the glass transition measurement, structural relaxation of the glassy state has been investigated through physical aging as well as the concept of limiting fictive temperature. In both cases, characteristic enthalpy recovery peaks related to the structural relaxation of the glass have been observed. Thermal lag corrections based on the comparison of glass transition temperatures measured by means of differential and fast scanning calorimetry have been proposed. The complementary investigations give an anhydrous amorphous starch glass transition temperature of 312±7°C. This estimation correlates with previous extrapolation performed on hydrated starches. Copyright © 2017 Elsevier Ltd. All rights reserved.

  6. Comparison of VFA titration procedures used for monitoring the biogas process

    DEFF Research Database (Denmark)

    Lützhøft, Hans-Christian Holten; Boe, Kanokwan; Fang, Cheng

    2014-01-01

    titration procedures. Currently, no standardized procedure is used and it is therefore difficult to compare the performance among plants. The aim of this study was to evaluate four titration procedures (for determination of VFA-levels of digested manure samples) and compare results with gas chromatographic...... (GC) analysis. Two of the procedures are commonly used in biogas plants and two are discussed in literature. The results showed that the optimal titration results were obtained when 40mL of four times diluted digested manure was gently stirred (200rpm). Results from samples with different VFA...... concentrations (1-11g/L) showed linear correlation between titration results and GC measurements. However, determination of VFA by titration generally overestimated the VFA contents compared with GC measurements when samples had low VFA concentrations, i.e. around 1g/L. The accuracy of titration increased when...

  7. Colorblindness and Titrations with Visual Indicators.

    Science.gov (United States)

    Diehl, Harvey; And Others

    1985-01-01

    Discusses various issues related to colorblind students performing titrations with visual indicators. Includes tables showing precisions in the titration of a weak acid by colorblind students using phenolphthalein and thymolphthalein and in the titration of a weak base by colorblind persons using methyl red and bromcresol green. (JN)

  8. Current status of tritium calorimetry at TLK

    International Nuclear Information System (INIS)

    Buekki-Deme, A.; Alecu, C.G.; Kloppe, B.; Bornschein, B.

    2015-01-01

    Inside a tritium facility, calorimetry is an important analytical method as it is the only reference method for accountancy (it is based on the measurement of the heat generated by the radioactive decay). Presently, at Tritium Laboratory Karlsruhe (TLK), 4 calorimeters are in operation, one of isothermal type and three of inertial guidance control type (IGC). The volume of the calorimeters varies between 0.5 and 20.6 liters. About two years ago we started an extensive work to improve our calorimeters with regard to reliability and precision. We were forced to upgrade 3 of our 4 calorimeters due to the outdated interfaces and software. This work involved creating new LabView programs driving the devices, re-tuning control loops and replacing obsolete hardware components. In this paper we give a review on the current performance of our calorimeters, comparing it to recently available devices from the market and in the literature. We also show some ideas for a next generation calorimeter based on experiences with our IGC calorimeters and other devices reported in the literature. (authors)

  9. Evaluation of an automatic uranium titration system

    International Nuclear Information System (INIS)

    Lewis, K.

    1980-01-01

    The titration system utilizes the constant current coulometric titration of Goldbeck and Lerner. U(VI) is reduced to U(IV) by Fe(II). V(V) is generated to titrate the U(IV), and the titration is followed potentiometrically. The evaluation shows that the recovery of uranium is 100% at the 40-mg level. The accuracy is generally +-0.10% or better. The smallest sample weight at which reliable results were obtained was 40 mg of uranium. Time for one analysis is 15 minutes. Advantages and disadvantages of the automated titrator are listed

  10. Micellization of bovine beta-casein studied by isothermal titration microcalorimetry and cryogenic transmission electron microscopy.

    Science.gov (United States)

    Portnaya, Irina; Cogan, Uri; Livney, Yoav D; Ramon, Ory; Shimoni, Karin; Rosenberg, Moshe; Danino, Dganit

    2006-07-26

    The association behavior, critical micellization concentration (CMC), and enthalpy of demicellization (DeltaHdemic) of bovine beta-casein were studied, for the first time by isothermal titration calorimetry, in a pH 7.0 phosphate buffer with 0.1 ionic strength and in pure water. In the buffer solutions, the CMC decreased asymptotically from 0.15 to 0.006 mM as the temperature was raised from 16 to 45 degrees C. DeltaHdemic decreased with increasing temperature between 16 and 28 degrees C but increased from 28 to 45 degrees C. Thermodynamic analysis below 30 degrees C is consistent with the Kegeles shell model, which suggests a stepwise association process. At higher temperatures, this model exhibits limitations, and the micellization becomes much more cooperative. The CMC values in water, measured between 17 and 28 degrees C, decreased with increasing temperature and, expectedly, were higher than those found in the buffer solutions. beta-Casein micelles were visualized and characterized, for the first time in their hydrated state, using advanced digital-imaging cryogenic transmission electron microscopy. The images revealed small, oblate micelles, about approximately 13 nm in diameter. The micelles shape and dimensions remained nearly constant in the temperature range of 24-35 degrees C.

  11. Application of »Mass Titration« to Determination of Surface Charge of Metal Oxides

    OpenAIRE

    1998-01-01

    The mass titration method, used for the point of zero charge determination, was extended to the measurement of the surface charge density. The results agree with the common method, which is the acid-base titration of the colloidal suspension. The advantage of mass titration is that one does not need to perform blank titration, instead one simply adds metal oxide powder to the electrolyte aqueous solution of known pH. To cover the pH range above and below the point of zero charge, two experime...

  12. Calorimetry exchange program annual data report for 1992

    International Nuclear Information System (INIS)

    Barnett, T.M.

    1992-01-01

    The goals of the Calorimetry Sample Exchange Program are: discuss measurement differences; review and improve analytical measurements and methods; discuss new measurement capabilities; provide data to DOE on measurement capabilities to evaluate shipper-receiver differences; provide characterized or standard materials as necessary for exchange participants; and provide a measurement control program for plutonium analysis. A sample of PuO 2 powder is available at each participating site for NDA measurement, including either or both calorimetry and high-resolution gamma-ray spectroscopy, the elements which are typically combined to provide a calorimetric assay of plutonium. The facilities measure the sample as frequently and to the level of precision which they desire, and then submit the data to the Exchange for analysis. The data report includes summary tables for each measurement and charts showing the performance of each laboratory. Comparisons are made to the accepted values for the exchange sample and to data previously reported by that laboratory. This information is presented, in the form of quarterly and annual reports, intended for use by Exchange participants in measurement control programs, or to indicate when bias corrections may be appropriate. No attempt, however, has been made to standardize methods or frequency of data collection, calibration, or operating procedures. Direct comparisons between laboratories may, therefore, be misleading since data have not been collected to the same precision or for the same time periods. A meeting of the participants of the Calorimetry Exchange is held annually at EG ampersand G Mound Applied Technologies. The purposes of this meeting are to discuss measurement differences, problems, and new measurement capabilities, and to determine the additional activities needed to fulfill the goals of the Exchange. This document provides data for 1992

  13. Fast differential scanning calorimetry of liquid samples with chips

    DEFF Research Database (Denmark)

    Splinter, R.; van Herwaarden, A. W.; van Wetten, I. A.

    2015-01-01

    Based on a modified version of standard chips for fast differential scanning calorimetry, DSC of liquid samples has been performed at temperature scan rates of up to 1000 °C/s. This paper describes experimental results with the protein lysozyme, bovine serum, and olive oil. The heating and cooling....... The bovine serum measurements show two main peaks, in good agreement with standard DSC measurements. Olive oil has been measured, with good agreement for the cooling curve and qualitative agreement for the heater curve, compared to DSC measurements....

  14. Scintillating glasses for total absorption dual readout calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Bonvicini, V. [INFN, Trieste; Driutti, A. [Udine U.; Cauz, D. [Udine U.; Pauletta, G. [Udine U.; Rubinov, P. [Fermilab; Santi, L. [Udine U.; Wenzel, H. [Fermilab

    2012-01-01

    Scintillating glasses are a potentially cheaper alternative to crystal - based calorimetry with common problems related to light collection, detection and processing. As such, their use and development are part of more extensive R&D aimed at investigating the potential of total absorption, combined with the readout (DR) technique, for hadron calorimetry. A recent series of measurements, using cosmic and particle beams from the Fermilab test beam facility and scintillating glass with the characteristics required for application of the DR technique, serve to illustrate the problems addressed and the progress achieved by this R&D. Alternative solutions for light collection (conventional and silicon photomultipliers) and signal processing are compared, the separate contributions of scintillation and Cherenkov processes to the signal are evaluated and results are compared to simulation.

  15. HypCal, a general-purpose computer program for the determination of standard reaction enthalpy and binding constant values by means of calorimetry.

    Science.gov (United States)

    Arena, Giuseppe; Gans, Peter; Sgarlata, Carmelo

    2016-09-01

    The program HypCal has been developed to provide a means for the simultaneous determination, from data obtained by isothermal titration calorimetry, of both standard enthalpy of reaction and binding constant values. The chemical system is defined in terms of species of given stoichiometry rather than in terms of binding models (e.g., independent or cooperative). The program does not impose any limits on the complexity of the chemical systems that can be treated, including competing ligand systems. Many titration curves may be treated simultaneously. HypCal can also be used as a simulation program when designing experiments. The use of the program is illustrated with data obtained with nicotinic acid (niacin, pyridine-3 carboxylic acid). Preliminary experiments were used to establish the rather different titration conditions for the two sets of titration curves that are needed to determine the parameters for protonation of the carboxylate and amine groups.

  16. Calorimetry exchange program. Quarterly data report, 2nd quarter 1992

    Energy Technology Data Exchange (ETDEWEB)

    Barnett, T.M.

    1996-07-01

    The goals of the Calorimetry Sample Exchange Program are: (1) Discuss measurement differences, (2) Review and improve analytical measurements and methods, (3) Discuss new measurement capabilities, (4) Provide data to DOE on measurement capabilities to evaluate shipper-receiver differences, (5) Provide characterized or standard materials as necessary for exchange participants, (6) Provide a measurement control program for plutonium analysis. A sample of PuO{sub 2} powder is available at each participating site for NDA measurement, including either or both calorimetry and high-resolution gamma-ray spectroscopy, the elements which are typically combined to provide a calorimetric assay of plutonium. The facilities measure the sample as frequently and to the level of precision which they desire, and then submit the data to the Exchange for analysis. Statistical tests are used to evaluate the data and to determine if there are significant differences from accepted values for the exchange sample or from data previously reported by that facility. This information is presented, in the form of a quarterly report, intended for use by Exchange participants in measurement control programs, or to indicate when bias corrections may be appropriate. No, attempt, however, has been made to standardize methods or frequency of data collection, calibration, or operating procedures. Direct comparisons between laboratories may, therefore, be misleading since data have not been collected to the same precision or for the same time periods. A meeting of the participants of the Calorimetry Exchange is held annually at EG&G Mound Applied Technologies. The purposes of this meeting are to discuss measurement differences, problems, and new measurement capabilities, and to determine the additional activities needed to fulfill the goals of the Exchange.

  17. Determination of the thermodynamic properties of complexation and extraction by micro-calorimetry

    International Nuclear Information System (INIS)

    Charbonnel, M.Ch.; Flandin, J.L.

    2000-01-01

    The CEA is currently developing the DIAMEX process, the first step in the strategy for the separation of minor actinides from high-level radioactive waste. The extractant belongs to the diamide family of molecules and is able to co-extract trivalent actinides and lanthanides. This study focuses on the thermodynamic properties (ΔH, ΔG, ΔS) of lanthanide extraction by malonamide in order to better understand the mechanisms involved and to account for differences in the behavior of various diamide extractants. The main technique used is microcalorimetric titration. The Thermal Activity Monitor (TAM) microcalorimeter is a modular system with a highly stable (± 0.1 mK) temperature-controlled bath containing up to four calorimetry vessel units. The sensor bulbs inserted in the reaction vessel can measure heat flows in static or dynamic conditions. Micro-calorimetry, and calorimetric titration in particular, is a fast growing field due to technical improvements in both hardware and software. In the case of an equilibrium reaction, titration allows both Δ r G and Δ r H (and thus Δ r S) to be determined simultaneously. It was decided to initiate this thermochemical investigation with a homogeneous phase reaction, and the first study concerned the aqueous phase complexation of a trivalent lanthanide ion by a water-soluble diamide, tetraethyl-malonamide (TEMA: (C 2 H 5 ) 2 NCO-CH 2 CON(C 2 H 5 ) 2 ). In the test system, the heat of dilution of the diamide in water is preponderant over the heat arising from the complexation reaction; the result is a positive value corresponding to an endothermic reaction. However, the equilibration constant K and Δ H are both very small, and cannot be calculated from the resulting Q v f(n TEMA ) curves. Moreover, in aqueous phase, the reactions involved are different from those observed when neodymium(III) is extracted into an organic phase, and the medium must be further characterized before the calorimetry data can be fully

  18. Calorimetry and thermal methods in catalysis

    CERN Document Server

    Auroux, Aline

    2013-01-01

    The book is about calorimetry and thermal analysis methods, alone or linked to other techniques, as applied to the characterization of catalysts, supports and adsorbents, and to the study of catalytic reactions in various domains: air and wastewater treatment, clean and renewable energies, refining of hydrocarbons, green chemistry, hydrogen production and storage. The book is intended to fill the gap between the basic thermodynamic and kinetics concepts acquired by students during their academic formation, and the use of experimental techniques such as thermal analysis and calorimetry to answ

  19. Effect of Body Position on Energy Expenditure of Preterm Infants as Determined by Simultaneous Direct and Indirect Calorimetry.

    Science.gov (United States)

    Bell, Edward F; Johnson, Karen J; Dove, Edwin L

    2017-04-01

    Background  Indirect calorimetry is the standard method for estimating energy expenditure in clinical research. Few studies have evaluated indirect calorimetry in infants by comparing it with simultaneous direct calorimetry. Our purpose was (1) to compare the energy expenditure of preterm infants determined by these two methods, direct calorimetry and indirect calorimetry; and (2) to examine the effect of body position, supine or prone, on energy expenditure. Study Design  We measured energy expenditure by simultaneous direct (heat loss by gradient-layer calorimeter corrected for heat storage) and indirect calorimetry (whole-body oxygen consumption and carbon dioxide production) in 15 growing preterm infants during two consecutive interfeeding intervals, once in the supine position and once in the prone position. Results  The mean energy expenditure for all measurements in both positions did not differ significantly by the method used: 2.82 (standard deviation [SD] 0.42) kcal/kg/h by direct calorimetry and 2.78 (SD 0.48) kcal/kg/h by indirect calorimetry. The energy expenditure was significantly lower, by 10%, in the prone than in the supine position, whether examined by direct calorimetry (2.67 vs. 2.97 kcal/kg/h, p  position than in the supine position. Thieme Medical Publishers 333 Seventh Avenue, New York, NY 10001, USA.

  20. New crystals for dual-readout calorimetry

    Czech Academy of Sciences Publication Activity Database

    Akchurin, N.; Bedeschi, F.; Cardini, A.; Carosi, R.; Ciapetti, G.; Ferrari, R.; Franchino, S.; Fraternali, M.; Gaudio, G.; Hauptman, J.; Incagli, M.; Korzhik, M.; Lacava, F.; La Rotonda, L.; Livan, M.; Meoni, E.; Nikl, Martin; Pinci, D.; Policicchio, A.; Popescu, S.; Scuri, F.; Sill, A.; Vandelli, W.; Vedda, A.; Venturelli, T.; Voena, C.; Volobouev, I.; Wigmans, R.

    2009-01-01

    Roč. 604, č. 3 (2009), s. 512-526 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10100521 Keywords : calorimetry * Cherenkov light * high-Z scintillating crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.317, year: 2009

  1. Monte Carlo studies of uranium calorimetry

    International Nuclear Information System (INIS)

    Brau, J.; Hargis, H.J.; Gabriel, T.A.; Bishop, B.L.

    1985-01-01

    Detailed Monte Carlo calculations of uranium calorimetry are presented which reveal a significant difference in the responses of liquid argon and plastic scintillator in uranium calorimeters. Due to saturation effects, neutrons from the uranium are found to contribute only weakly to the liquid argon signal. Electromagnetic sampling inefficiencies are significant and contribute substantially to compensation in both systems. 17 references

  2. Acid/base titrations of simulated PWR crevice environments

    International Nuclear Information System (INIS)

    Pang, J.; Macdonald, D.D.; Millett, P.J.

    1993-01-01

    The construction and operation of a titration system that is capable of exploring the acid/base properties of aqueous systems at temperatures solution is measured using YSZ sensors of the type Hg/HgO/ZrO 2 (Y 2 O 3 )/Solution in conjunction with a suitable reference electrode. The use of the system for measuring the pH of the titrated solutions (NaOH/H 2 SO 4 ) is discussed, and we show that the YSZ pH sensor is capable of consistent and precise pH measurements at elevated temperature (275-325 degrees C) and pressures (100-150 bars). However, the accuracy of the measured pH depends critically on the performance of the reference electrode. In the present work, we ensure the viability of the reference electrode. In the present work, we ensure the viability of the reference electrode by periodically calibrating it in situ using the pH sensor and a standard solution of known pH versus temperature characteristics. The titration data obtained in this study are compared with predictions from EPRI's MULTEQ code, and are found to be in satisfactory agreement in the alkaline pH region. Observed discrepancies in the acidic pH region between the two sets of data are attributed to corrosion of the alloys used to fabricate the titration system

  3. Risks and Benefits of Rapid Clozapine Titration.

    Science.gov (United States)

    Lochhead, Jeannie D; Nelson, Michele A; Schneider, Alan L

    2016-05-18

    Clozapine is often considered the gold standard for the treatment of schizophrenia. Clinical guidelines suggest a gradual titration over 2 weeks to reduce the risks of adverse events such as seizures, hypotension, agranulocytosis, and myocarditis. The slow titration often delays time to therapeutic response. This raises the question of whether, in some patients, it may be safe to use a more rapid clozapine titration. The following case illustrates the potential risks associated with the use of multiple antipsychotics and rapid clozapine titration. We present the case of a young man with schizophrenia who developed life threatening neuroleptic malignant syndrome (NMS) during rapid clozapine titration and treatment with multiple antipsychotics. We were unable to find another case in the literature of NMS associated with rapid clozapine titration. This case is meant to urge clinicians to carefully evaluate the risks and benefits of rapid clozapine titration, and to encourage researchers to further evaluate the safety of rapid clozapine titration. Rapid clozapine titration has implications for decreasing health care costs associated with prolonged hospitalizations, and decreasing the emotional suffering associated with uncontrolled symptoms of psychosis. Clozapine is considered the most effective antipsychotic available thus efforts should focus on developing strategies that would allow for safest and most efficient use of clozapine to encourage its utilization for treatment resistance schizophrenia.

  4. Risks and benefits of rapid clozapine titration

    Directory of Open Access Journals (Sweden)

    Jeannie D. Lochhead

    2016-05-01

    Full Text Available Clozapine is often considered the gold standard for the treatment of schizophrenia. Clinical guidelines suggest a gradual titration over 2 weeks to reduce the risks of adverse events such as seizures, hypotension, agranulocytosis, and myocarditis. The slow titration often delays time to therapeutic response. This raises the question of whether, in some patients, it may be safe to use a more rapid clozapine titration. The following case illustrates the potential risks associated with the use of multiple antipsychotics and rapid clozapine titration. We present the case of a young man with schizophrenia who developed life threatening neuroleptic malignant syndrome (NMS during rapid clozapine titration and treatment with multiple antipsychotics. We were unable to find another case in the literature of NMS associated with rapid clozapine titration. This case is meant to urge clinicians to carefully evaluate the risks and benefits of rapid clozapine titration, and to encourage researchers to further evaluate the safety of rapid clozapine titration. Rapid clozapine titration has implications for decreasing health care costs associated with prolonged hospitalizations, and decreasing the emotional suffering associated with uncontrolled symptoms of psychosis. Clozapine is considered the most effective antipsychotic available thus efforts should focus on developing strategies that would allow for safest and most efficient use of clozapine to encourage its utilization for treatment resistance schizophrenia.

  5. Contributions to the theory of catalytic titrations-III Neutralization catalytic titrations.

    Science.gov (United States)

    Gaál, F F; Abramović, B F

    1985-07-01

    Neutralization catalytic titrations of weak monoprotic adds and bases with both volumetric and coulometric addition of the titrant (strong base/acid) have been simulated by taking into account the equilibrium concentration of the catalyst during the titration. The influence of several factors on the shape of the simulated catalytic titration curve has been investigated and is discussed.

  6. Nap-titration : An effective alternative for continuous positive airway pressure titration

    NARCIS (Netherlands)

    Hoekema, A; Stegenga, B; Meinesz, AF; van der Hoeven, JH; Wijkstra, PJ

    When treating Obstructive Steep Apnea-Hypopnea Syndrome (OSAHS) several alternatives for standard (manual) continuous positive airway pressure (CPAP) titration are feasible. A practical alternative is titration without polysomnography during an afternoon nap (Nap-titration). The aim of the present

  7. Titration curves: a useful instrument for assessing the buffer systems of acidic mining waters.

    Science.gov (United States)

    Totsche, Oliver; Fyson, Andrew; Kalin, Margarete; Steinberg, Christian E W

    2006-07-01

    The acidification of mine waters is generally caused by metal sulfide oxidation, related to mining activities. These waters are characterized by low pH and high acidity due to strong buffering systems. The standard acidity parameter, the Base Neutralization Capacity (BNC), is determined by endpoint titration, and reflects a cumulative parameter of both hydrogen ions and all buffering systems, but does not give information on the individual buffer systems. We demonstrate that a detailed interpretation of titration curves can provide information about the strength of the buffering systems. The buffering systems are of importance for environmental studies and treatment of acidic mining waters. Titrations were carried out by means of an automatic titrator using acidic mining waters from Germany and Canada. The curves were interpreted, compared with each other, to endpoint titration results and to elemental concentrations contained therein. The titration curves were highly reproducible, and contained information about the strength of the buffer systems present. Interpretations are given, and the classification and comparison of acidic mining waters, by the nature and strength of their buffering systems derived from titration curves are discussed. The BNC-values calculated from the curves were more precise than the ones determined by the standard endpoint titration method. Due to the complex buffer mechanisms in acidic mining waters, the calculation of major metal concentrations from the shape of the titration curve resulted in estimates, which should not be confused with precise elemental analysis results. Titration curves provide an inexpensive, valuable and versatile tool, by which to obtain sophisticated information of the acidity in acidic water. The information about the strength of the present buffer systems can help to understand and document the complex nature of acidic mining water buffer systems. Finally, the interpretation of titration curves could help to

  8. Green chemistry volumetric titration kit for pharmaceutical ...

    African Journals Online (AJOL)

    Stopcock SC and Spring Sp models of Econoburette (Calibrated, RTC (NR), Ministry of Small Scale Industries, Government of India), developed for semimicro volumetric titration of pharmaceutical formulations are reported. These are economized and risk free titration where pipette is replaced by an inbuilt pipette and ...

  9. A Tabular Approach to Titration Calculations

    Science.gov (United States)

    Lim, Kieran F.

    2012-01-01

    Titrations are common laboratory exercises in high school and university chemistry courses, because they are easy, relatively inexpensive, and they illustrate a number of fundamental chemical principles. While students have little difficulty with calculations involving a single titration step, there is a significant leap in conceptual difficulty…

  10. Calorimetry and thermodynamics of living systems

    Energy Technology Data Exchange (ETDEWEB)

    Lamprecht, Ingolf

    2003-10-14

    Calorimetry of living systems and classical thermodynamics developed in parallel, from Lavoisier's early ice calorimeter experiments on guinea pigs, followed by Dubrunfaut's macrocalorimetric research of fermentation processes and Atwater-Rosa's whole-body calorimetry on humans and domestic animals, to the introduction of the famous Tian-Calvet instrument that found entrance into so many different fields of biology. In this work, six examples of living-system calorimetry and thermodynamics are presented. These are: (i) glycolytic oscillations far off the thermodynamic equilibrium; (ii) growth and energy balances in fermenting and respiring yeast cultures; (iii) direct and indirect calorimetric monitoring of electrically stimulated reptile metabolism; (iv) biologic and climatic factors influencing the temperature constancy and distribution in the mound of a wood ant colony as an example of a complex ecological system; (v) energetic considerations on the clustering of European honeybees in winter as a means to save energy and stored food as well as for their Japanese counterparts in defending against hornet predators; and (vi) energetic and evolutionary aspects of the mass specific entropy production rate, the so-called bound dissipation or psiu-function. The examples presented here are just a very personal selection of living systems from a broad spectrum at all levels of complexity. Common for all of them is that they were investigated calorimetrically on the background of classical and irreversible thermodynamics.

  11. Calorimetry and thermodynamics of living systems

    International Nuclear Information System (INIS)

    Lamprecht, Ingolf

    2003-01-01

    Calorimetry of living systems and classical thermodynamics developed in parallel, from Lavoisier's early ice calorimeter experiments on guinea pigs, followed by Dubrunfaut's macrocalorimetric research of fermentation processes and Atwater-Rosa's whole-body calorimetry on humans and domestic animals, to the introduction of the famous Tian-Calvet instrument that found entrance into so many different fields of biology. In this work, six examples of living-system calorimetry and thermodynamics are presented. These are: (i) glycolytic oscillations far off the thermodynamic equilibrium; (ii) growth and energy balances in fermenting and respiring yeast cultures; (iii) direct and indirect calorimetric monitoring of electrically stimulated reptile metabolism; (iv) biologic and climatic factors influencing the temperature constancy and distribution in the mound of a wood ant colony as an example of a complex ecological system; (v) energetic considerations on the clustering of European honeybees in winter as a means to save energy and stored food as well as for their Japanese counterparts in defending against hornet predators; and (vi) energetic and evolutionary aspects of the mass specific entropy production rate, the so-called bound dissipation or psiu-function. The examples presented here are just a very personal selection of living systems from a broad spectrum at all levels of complexity. Common for all of them is that they were investigated calorimetrically on the background of classical and irreversible thermodynamics

  12. Efficacy of daytime continuous positive airway pressure titration in severe obstructive sleep apnoea.

    Science.gov (United States)

    Rudkowski, J C; Verschelden, P; Kimoff, R J

    2001-09-01

    The aim of this study was to evaluate manual nasal continuous positive airway pressure (nCPAP) titration during daytime polysomnography compared with conventional overnight titration for patients with severe obstructive sleep apnoea. Thirty-two patients who underwent daytime titration were retrospectively matched (for age, sex, body mass index and apnoea/hypopnoea index (AHI)) to a group titrated overnight during the same period. Successful titration was defined as the identification of the nCPAP level (effective nCPAP (Peff)) required to eliminate respiratory events during all sleep stages. After 3 months of therapy on nCPAP at Peff, nCPAP utilization history was obtained and a group of patients underwent a repeat polysomnogram (PSG) and completed a follow-up Epworth Sleepiness Scale (ESS) score. Initial titration was successful in 91% of daytime patients and 91% of overnight patients. The success of daytime titration was not related to diagnostic AHI or ESS score. Subjective nCPAP utilization was statistically similar in both groups. On the follow-up PSG, there were no significant differences between daytime (n=11) and overnight (n=11) patients in measures of sleep quality or respiratory disturbance. Both groups demonstrated similar and significant improvements in ESS score. These findings suggest that the effective nasal continuous positive airway pressure can be accurately established during daytime titration in a substantial proportion of severe, symptomatic obstructive sleep apnoea patients.

  13. Potentiometric Titration Method for Quantitative Determination of Hydrogen Peroxide

    National Research Council Canada - National Science Library

    Bessette, Russell R

    2005-01-01

    An electrochemical potentiometric titration method that entails titration of a known volume of a catholyte containing an unknown amount of hydrogen peroxide in a titration cell having two electrodes...

  14. Non-aqueous titration of hydroxamic acids.

    Science.gov (United States)

    Stamey, T W; Christian, R

    1966-01-01

    Benzohydroxamic acid is titrated with 0.1M tetrabutyl-anunonium hydroxide in nine non-aqueous solvents with three different indicating electrodes. The best results are obtained using dimethylformamide as solvent and platinum-platinum electrodes. Four monoprotic and three diprotic hydroxamie acids and iron(III) benzohydroxamate have been successfully titrated with this system. The effect of quantitative additions of carbon dioxide to the titrant on its apparent molarity are found to be dependent on the amount added, the strength and sample size of acid titrated and the solvent used.

  15. Isothermal calorimetry of enzymatic biodiesel reaction

    DEFF Research Database (Denmark)

    Fjerbæk Søtoft, Lene; Westh, Peter; Christensen, Knud Villy

    2010-01-01

      Isothermal calorimetry ITC has been used to investigate enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by the immobilized lipase Novozym 435 at 40°C. The ITC-experiments clearly demonstrate the possibilities of investigating complex...... and composition change in the system, the heat of reaction at 40°C for the two systems has been determined to -9.8 ± 0.9 kJ/mole biodiesel formed from rapeseed oil and methanol, and - 9.3 ± 0.7 kJ/mole when rapeseed oil and ethanol is used....

  16. Scintillating Fibre Calorimetry at the LHC

    CERN Multimedia

    2002-01-01

    Good electromagnetic and hadronic calorimetry will play a central role in an LHC detector. The lead/scintillating fibre calorimeter technique provides a fast signal response well matched to the LHC rate requirements. It can be made to give equal response for electrons and hadrons (compensation) with good electromagnetic and hadronic energy resolutions.\\\\ \\\\ The aim of this R&D proposal is to study in detail the aspects that are relevant for application of this type of calorimeter in an LHC environment, including its integration in a larger system of detectors, e.g.~projective geometry, radiation hardness, light detection, calibration and stability monitoring, electron/hadron separation.....

  17. Complexometric titration of lanthanides and yttrium

    International Nuclear Information System (INIS)

    Ionashiro, M.; Graner, C.A.F.; Zuanon Netto, J.

    1983-01-01

    The pH variation of the solution and the ammonium acetate buffering were studied when different quantities of lanthanides and yttrium were titrated with EDTA, and xylenol orange as indicator. (Author) [pt

  18. Characterization of antibody-chelator conjugates: Determination of chelator content by terbium fluorescence titration

    Energy Technology Data Exchange (ETDEWEB)

    Brandt, K.D.; Schnobrich, K.E.; Johnson, D.K. (Abbott Laboratories, Department 90M, Abbott Park, IL (United States))

    1991-01-01

    Fluorescence titrations were performed by adding varying mole ratios of terbium(III) to antibody conjugates formed by benzyl isothiocyanate derivatives of three different polyaminopolycarboxylate chelators (NTA, EDTA, and DTPA) and the results compared to values for average chelator content obtained by cobalt-57 binding assays. For two different murine monoclonal antibodies, the average chelator content obtained by terbium fluorescence titration correlated closely with that measured by the cobalt-57 binding assay. It is concluded that lanthanide fluorescence titrations provide a useful alternative to radiometal binding assays for the determination of chelator content in protein-chelator conjugates.

  19. Accurate heat capacity data at phase transitions from relaxation calorimetry

    Science.gov (United States)

    Suzuki, Hal; Inaba, Akira; Meingast, Christoph

    2010-10-01

    Extracting accurate heat capacities by conventional relaxation calorimetry at first-order or very sharp second-order phase transitions is extremely difficult. The so-called "scanning method" provides a key to overcome this challenge. Here, we introduce new corrections in the data analysis of this method. Critical examinations of the improvements are made experimentally by investigating the well-studied first-order ferroelectric phase transitions of KH 2PO 4 and BaTiO 3 using a commercial relaxation calorimeter Physical Property Measurement System (PPMS) supplied by Quantum Design. The results for KH 2PO 4 are shown to be excellent; a very sharp peak in heat capacity is obtained and the absolute values are shown to agree well with the previous results obtained by adiabatic calorimetry on much larger samples. The critical behavior of the heat capacity in the vicinity of the transition temperature, as well as the thermodynamic quantities such as the transition enthalpy and entropy, also agrees very well with the previous results. For BaTiO 3, clear hysteretic behavior of the transition is observed for heating and cooling curves.

  20. Theory of titration curves-VII The properties of derivative titration curves for strong acid-strong base and other isovalent ion-combination titrations.

    Science.gov (United States)

    Meites, T; Meites, L

    1970-06-01

    This paper deals with isovalent ion-combination titrations based on reactions that can be represented by the equation M(n+) + X(n-) --> MX, where the activity of the product MX is invariant throughout a titration, and with the derivative titration curves obtained by plotting d[M(+)]/dfversus f for such titrations. It describes some of the ways in which such curves can be obtained; it compares and contrasts them both with potentiometric titration curves, which resemble them in shape, and with segmented titration curves, from which they are derived; and it discusses their properties in detail.

  1. Analysis of rotator phase transitions in the linear alkanes hexacosane to triacontane by adiabatic scanning calorimetry and by photopyroelectric calorimetry

    Science.gov (United States)

    Paoloni, S.; Mercuri, F.; Zammit, U.; Leys, J.; Glorieux, C.; Thoen, J.

    2018-03-01

    The study of the nature of various phase transitions between rotator phases in several linear alkanes was performed by analyzing the hysteretic behavior of the specific heat between heating and cooling measurements. The investigations have been carried out by both adiabatic scanning calorimetry and photopyroelectric calorimetry techniques, whose combined use has provided complementary information concerning the changes occurring in the samples' structure during their temperature change. The study enabled to establish that, unlike what previously reported, the Riii-Riv and the Rii-Riv transitions are of first order, despite them not showing any sharp peak profile in the temperature dependence of the specific heat. The first order of the Rv-Rii transition was confirmed also in the present study and, finally the Rv-Riii transition could be observed by calorimetric detection for the first time and shown to be of second order. The obtained results were discussed in terms of order parameters power terms in the Landau free energy expansion.

  2. Non-Aqueous Titration Method for Determining Suppressor Concentration in the MCU Next Generation Solvent (NGS)

    International Nuclear Information System (INIS)

    Taylor-Pashow, Kathryn M. L.; Jones, Daniel H.

    2017-01-01

    A non-aqueous titration method has been used for quantifying the suppressor concentration in the MCU solvent hold tank (SHT) monthly samples since the Next Generation Solvent (NGS) was implemented in 2013. The titration method measures the concentration of the NGS suppressor (TiDG) as well as the residual tri-n-octylamine (TOA) that is a carryover from the previous solvent. As the TOA concentration has decreased over time, it has become difficult to resolve the TiDG equivalence point as the TOA equivalence point has moved closer. In recent samples, the TiDG equivalence point could not be resolved, and therefore, the TiDG concentration was determined by subtracting the TOA concentration as measured by semi-volatile organic analysis (SVOA) from the total base concentration as measured by titration. In order to improve the titration method so that the TiDG concentration can be measured directly, without the need for the SVOA data, a new method has been developed that involves spiking of the sample with additional TOA to further separate the two equivalence points in the titration. This method has been demonstrated on four recent SHT samples and comparison to results obtained using the SVOA TOA subtraction method shows good agreement. Therefore, it is recommended that the titration procedure be revised to include the TOA spike addition, and this to become the primary method for quantifying the TiDG.

  3. Non-Aqueous Titration Method for Determining Suppressor Concentration in the MCU Next Generation Solvent (NGS)

    Energy Technology Data Exchange (ETDEWEB)

    Taylor-Pashow, Kathryn M. L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Jones, Daniel H. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-10-23

    A non-aqueous titration method has been used for quantifying the suppressor concentration in the MCU solvent hold tank (SHT) monthly samples since the Next Generation Solvent (NGS) was implemented in 2013. The titration method measures the concentration of the NGS suppressor (TiDG) as well as the residual tri-n-octylamine (TOA) that is a carryover from the previous solvent. As the TOA concentration has decreased over time, it has become difficult to resolve the TiDG equivalence point as the TOA equivalence point has moved closer. In recent samples, the TiDG equivalence point could not be resolved, and therefore, the TiDG concentration was determined by subtracting the TOA concentration as measured by semi-volatile organic analysis (SVOA) from the total base concentration as measured by titration. In order to improve the titration method so that the TiDG concentration can be measured directly, without the need for the SVOA data, a new method has been developed that involves spiking of the sample with additional TOA to further separate the two equivalence points in the titration. This method has been demonstrated on four recent SHT samples and comparison to results obtained using the SVOA TOA subtraction method shows good agreement. Therefore, it is recommended that the titration procedure be revised to include the TOA spike addition, and this to become the primary method for quantifying the TiDG.

  4. Coulometric titration at low temperatures-nonstoichiometric silver selenide

    OpenAIRE

    Beck, Gesa K.; Janek, Jürgen

    2003-01-01

    A modified coulometric titration technique is described for the investigation of nonstoichiometric phases at low temperatures. It allows to obtain titration curves at temperatures where the conventional coulometric titration technique fails because of too small chemical diffusion coefficients of the mobile component. This method for indirect coulometric titration is applied to silver selenide between -100 and 100 °C. The titration curves are analyzed on the basis of a defect chemical model an...

  5. Bipolar monolithic preamplifiers for SSC silicon calorimetry

    International Nuclear Information System (INIS)

    Britton, C.L. Jr.; Todd, R.A.; Bauer, M.L.; Kennedy, E.J.; Bugg, W.M.

    1990-01-01

    This paper describes preamplifiers designed specifically to address the requirements of silicon calorimetry for the Superconducting Super Collider (SSC). Eight different preamplifiers designed for detector capacitances ranging from 20 pF to 500 pF and operating temperatures from 25 degree C to -20 degree C are discussed. The preamplifiers were fabricated with two different high-frequency processes (one with the VTC, Inc. VJ900 process, seven with the Harris Semiconductor VHF Process). The different topologies and their features are discussed in addition to the design methodologies employed. The results for noise, power consumption, speed, and radiation damage effects as well as data for post-damage annealing are presented for the VTC process preamplifier. Simulations for the VHF Process circuits are presented. This work was funded through SSC Generic Detector funding, SSC Detector Subsystem funding, and the Oak Ridge National Laboratory (ORNL) Detector Center

  6. Imaging hadron calorimetry for future Lepton Colliders

    Energy Technology Data Exchange (ETDEWEB)

    Repond, José, E-mail: repond@hep.anl.gov

    2013-12-21

    To fully exploit the physics potential of a future Lepton Collider requires detectors with unprecedented jet energy and dijet-mass resolution. To meet these challenges, detectors optimized for the application of Particle Flow Algorithms (PFAs) are being designed and developed. The application of PFAs, in turn, requires calorimeters with very fine segmentation of the readout, so-called imaging calorimeters. This talk reviews progress in imaging hadron calorimetry as it is being developed for implementation in a detector at a future Lepton Collider. Recent results from the large prototypes built by the CALICE Collaboration, such as the Scintillator Analog Hadron Calorimeter (AHCAL) and the Digital Hadron Calorimeters (DHCAL and SDHCAL) are being presented. In addition, various R and D efforts beyond the present prototypes are being discussed.

  7. Calorimetry for Fast Authentication of Edible Oils

    Science.gov (United States)

    Angiuli, Marco; Bussolino, Gian Carlo; Ferrari, Carlo; Matteoli, Enrico; Righetti, Maria Cristina; Salvetti, Giuseppe; Tombari, Elpidio

    2009-06-01

    There are little data in the literature on how to authenticate edible oils through calorimetry techniques. However, oil melting curves can be used to represent correlations between calorimetric results and oil quality. A calorimetric method has been developed for studying the solid-liquid phase transitions of olive oil and seed oils, in which melting peak behavior is correlated to the type, quality, and composition of the oil. Good reproducible thermograms were obtained by defining precise protocols for use in testing, which take into account the specific characteristics of a particular oil. This approach does not replace classical analytical methods; nevertheless, it is believed that calorimetric tests could be a useful preliminary stage for quality testing. The calorimetric technique allows the detection of the adulterant (seed oils or refined olive oil), oil origin, and possible photo-oxidation degradation processes, before more complex and expensive procedures and analyses are applied.

  8. Isothermal calorimetry on enzymatic biodiesel production

    DEFF Research Database (Denmark)

    Fjerbæk, Lene

    2008-01-01

    information about effects taking place when using lipases immobilized on an inert carrier for transesterification of a triglyceride and an alcohol as for biodiesel production. The biodiesel is produced by rapeseed oil and methanol as well as ethanol and a commercial biocatalyst Novozym 435 from Novozymes...... containing a Candida Antarctica B lipase immobilized on an acrylic resin. The reaction investigated is characterized by immiscible liquids (oil, methanol, glycerol and biodiesel) and enzymes imm. on an inert carrier during reaction, which allows several effects to take place that during normal reaction...... conditions can not be elucidated. These effects have been observed with isothermal calorimetry bringing forth new information about the reaction of enzymes catalyzing transesterification. Enzymatic biodiesel production has until now not been investigated with isothermal microcalorimetry, but the results...

  9. CMS Forward Calorimetry R&D

    Energy Technology Data Exchange (ETDEWEB)

    Bilki, Burak [Univ. of Iowa, Iowa City, IA (United States); Argonne National Lab. (ANL), Argonne, IL (United States)

    2013-11-11

    This is a technical scope of work (TSW) between the Fermi National Accelerator Laboratory (Fermilab) and the experimenters of the CMS Forward Calorimetry Taskforce (FCAL group) who have committed to participate in beam tests to be carried out during the 2013-2016 Fermilab Test Beam Facility program. The TSW is intended primarily for the purpose of recording expectations for budget estimates and work allocations for Fermilab, the funding agencies and the participating institutions. It reflects an arrangement that currently is satisfactory to the parties; however, it is recognized and anticipated that changing circumstances of the evolving research program will necessitate revisions. The parties agree to modify this scope of work to reflect such required adjustments. Actual contractual obligations will be set forth in separate documents.

  10. End-point construction and systematic titration error in linear titration curves-complexation reactions

    NARCIS (Netherlands)

    Coenegracht, P.M.J.; Duisenberg, A.J.M.

    The systematic titration error which is introduced by the intersection of tangents to hyperbolic titration curves is discussed. The effects of the apparent (conditional) formation constant, of the concentration of the unknown component and of the ranges used for the end-point construction are

  11. Complexation of Phenols and Thiophenol by Phosphine Oxides and Phosphates. Extraction, Isothermal Titration Calorimetry, and ab Initio Calculations

    NARCIS (Netherlands)

    Cuypers, R.; Burghoff, B.; Marcelis, A.T.M.; Sudhölter, E.J.R.; Haan, de A.B.; Zuilhof, H.

    2008-01-01

    To develop a new solvent-impregnated resin system for the removal of phenols from water the complex formation of triisobutylphosphine sulfide (TIBPS), tributylphosphate (TBP), and tri-n-octylphosphine oxide (TOPO) with a series of phenols (phenol, thiophenol, 3-chlorophenol, 3,5-dichlorophenol,

  12. The Role of Water in Protein-Ligand Binding: A Comprehensive Study by Crystallography and Isothermal Titration Calorimetry

    OpenAIRE

    Biela, Adam

    2012-01-01

    The aim of this work is to investigate the impact of desolvation effects on protein-ligand interactions. In all complex structures with thrombin and pyridine, it is evident that preserving the original solvation state of Asp189 is a crucial and a common feature upon binding of the pyridine inhibitors. However, the associated entropic losses are immense. In two ligand complexes even disordered ligand portions are found in the S1 ...

  13. Use of isothermal titration calorimetry to study the interaction of short-chain alcohols with lipid membranes

    DEFF Research Database (Denmark)

    Trandum, Christa; Westh-Andersen, Peter; Jørgensen, Kent

    1999-01-01

    The molecular mechanisms by which ethanol and other short-chain alcohols exert their effect in biological systems have been suggested to involve specific interactions with proteins and/or non-specific interactions with the lipid bilayer part of the cell membrane. To gain insight into the effect...

  14. Detection of conformational changes in immunoglobulin G using isothermal titration calorimetry with low-molecular-weight probes

    NARCIS (Netherlands)

    Rispens, Theo; Lakemond, Catriona M. M.; Derksen, Ninotska I. L.; Aalberse, Rob C.

    2008-01-01

    Proteins for therapeutic use may contain small amounts of partially misfolded monomeric precursors to postproduction aggregation. To detect these misfolded proteins in the presence of an excess of properly folded protein, fluorescent probes such as 8-anilino-1-naphthalene sulfonate (ANS) are

  15. Hydroxylamine nitrate self-catalytic kinetics study with adiabatic calorimetry

    International Nuclear Information System (INIS)

    Liu Lijun; Wei Chunyang; Guo Yuyan; Rogers, William J.; Sam Mannan, M.

    2009-01-01

    Hydroxylamine nitrate (HAN) is an important member of the hydroxylamine compound family with applications that include equipment decontamination in the nuclear industry and aqueous or solid propellants. Due to its instability and autocatalytic behavior, HAN has been involved in several incidents at the Hanford and Savannah River Site (SRS) [Technical Report on Hydroxylamine Nitrate, US Department of Energy, 1998]. Much research has been conducted on HAN in different areas, such as combustion mechanism, decomposition mechanism, and runaway behavior. However, the autocatalytic decomposition behavior of HAN at runaway stage has not been fully addressed due to its highly exothermic and rapid decomposition behavior. This work is focused on extracting HAN autocatalytic kinetics and analyzing HAN critical behavior from adiabatic calorimetry measurements. A lumped autocatalytic kinetic model for HAN and associated model parameters are determined. Also the storage and handling critical conditions of diluted HAN solution without metal presence are quantified

  16. Novel investigation of enzymatic biodiesel reaction by isothermal calorimetry

    DEFF Research Database (Denmark)

    Søtoft, Lene Fjerbaek; Westh, Peter; Christensen, Knud V.

    2010-01-01

    Isothermal calorimetry (ITC) was used to investigate solvent-free enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by immobilized lipase Novozym 435 at 40 °C. The aim of the study was to determine reaction enthalpy for the enzymatic...... transesterification and to elucidate the mass transfer and energetic processes taking place. Based on the measured enthalpy and composition change in the system, the heat of reaction at 40 °C for the two systems was determined as −9.8 ± 0.9 kJ/mole biodiesel formed from rapeseed oil and methanol, and −9.3 ± 0.7 k...

  17. Low-temperature transitions in cod and tuna determined by differential scanning calorimetry

    DEFF Research Database (Denmark)

    Jensen, Kristina Nedenskov; Jørgensen, Bo; Nielsen, Jette

    2003-01-01

    Differential scanning calorimetry measurements have revealed different thermal transitions in cod and tuna samples. Transition temperatures detected Lit -11degreesC, -15degreesC and -21degreesC were highly dependent on the annealing temperature. In tuna muscle an additional transition was observed...

  18. Coulometry and Calorimetry of Electric Double Layer Formation in Porous Electrodes

    NARCIS (Netherlands)

    Janssen, Mathijs; Griffioen, Elian; Biesheuvel, P. M.; Van Roij, René; Erné, Ben

    2017-01-01

    Coulometric measurements on salt-water-immersed nanoporous carbon electrodes reveal, at a fixed voltage, a charge decrease with increasing temperature. During far-out-of-equilibrium charging of these electrodes, calorimetry indicates the production of both irreversible Joule heat and reversible

  19. Chemical calibration of Isothermal Titration Calorimeters: An evaluation of the dilution of propan-1-ol into water as a test reaction using different calorimeters, concentrations, and temperatures

    International Nuclear Information System (INIS)

    Adão, Regina; Bai, Guangyue; Loh, Watson; Bastos, Margarida

    2012-01-01

    Highlights: ► We address the importance of test reactions in Isothermal Titration Calorimetry. ► We re-evaluate a test reaction and provide a new value for it at 308.15 K. ► Different concentrations are tested to account for instrument sensitivity. ► We compare the performance of two very sensitive calorimeters of different design. ► We suggest appropriate experimental conditions for the use of this test reaction. - Abstract: The use of a good chemical calibration or test reaction in Isothermal Titration Calorimetry is crucial for getting reliable enthalpy values that can be compared across different laboratories. Indeed most titration calorimeters are used to measure both equilibrium constants and molar enthalpies of reaction. But a necessary prerequisite for such measurements is to first perform the enthalpy measurement accurately and precisely. The values of the equilibrium constant(s) are then calculated by regression from an appropriate model. As such, we found it timely to extensively test a previously proposed test reaction, the dilution of propan-1-ol into water, using two calorimeters of different design (heat conduction and power compensation calorimeters) and sensitivity. Experiments were performed at 298.15 K for the previously suggested 10% mass fraction propan-1-ol solution, as well as for the lower concentrations of 5% and 2% mass fractions. Due to our capacity to use insertion heaters with one of the used calorimeters, which allows for very accurate calibration constants to be obtained, we also determined a value for the enthalpy of dilution of 10% mass fraction solution at 308.15 K, previously not available, and closer to the temperatures commonly used in titration experiments involving biological samples. The observed change in the enthalpy of dilution was found to decrease in absolute value, but to an extent that did not justify the determination of new values for the less concentrated solutions. The values obtained with the two

  20. An accurate potentiometric titration of 5-25 mg uranium

    International Nuclear Information System (INIS)

    Slanina, J.; Bakker, F.; Lingerak, W.A.

    1976-01-01

    A potentiometric titration of 5 to 25 mg uranium is described. Sulphamic and phosphoric acid are added to the sample (volume 1 ml), U VI is reduced to U IV by Fe 2+ and the excess of Fe 2+ is oxidized by a mixture of nitric acid, sulphamic acid and ammonium molybdate; vanadyl sulphate is added to ensure a sharp end-point of the titration. The resultant U IV is titrated automatically with 0.02500N potassiumdichromate using a platinum indicator electrode. The automatic titration is performed both with a commercial titrator (Mettler) and with an R.C.N. titrator which waits after each addition until the equilibrium is reached. Using the Mettler titrator an accuracy of 0.05% relative was reached. The R.C.N. setpoint titrator gave results with an accuracy of 0.04% relative at the 20-mg U level. Each titration takes 5 to 7 min. (author)

  1. Considerations for Calorimetry at a Super B Factory

    Energy Technology Data Exchange (ETDEWEB)

    Wisniewski, William

    2003-09-18

    The study of B physics at e{sup +}e{sup -} colliders running the {Upsilon} region imposes significant performance requirements on calorimetry. The environment of a very high luminosity B factor further restricts calorimetry choices. Calorimeter design is discussed in light of these constraints. A solution using scintillating crystals is explored.

  2. Studies of factors affecting uranium determinations by automated coulometric titration (New Brunswick Laboratory/Davies--Gray Method)

    International Nuclear Information System (INIS)

    Harrar, J.E.; Boyle, W.G.

    1976-01-01

    The method's errors are defined to ascertain its absolute accuracy. An analytical technique was developed to examine vanadyl sulfate diluent for vanadium (V). None could be found in any of the lots tested. Certain lots of reagent-grade phosphoric acid contained an unidentified impurity that caused high generator-electrode potentials and a positive error. The current-potential characteristics of the generator electrode were measured. The data indicated that a significant fraction of uranium (IV) was oxidized directly during the early stages of titration. Using equations theoretically applicable to such a titration, a negligible difference was found between the inflection point of the titration curve and the equivalence point in the titration. However, the actual experimental curves did not agree with the theoretical curves early in the titration. Measurements of the background current indicated a level equivalent to approximately 0.2 mg uranium. The evaluation of the reagent delivery system used in the automated analyzer revealed adequate reproducibility. 8 tables

  3. Multi-slope warm-up calorimetry of Integrated Dewar-Detector Assemblies

    Science.gov (United States)

    Veprik, Alexander; Shlomovich, Baruch; Tuito, Avi

    2015-05-01

    Boil-off isothermal calorimetry of Integrated Dewar-Detector Assemblies (IDDA) is a routine part of acceptance testing. In this traditional approach, the cryogenic liquid coolant (typically LN2) is allowed to naturally boil off from the Dewar well to the atmosphere. The parasitic heat load is then evaluated as the product of the latent heat of vaporization and the "last drop" boil-off rate monitored usually by a mass flow meter. An inherent limitation of this technique is that it is applicable only at the fixed boiling temperature of the chosen liquid coolant, for example, 77K for LN2. There is a need, therefore, to use other (often exotic) cryogenic liquids when calorimetry is needed at temperatures other than 77K. A further drawback is related to the transitional nature of last drop boiling, which manifests itself in development of enlarged bubbles, explosions and geysering. This results in an uneven flow rate and also affects the natural temperature gradient along the cold finger. Additionally, mass flow meters are known to have limited measurement accuracy. The above considerations especially hold true for advanced High Operational Temperature IDDAs, typically featuring short cold fingers and working at 150K and above. In this work, we adapt the well-known technique of dual-slope calorimetry and show how accurate calorimetry may be performed by precooling the IDDA and comparing the warm-up slopes of the thermal transient processes under different trial added heat loads. Because of the simplicity, accuracy and ability to perform calorimetry literally at any temperature of interest, this technique shows good potential for replacing traditional boil-off calorimetry.

  4. National absorbed dose to water references for radiotherapy medium energy X-rays by water calorimetry

    International Nuclear Information System (INIS)

    Perichon, N.

    2012-01-01

    LNE-LNHB current references for medium energy X-rays are established in terms of air kerma. Absorbed dose to water, which is the quantity of interest for radiotherapy, is obtained by transfer dosimetric techniques following a methodology described in international protocols. The aim of the thesis is to establish standards in terms of absorbed dose to water in the reference protocol conditions by water calorimetry. The basic principle of water calorimetry is to measure the absorbed dose from the rise in temperature of water under irradiation. A calorimeter was developed to perform measurements at a 2 cm depth in water according to IAEA TRS-398 protocol for medium energy x-rays. Absorbed dose rates to water measured by calorimetry were compared to the values established using protocols based on references in terms of air kerma. A difference lower than 2.1% was reported. Standard uncertainty of water calorimetry being 0.8%, the one associated to the values from protocols being around 3.0%, results are consistent considering the uncertainties. Thanks to these new standards, it will be possible to use IAEA TRS-398 protocol to determine absorbed dose to water: a significant reduction of uncertainties is obtained (divided by 3 by comparison with the application of the IAEA TRS-277 protocol). Currently, none of the counterparts' laboratories own such an instrument allowing direct determination of standards in the reference conditions recommended by the international radiotherapy protocols. (author) [fr

  5. Comparison of VFA titration procedures used for monitoring the biogas process.

    Science.gov (United States)

    Lützhøft, Hans-Christian Holten; Boe, Kanokwan; Fang, Cheng; Angelidaki, Irini

    2014-05-01

    Titrimetric determination of volatile fatty acids (VFAs) contents is a common way to monitor a biogas process. However, digested manure from co-digestion biogas plants has a complex matrix with high concentrations of interfering components, resulting in varying results when using different titration procedures. Currently, no standardized procedure is used and it is therefore difficult to compare the performance among plants. The aim of this study was to evaluate four titration procedures (for determination of VFA-levels of digested manure samples) and compare results with gas chromatographic (GC) analysis. Two of the procedures are commonly used in biogas plants and two are discussed in literature. The results showed that the optimal titration results were obtained when 40 mL of four times diluted digested manure was gently stirred (200 rpm). Results from samples with different VFA concentrations (1-11 g/L) showed linear correlation between titration results and GC measurements. However, determination of VFA by titration generally overestimated the VFA contents compared with GC measurements when samples had low VFA concentrations, i.e. around 1 g/L. The accuracy of titration increased when samples had high VFA concentrations, i.e. around 5 g/L. It was further found that the studied ionisable interfering components had lowest effect on titration when the sample had high VFA concentration. In contrast, bicarbonate, phosphate and lactate had significant effect on titration accuracy at low VFA concentration. An extended 5-point titration procedure with pH correction was best to handle interferences from bicarbonate, phosphate and lactate at low VFA concentrations. Contrary, the simplest titration procedure with only two pH end-points showed the highest accuracy among all titration procedures at high VFA concentrations. All in all, if the composition of the digested manure sample is not known, the procedure with only two pH end-points should be the procedure of

  6. Inherent limitations of fixed-time, servo-controlled radiometric calorimetry

    International Nuclear Information System (INIS)

    Wetzel, J.R.; Lemming, J.F.; Duff, M.F.

    1987-01-01

    Interest has been shown in using fixed-time, servo-controlled calorimetry to shorten the measurement times for certain samples that require low precision values (3 to 5%). This type of calorimeter measurement could be particularly useful for screening scrap samples to determine whether there is a need for a more accurate measurement or for certain confirmatory measurements for which low precision numbers are sufficient. The equipment required for this type of measurement is a servo-controlled calorimeter and a preconditioning unit. Samples to be measured are placed in the preconditioning unit, which is maintained at the internal temperature of the calorimeter. The power value for the sample is determined at a fixed time after loading into the calorimeter, for example, 30 min. When a calorimeter is operated using a fixed cutoff time, there are additional sources of uncertainty that need to be considered. The major factors affecting the uncertainty of the calorimetry power values are discussed. 2 refs., 4 figs

  7. Titrated Misoprostol Versus Dinoprostone for Labor Induction

    African Journals Online (AJOL)

    . Studied women were randomized into; Group I: 104 women included and received oral 200 µg misoprostol in 200 ml water titrated over 12 h and Group II: 108 women included and received vaginal dinoprostone tablet (3 mg) maximum two ...

  8. Titration Calculations with Computer Algebra Software

    Science.gov (United States)

    Lachance, Russ; Biaglow, Andrew

    2012-01-01

    This article examines the symbolic algebraic solution of the titration equations for a diprotic acid, as obtained using "Mathematica," "Maple," and "Mathcad." The equilibrium and conservation equations are solved symbolically by the programs to eliminate the approximations that normally would be performed by the student. Of the three programs,…

  9. NBL-Davies-Gray weight titration method

    International Nuclear Information System (INIS)

    Hassell, C.

    1981-01-01

    The titration method for uranium consists of the following basic steps: reduction of U +6 to U +4 by Fe +2 ; selective oxidation of excess Fe +2 by HNO 3 with Mo +6 catalyst, all in strong phosphoric acid solution; and titration of the U +4 with standard dichromate after dilution. In this paper, detailed procedure of the NBL method, its modification to a gravimetric system or weight titration technique, and miniaturization of the NBL titrimetric method are discussed. Improved precisions and accuracy (2 to 3 times), of the gravimetric titrant delivery has made it possible to reduce the amount of uranium taken for each analysis. At present, using gravimetric delivery, most samples are titrated in the 30 to 50 mg range. Improved precision has led to investigating the possibility of a scaled-down version of the basic method so as to reduce the volume of phosphoric acid waste generated. Because all reactions are carried out in the same vessel, this method can be automated. Analysts at NBL have been able to restrict error to 0.05% or better in the 30 to 100 mg range using the basic procedure

  10. Coulometric titration of ketotifen in tablets.

    Science.gov (United States)

    Ciesielski, W; Zakrzewski, R; Złobińska, U

    2005-03-01

    A method for the determination of ketotifen involving its reaction with iodine in an alkaline medium is presented. In coulometric titration using biamperometric end-point detection 0.25-2 micromol (77-618 microg) of ketotifen was successfully determined. The elaborated method was applied to the determination of ketotifen in drugs.

  11. Process monitored spectrophotometric titration coupled with chemometrics for simultaneous determination of mixtures of weak acids.

    Science.gov (United States)

    Liao, Lifu; Yang, Jing; Yuan, Jintao

    2007-05-15

    A new spectrophotometric titration method coupled with chemometrics for the simultaneous determination of mixtures of weak acids has been developed. In this method, the titrant is a mixture of sodium hydroxide and an acid-base indicator, and the indicator is used to monitor the titration process. In a process of titration, both the added volume of titrant and the solution acidity at each titration point can be obtained simultaneously from an absorption spectrum by least square algorithm, and then the concentration of each component in the mixture can be obtained from the titration curves by principal component regression. The method only needs the information of absorbance spectra to obtain the analytical results, and is free of volumetric measurements. The analyses are independent of titration end point and do not need the accurate values of dissociation constants of the indicator and the acids. The method has been applied to the simultaneous determination of the mixtures of benzoic acid and salicylic acid, and the mixtures of phenol, o-chlorophenol and p-chlorophenol with satisfactory results.

  12. Antiepileptic Drug Titration and Related Health Care Resource Use and Costs.

    Science.gov (United States)

    Fishman, Jesse; Kalilani, Linda; Song, Yan; Swallow, Elyse; Wild, Imane

    2018-02-27

    Unexpected breakthrough seizures resulting from suboptimal antiepileptic drug (AED) dosing during the titration period, as well as adverse events resulting from rapid AED titration, may influence the titration schedule and significantly increase health care resource use (HRU) and health care costs. To assess the relationship between AEDs, HRU, and costs during AED titration and maintenance. Practicing neurologists were recruited from a nationwide panel to provide up to 3 patient records each for this retrospective medical chart review. Patients with epilepsy who were aged ≥ 18 years and had initiated an AED between January 1, 2014, and January 1, 2016, were followed for 6 months from AED initiation. Titration duration was the time from AED initiation to the beginning of treatment maintenance as determined by the physician. Outcomes were epilepsy-specific HRU (hospitalizations, emergency department visits, outpatient visits, physician referral, laboratory testing/diagnostic imaging, and phone calls) and related costs that occurred during the titration or maintenance treatment periods. Of 811 patients, 156, 128, 125, 120, 114, 107, and 61 initiated the following AEDs: levetiracetam, lamotrigine, lacosamide, valproate, topiramate, carbamazepine, and phenytoin, respectively. Most patients (619/803 [77.1%] with complete AED data) received monotherapy. Baseline characteristics were similar across AEDs (mean [SD] age, 36.6 [14.4] years; 59.0% male). Kaplan-Meier estimates of titration duration ranged from 3.3 weeks (phenytoin) to 8.1 weeks (lamotrigine). From titration to maintenance, the overall incidence of HRU per person-month decreased 54.5%-89.3% for each HRU measure except outpatient visits (24.6% decrease). Total epilepsy-related costs decreased from $80.48 to $42.77 per person-month, or 46.9% from titration to maintenance. AED titration periods had higher HRU rates and costs than AED maintenance, suggesting that use of AEDs with shorter titration requirements

  13. Applying fast calorimetry on a spent nuclear fuel calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Liljenfeldt, Henrik [Swedish Nuclear Fuel and Waste Management (Sweden); Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Uppsala Univ. (Sweden)

    2015-04-15

    Recently at Los Alamos National Laboratory, sophisticated prediction algorithms have been considered for the use of calorimetry for treaty verification. These algorithms aim to predict the equilibrium temperature based on early data and therefore be able to shorten the measurement time while maintaining good accuracy. The algorithms have been implemented in MATLAB and applied on existing equilibrium measurements from a spent nuclear fuel calorimeter located at the Swedish nuclear fuel interim storage facility. The results show significant improvements in measurement time in the order of 15 to 50 compared to equilibrium measurements, but cannot predict the heat accurately in less time than the currently used temperature increase method can. This Is both due to uncertainties in the calibration of the method as well as identified design features of the calorimeter that limits the usefulness of equilibrium type measurements. The conclusions of these findings are discussed, and suggestions of both improvements of the current calorimeter as well as what to keep in mind in a new design are given.

  14. An Olfactory Indicator for Acid-Base Titrations.

    Science.gov (United States)

    Flair, Mark N.; Setzer, William N.

    1990-01-01

    The use of an olfactory acid-base indicator in titrations for visually impaired students is discussed. Potential olfactory indicators include eugenol, thymol, vanillin, and thiophenol. Titrations performed with each indicator with eugenol proved to be successful. (KR)

  15. Test of calorimetry for high burn-up plutonium

    International Nuclear Information System (INIS)

    Beets, C.; Carchon, R.; Fettweis, P.

    1984-01-01

    In recent times, the interest of applying calorimetry for safeguards purpose is steadily increasing. Calorimetric measurements have been performed on a set of high burn-up (25000 MWd/t) Pu samples, ranging in mass between 60 g and 2.5 kg Pu, distributed as PuO 2 powder embedded in stainless steel containers. The powers produced by these containers ranged between 0.8 W and 36 W. The calorimeter used was the Mound 150 type, and the isotopics and the Am content have been determined earlier by mass spectroscopy, completed with α and γ counting, and were later verified by the same methods. Watts/gram measurements were made on twelve 60 g samples of the same plutonium lot to demonstrate the Pu elemental and isotopic homogeneity, and hence, its suitability for subsequent NDA experiments. These samples were also measured in a stacked way to fill up the mass and wattage gaps between 60 g (0.8W) and 1 kg (14W). Calorimetric assay values, obtained with both isotopic measurements are discussed

  16. Microculture virus titration--a simple colourimetric assay for influenza virus titration.

    Science.gov (United States)

    Levi, R; Beeor-Tzahar, T; Arnon, R

    1995-03-01

    Influenza antigens can be detected by several well established methods. However, when it is important to determine the titre of infective virions, a bioassay should be employed. The standard and the most widely used tests for influenza infectivity are titration carried out in embryonated hen eggs, or the plaque assay employing tissue culture techniques. A simple colourimetric assay for influenza virus detection and titration is described. Samples of allantoic fluid or mice lung homogenates were used to infect MDCK cultures in microplate wells. After an incubation period, the tetrazolium (MTT) colourimetric assay was used to determine cell viability, and when compared to untreated culture control enabled the detection and titration of several influenza strains. When samples were assayed simultaneously in embryonated eggs and by the MCVT method, good correlation in determined titres was obtained. The availability of an additional method for influenza titration allows more flexibility in the choice of titration method according to the specific needs of the study. Furthermore, this method lends itself to full automatization. Similar procedures should also be applicable to titration of other cytopathic viruses.

  17. Ion-selective electrodes in potentiometric titrations; a new method for processing and evaluating titration data.

    Science.gov (United States)

    Granholm, Kim; Sokalski, Tomasz; Lewenstam, Andrzej; Ivaska, Ari

    2015-08-12

    A new method to convert the potential of an ion-selective electrode to concentration or activity in potentiometric titration is proposed. The advantage of this method is that the electrode standard potential and the slope of the calibration curve do not have to be known. Instead two activities on the titration curve have to be estimated e.g. the starting activity before the titration begins and the activity at the end of the titration in the presence of large excess of titrant. This new method is beneficial when the analyte is in a complexed matrix or in a harsh environment which affects the properties of the electrode and the traditional calibration procedure with standard solutions cannot be used. The new method was implemented both in a method of linearization based on the Grans's plot and in determination of the stability constant of a complex and the concentration of the complexing ligand in the sample. The new method gave accurate results when using titrations data from experiments with samples of known composition and with real industrial harsh black liquor sample. A complexometric titration model was also developed. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. The CLEO-III Trigger: Calorimetry and tracking

    International Nuclear Information System (INIS)

    Bergfeld, T.J.; Gollin, G.D.; Haney, M.J.

    1996-01-01

    The CLEO-III Trigger provides a trigger decision every 42ns, with a latency of approximately 2.5μs. This paper describes the pipelined signal processing and pattern recognition schemes used by the calorimeter, and the axial and stereo portions of the drift chamber, to provide the information necessary to make these decisions. Field programmable gate arrays are used extensively to provide cluster filtering and location sorting for calorimetry, and path finding for tracking. Analog processing is also employed in the calorimetry to provide additional leverage on the problem. Timing information is extracted from both calorimetry and tracking

  19. Potentiometric determination of milligram amounts of uranium by semiautomatic titrator

    International Nuclear Information System (INIS)

    Ryzhinskij, M.V.; Stepanov, A.V.; Preobrazhenskaya, L.D.; Solntseva, L.F.; Gromova, E.A.

    1978-01-01

    A semiautomatic titrator is described which allows gravimetriotentiometricc-p titrat mg amounts of substances. Milligram amounts of uranium (absolute contents and oxygen/uranium ratio) in U 3 O 8 were determined as an example of the titrator action. The relative standard deviation was less than 0.001

  20. Thermodynamics of binding interactions between extracellular polymeric substances and heavy metals by isothermal titration microcalorimetry.

    Science.gov (United States)

    Yan, Peng; Xia, Jia-Shuai; Chen, You-Peng; Liu, Zhi-Ping; Guo, Jin-Song; Shen, Yu; Zhang, Cheng-Cheng; Wang, Jing

    2017-05-01

    Extracellular polymeric substances (EPS) play a crucial role in heavy metal bio-adsorption using activated sludge, but the interaction mechanism between heavy metals and EPS remains unclear. Isothermal titration calorimetry was employed to illuminate the mechanism in this study. The results indicate that binding between heavy metals and EPS is spontaneous and driven mainly by enthalpy change. Extracellular proteins in EPS are major participants in the binding process. Environmental conditions have significant impact on the adsorption performance. Divalent and trivalent cations severely impeded the binding of heavy metal ions to EPS. Electrostatic interaction mainly attributed to competition between divalent cations and heavy metal ions; trivalent cations directly competed with heavy metal ions for EPS binding sites. Trivalent cations were more competitive than divalent cations for heavy metal ion binding because they formed complexing bonds. This study facilitates a better understanding about the interaction between heavy metals and EPS in wastewater treatment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. A bipolar monolithic preamplifier for high-capacitance SSC [Superconducting Super Collider] silicon calorimetry

    International Nuclear Information System (INIS)

    Britton, C.L. Jr.; Kennedy, E.J.; Bugg, W.M.

    1990-01-01

    This paper describes a preamplifier designed and fabricated specifically to address the requirements of silicon calorimetry for the Superconducting Super Collider (SSC). The topology and its features are discussed in addition to the design methodology employed. The simulated and measured results for noise, power consumption, and speed are presented. Simulated an measured data for radiation damage effects as well as data for post-damage annealing are also presented. 8 refs., 7 figs., 2 tabs

  2. A titration model for evaluating calcium hydroxide removal techniques

    Directory of Open Access Journals (Sweden)

    Mark PHILLIPS

    2015-02-01

    Full Text Available Objective Calcium hydroxide (Ca(OH2 has been used in endodontics as an intracanal medicament due to its antimicrobial effects and its ability to inactivate bacterial endotoxin. The inability to totally remove this intracanal medicament from the root canal system, however, may interfere with the setting of eugenol-based sealers or inhibit bonding of resin to dentin, thus presenting clinical challenges with endodontic treatment. This study used a chemical titration method to measure residual Ca(OH2 left after different endodontic irrigation methods. Material and Methods Eighty-six human canine roots were prepared for obturation. Thirty teeth were filled with known but different amounts of Ca(OH2 for 7 days, which were dissolved out and titrated to quantitate the residual Ca(OH2 recovered from each root to produce a standard curve. Forty-eight of the remaining teeth were filled with equal amounts of Ca(OH2 followed by gross Ca(OH2 removal using hand files and randomized treatment of either: 1 Syringe irrigation; 2 Syringe irrigation with use of an apical file; 3 Syringe irrigation with added 30 s of passive ultrasonic irrigation (PUI, or 4 Syringe irrigation with apical file and PUI (n=12/group. Residual Ca(OH2 was dissolved with glycerin and titrated to measure residual Ca(OH2 left in the root. Results No method completely removed all residual Ca(OH2. The addition of 30 s PUI with or without apical file use removed Ca(OH2 significantly better than irrigation alone. Conclusions This technique allowed quantification of residual Ca(OH2. The use of PUI (with or without apical file resulted in significantly lower Ca(OH2 residue compared to irrigation alone.

  3. Titration ELISA as a Method to Determine the Dissociation Constant of Receptor Ligand Interaction.

    Science.gov (United States)

    Eble, Johannes A

    2018-02-15

    The dissociation constant describes the interaction between two partners in the binding equilibrium and is a measure of their affinity. It is a crucial parameter to compare different ligands, e.g., competitive inhibitors, protein isoforms and mutants, for their binding strength to a binding partner. Dissociation constants are determined by plotting concentrations of bound versus free ligand as binding curves. In contrast, titration curves, in which a signal that is proportional to the concentration of bound ligand is plotted against the total concentration of added ligand, are much easier to record. The signal can be detected spectroscopically and by enzyme-linked immunosorbent assay (ELISA). This is exemplified in a protocol for a titration ELISA that measures the binding of the snake venom-derived rhodocetin to its immobilized target domain of α2β1 integrin. Titration ELISAs are versatile and widely used. Any pair of interacting proteins can be used as immobilized receptor and soluble ligand, provided that both proteins are pure, and their concentrations are known. The difficulty so far has been to determine the dissociation constant from a titration curve. In this study, a mathematical function underlying titration curves is introduced. Without any error-prone graphical estimation of a saturation yield, this algorithm allows processing of the raw data (signal intensities at different concentrations of added ligand) directly by mathematical evaluation via non-linear regression. Thus, several titration curves can be recorded simultaneously and transformed into a set of characteristic parameters, among them the dissociation constant and the concentration of binding-active receptor, and they can be evaluated statistically. When combined with this algorithm, titration ELISAs gain the advantage of directly presenting the dissociation constant. Therefore, they may be used more efficiently in the future.

  4. Determining a Solubility Product Constant by Potentiometric Titration to Increase Students' Conceptual Understanding of Potentiometry and Titrations

    Science.gov (United States)

    Grabowski, Lauren E.; Goode, Scott R.

    2017-01-01

    Potentiometric titrations are widely taught in first-year undergraduate courses to connect electrochemistry, stoichiometry, and equilibria and to reinforce acid-base titrations. Students perform a potentiometric titration that is then analyzed to determine analyte concentrations and the solubility product constant of the solid species.

  5. Optimal level of continuous positive airway pressure: auto-adjusting titration versus titration with a predictive equation.

    Science.gov (United States)

    Choi, Ji Ho; Jun, Young Joon; Oh, Jeong In; Jung, Jong Yoon; Hwang, Gyu Ho; Kwon, Soon Young; Lee, Heung Man; Kim, Tae Hoon; Lee, Sang Hag; Lee, Seung Hoon

    2013-05-01

    The aims of the present study were twofold. We sought to compare two methods of titrating the level of continuous positive airway pressure (CPAP) - auto-adjusting titration and titration using a predictive equation - with full-night manual titration used as the benchmark. We also investigated the reliability of the two methods in patients with obstructive sleep apnea syndrome (OSAS). Twenty consecutive adult patients with OSAS who had successful, full-night manual and auto-adjusting CPAP titration participated in this study. The titration pressure level was calculated with a previously developed predictive equation based on body mass index and apnea-hypopnea index. The mean titration pressure levels obtained with the manual, auto-adjusting, and predictive equation methods were 9.0 +/- 3.6, 9.4 +/- 3.0, and 8.1 +/- 1.6 cm H2O,respectively. There was a significant difference in the concordance within the range of +/- 2 cm H2O (p = 0.019) between both the auto-adjusting titration and the titration using the predictive equation compared to the full-night manual titration. However, there was no significant difference in the concordance within the range of +/- 1 cm H2O (p > 0.999). When compared to full-night manual titration as the standard method, auto-adjusting titration appears to be more reliable than using a predictive equation for determining the optimal CPAP level in patients with OSAS.

  6. Determination of the titratable acidity and the pH of wine based on potentiometric flow injection analysis.

    Science.gov (United States)

    Vahl, Katja; Kahlert, Heike; von Mühlen, Lisandro; Albrecht, Anja; Meyer, Gabriele; Behnert, Jürgen

    2013-07-15

    A FIA system using a pH-sensitive detector based on a graphite/quinhydrone/silicone composite electrode was applied to determine sequentially the titratable acidity and the pH of wine, as well as the sum of calcium and magnesium ions. For all measurements the same FIA configuration was used employing different carrier solutions. The results for the determination of acidity and pH are in good agreement with those obtained by classical potentiometric titrations and by pH measurements using a conventional glass electrode. The standard deviation was less than 1.5% for both kinds of measurements and the sample volume was 150 μL. The method allows about 40 determinations of titratable acidity per hour and 30 pH measurements per hour. The titration method can be adjusted to the legal requirements in USA and Europe. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Kinetic Titration Series with Biolayer Interferometry

    Science.gov (United States)

    Frenzel, Daniel; Willbold, Dieter

    2014-01-01

    Biolayer interferometry is a method to analyze protein interactions in real-time. In this study, we illustrate the usefulness to quantitatively analyze high affinity protein ligand interactions employing a kinetic titration series for characterizing the interactions between two pairs of interaction patterns, in particular immunoglobulin G and protein G B1 as well as scFv IC16 and amyloid beta (1–42). Kinetic titration series are commonly used in surface plasmon resonance and involve sequential injections of analyte over a desired concentration range on a single ligand coated sensor chip without waiting for complete dissociation between the injections. We show that applying this method to biolayer interferometry is straightforward and i) circumvents problems in data evaluation caused by unavoidable sensor differences, ii) saves resources and iii) increases throughput if screening a multitude of different analyte/ligand combinations. PMID:25229647

  8. Coulometrische titration von hypochloriten und chloraten.

    Science.gov (United States)

    Gründler, P; Holzapfel, H

    1970-03-01

    Hypochlorite was determined by direct coulometric titration with iron(II) in an acetate buffered solution. Chlorate was titrated with titanium(III) in 2M hydrochloric acid. Amperometric indication with one and two electrodes, respectively, was used. Mixtures of hypochlorites and chlorates, e.g., in industrial electrolytes, may be analysed. On a déterminé l'hypochlorite par titrage coulométrique direct avec le fer(II) dans une solution tamponnée à l'acétate. On a titré le chlorate avec le titane(III) en acide chlorhydrique 2M. On a utilisé l'indication ampérométrique une et deux électrodes respectivement. On peut analyser des mélanges d'hypochlorites et de chlorates, par exemple dans des électrolytes industriels.

  9. Spectrophotometric titration of zirconium in siliceous materials

    International Nuclear Information System (INIS)

    Sugawara, K.F.; Su, Y.-S.; Strzegowski, W.R.

    1978-01-01

    An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1 to 5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. (author)

  10. Front-End Electronics in calorimetry: from LHC to ILC

    International Nuclear Information System (INIS)

    De La Taille, Ch.

    2009-09-01

    This report summarizes the electronics developments for liquid argon calorimeter read-out at LHC and the development carried out in the framework of the CALICE collaboration for those of the future linear collider (ILC). It also includes chips designed for multi-anode photomultipliers (MaPMT) used in the OPERA experiment or on ATLAS luminometer, which also find applications in medical imaging. Started in the early 90's, the development for ATLAS calorimetry was extremely challenging in terms of readout speed, radiation tolerance and measurement accuracy. The high speed has required a new approach using current-sensitive preamplifiers instead of charge sensitive ones and the redefinition of noise performance in terms of ENI. The preamplifiers developed at Orsay and the monolithic shapers are described in Chapter 1, including considerations of digital filtering, which was a new technique in our field. Chapter 2 is dedicated to the calibration system, designed and built by Orsay, for which the high performance and accuracy necessitated in-depth studies. The 3. chapter closes the studies for ATLAS with a summary of the detector measurements which had to be carried out on the 200 000 channels in order to understand and model the detector and achieve everywhere the accuracy and uniformity at per-cent level. These developments for ATLAS ended in 2004, although parallel work was also carried out for the NA48 and DO calorimeters which are not detailed here. The next generation of collider will require a new generation of calorimeters, much more granular, referred to as 'imaging calorimetry' with embedded read-out electronics. The ASICs developed for this purpose in the framework of the CALICE collaboration are described in Chapter 4. They integrate all the functionalities of amplification, digitization and read-out making them complex 'System-On-Chip' circuits extremely efficient that find many other applications. A family of 3 chips reads out the Si-W electromagnetic

  11. Determination of milligram amounts of neptunium by potentiometric titration

    International Nuclear Information System (INIS)

    Ryzhinskij, M.V.; Solntseva, L.F.

    1981-01-01

    Two procedures of potentiometric titration of about 1 mg Np are reported which are based on its oxidation to neptunium (6) with silver (2) oxide followed by titration with iron (2) to neptunium (5) in one case and to neptunium (4) in the alternative one. The error is not greater than 0.2% rel. Ten-fold uranium excess does not interfere. Up to 1% of plutonium relative to neptunium does not interfere in the case of the titration to neptunium (5). In the titration to neptunium (4), plutonium is titrated stoichiometrically [ru

  12. Novel investigation of enzymatic biodiesel reaction by isothermal calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Sotoft, Lene Fjerbaek, E-mail: lfj@kbm.sdu.dk [Institute of Chemical Engineering, Biotechnology and Environmental Technology, University of Southern Denmark, Campusvej 55, DK-5230 Odense M (Denmark); Westh, Peter [Department of Life Science and Chemistry, Roskilde University, PO Box 260, DK-4000 Roskilde (Denmark); Christensen, Knud V.; Norddahl, Birgir [Institute of Chemical Engineering, Biotechnology and Environmental Technology, University of Southern Denmark, Campusvej 55, DK-5230 Odense M (Denmark)

    2010-03-30

    Isothermal calorimetry (ITC) was used to investigate solvent-free enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by immobilized lipase Novozym 435 at 40 {sup o}C. The aim of the study was to determine reaction enthalpy for the enzymatic transesterification and to elucidate the mass transfer and energetic processes taking place. Based on the measured enthalpy and composition change in the system, the heat of reaction at 40 {sup o}C for the two systems was determined as -9.8 {+-} 0.9 kJ/mole biodiesel formed from rapeseed oil and methanol, and -9.3 {+-} 0.7 kJ/mole when rapeseed oil and ethanol was used. Simple Michaelis-Menten kinetics was not an appropriate choice for describing the kinetics of this heterogeneous system. The experiments demonstrated the possibility of investigating complex reaction mixtures using ITC. Although it is possible to determine thermodynamic properties such as reaction enthalpy and reaction rate, the difficulty in actually measuring the true non-mass-transfer-limited reaction kinetics is exposed by the high time resolution of ITC.

  13. A new sensor for thermometric titrations.

    Science.gov (United States)

    Najib, Fadhil M; Zewar, Sardir; Abdulla, Ahmad M

    2007-01-15

    A new thermometric sensor, which is a transistor (OC71), has been introduced to follow thermometric titrations successfully to clear end points. The sensor was suitable in both normal and differential modes of titration. It is possible to titrate down to 1.32micromol of HCl and 26.4micromol of H(3)BO(3)in a final 20ml solution with accuracy and precision of 1%, 2.2% and 1.4%, 2.2%, respectively. The sensor, in association with a pH glass electrode, was used for the determination of pK values of some well established weak acids such as, acetic acid (4.77), phosphoric acid (pK(1)=2.18, pK(2)=7.20 and pK(3)=12.32) as well as for a very weak acid of uncertain pK values H(3)BO(3) (pK(1)=9.20, pK(2)=12.7 and pK(3)=13.80). The sensor was also examined for kinetic catalytic determination of iron(III) in water, milk and pharmaceuticals.

  14. A monosegmented-flow Karl Fischer titrator.

    Science.gov (United States)

    de Aquino, Emerson Vidal; Rohwedder, Jarbas José Rodrigues; Pasquini, Celio

    2007-02-28

    A monosegmented volumetric Karl Fischer titrator is described to mechanize the determination of water content in organic solvents. The system is based on the flow-batch characteristics of the monosegmented analysis concept and employs biamperometry to monitor the progress of the titration. The system shows accuracy and precision that are highly independent of the flow rate, does not require calibration, and is carried out in a closed system capable of minimizing contact of the sample and reagents with ambient moisture. Sample volumes in the range of 40-300muL are employed, depending on the water concentration. An automatic dilution is provided to deal with concentrated samples. The consumption of Karl Fischer reagent depends on the water content of the sample but is not larger than 100muL. The system was evaluated for determination of water in ethanol and methanol in the range 0.02-0.5% (w/w). The average relative precision estimated in that range (9-3%) is comparable to that obtained with a larger volume commercial system and no significant difference was observed between the results obtained for the two systems at the 95% confidence level. A complete titration can be performed in less than 5min employing the proposed system.

  15. Potentiometric titrations in anhydrous acetic acid

    International Nuclear Information System (INIS)

    Le Port, L.

    1966-03-01

    The method used for studying anhydrous acetic acid is potentiometry with a glass electrode. We have in this way studied the titration of common inorganic acids (HClO 4 - HBr - H 2 SO 4 - HCl - HNO 3 - H 3 PO 4 ) and of some metallic salts. Furthermore we have shown that complex acids are formed between HCl and some metallic chlorides. An analysis of the titration curves for the inorganic acids against pyridinium chloride has made it possible to calculate a certain number of values for the dissociation pK of these acids and of the corresponding pyridinium salts. The titration of metallic perchlorates constitutes a method of studying the stability of acetates; we have thus been able to draw up a classification for some of these acetates. The metallic chlorides studied fall into two groups according to their behaviour in weak or strong acids. The differences have been explained on the basis of the role played by solvolysis. In the third part we have studied the acidic properties of mixtures of HCl with certain metallic chlorides. This work has demonstrated the existence, in certain cases, of acid complexes of the type (HCl) m MCl n . (author) [fr

  16. Interactions between poly(acrylic acid) and sodium dodecyl sulfate: isothermal titration calorimetric and surfactant ion-selective electrode studies.

    Science.gov (United States)

    Wang, C; Tam, K C

    2005-03-24

    Interaction between a monodispersed poly(acrylic acid) (PAA) (M(W) = 5670 g/mol, M(w)/M(n) = 1.02) with sodium dodecyl sulfate (SDS) was investigated using isothermal titration calorimetry (ITC), ion-selective electrode (ISE), and dynamic light scattering measurements. Contrary to previous studies, we report for the first time evidence of interaction between SDS and PAA when the degree of neutralization (alpha) of PAA is lower than 0.2. Hydrocarbon chains of SDS cooperatively bind to apolar segments of PAA driven by hydrophobic interaction. The interaction is both enthalpy and entropy favored (deltaH is negative but deltaS is positive). In 0.05 wt % PAA solution, the SDS concentration corresponding to the onset of binding (i.e., CAC) is approximately 2.4 mM and the saturation concentration (i.e., C(S)) is approximately 13.3 mM when alpha = 0. When PAA was neutralized and ionized, the binding was hindered by the enhanced electrostatic repulsion between negatively charged SDS and PAA chains and improved solubility of the polymer. With increasing alpha to 0.2, CAC increases to approximately 6.2 mM, C(S) drops to 8.6 mM, and the interaction is significantly weakened where the amount of bound SDS on PAA is reduced considerably. The values of CAC and C(S) derived from different techniques are in good agreement. The binding results in the formation of mixed micelles on apolar PAA coils, which then expands and dissociates into single PAA chains. The majority of unneutralized PAA molecules exist as single polymer chains stabilized by bound SDS micelles in solution after the saturation concentration.

  17. Titrated flow versus fixed flow Bubble Nasal CPAP for respiratory distress in preterm neonates.

    Directory of Open Access Journals (Sweden)

    Srinivas eMurki

    2015-10-01

    Full Text Available Background: The clinical effects of a pre-fixed flow of air-oxygen versus a flow titrated according to visible bubbling are not well understood.Objective: To compare the effects of a fixed flow (5 L/min and titrated flow ( flow just enough to ensure bubbling at different set pressures on delivered intra-prong pressure, gas exchange and clinical parameters in preterm infants on bubble CPAP for respiratory distress.Methods: Preterm infants less than 35 weeks gestation on bubble CPAP and less than 96 h of age, were enrolled in this cross over study. They were subjected to 30 minute periods of titrated flow and fixed flow. At the end of both epochs, gas flow rate, set pressure, FiO2, SpO2, Silverman retraction score, respiratory rate , abdominal girth, and blood gases were recorded. The delivered intra-prong pressure was measured by an electronic manometer. Results: Sixty nine recordings were made in 54 infants. For each of the set CPAP pressures (4, 5 and 6 cm H2O, the mean delivered pressure with a fixed flow of 5 L/min was higher than that delivered by the titrated flow. During the fixed flow epoch, the delivered pressure was closer to and higher than the set pressure resulting in higher PaO2 and lower PaCO2 as compared to titrated flow epoch. In the titrated flow period, the delivered pressure was consistently lower than the set pressure. Conclusion: In preterm infants on bubble CPAP with set pressures of 4 to 6 cm H2O, a fixed flow of 5 L/min is more effective than a flow titrated to ensure adequate visible bubbling. It achieves higher delivered pressures, better oxygenation and ventilation.

  18. Isothermal titration calorimetric studies of the acid-base properties of poly(N-isopropylacrylamide-co-4-vinylpyridine) cationic polyelectrolyte colloidal microgels

    International Nuclear Information System (INIS)

    Seidel, J.; Pinkrah, V.T.; Mitchell, J.C.; Chowdhry, B.Z.; Snowden, M.J.

    2004-01-01

    Isothermal titration calorimetry (ITC) and potentiometric titration were used to study the protonation properties of the 4-vinylpyridine (4-VP) moiety in cationic poly(N-isopropylacrylamide-co-4-vinylpyridine) colloidal microgels [poly(NIPAM-co-4-VP)]. Calorimetric pH titrations were performed using microgels of different 4-VP content and the influence of ionic strength and counter ions have been examined. The calorimetric titration output consists of several thermal contributions reflecting the complex nature of the interactions in the aqueous microgel dispersions. In contrast to the potentiometric results, the calorimetric titration data could not be completely described by a theoretical model solely taking into account protonation equilibria. Deviations from the proposed model correlate with swelling or shrinking of the gel particles. The calorimetric results also reveal a pronounced counter-ion effect of perchlorate compared to chloride ions. In the presence of perchlorate ions, small secondary thermal effects accompany protonation of the 4-VP moiety due, in part, to kinetically limited conformational changes in the co-polymer microgel

  19. Is automatic CPAP titration as effective as manual CPAP titration in OSAHS patients? A meta-analysis.

    Science.gov (United States)

    Gao, Weijie; Jin, Yinghui; Wang, Yan; Sun, Mei; Chen, Baoyuan; Zhou, Ning; Deng, Yuan

    2012-06-01

    It is costly and time-consuming to conduct the standard manual titration to identify an effective pressure before continuous positive airway pressure (CPAP) treatment for obstructive sleep apnea (OSA) patients. Automatic titration is cheaper and more easily available than manual titration. The purpose of this systematic review was to evaluate the effect of automatic titration in identifying a pressure and on the improvement of apnea/hyponea index (AHI) and somnolence, the change of sleep quality, and the acceptance and compliance of CPAP treatment, compared with the manual titration. A systematic search was made of the PubMed, EMBASE, Cochrane Library, SCI, China Academic Journals Full-text Databases, Chinese Biomedical Literature Database, Chinese Scientific Journals Databases and Chinese Medical Association Journals. Randomized controlled trials comparing automatic titration and manual titration were reviewed. Studies were pooled to yield odds ratios (OR) or mean differences (MD) with 95% confidence intervals (CI). Ten trials involving 849 patients met the inclusion criteria. It is hard to identify a trend in the pressures determined by either automatic or manual titration. Automatic titration can improve the AHI (MD = 0.03/h, 95% CI = -4.48 to 4.53) and Epworth sleepiness scale (SMD = -0.02, 95% CI = -0.34 to 0.31,) as effectively as the manual titration. There is no difference between sleep architecture under automatic titration or manual titration. The acceptance of CPAP treatment (OR = 0.96, 95% CI = 0.60 to 1.55) and the compliance with treatment (MD = -0.04, 95% CI = -0.17 to 0.10) after automatic titration is not different from manual titration. Automatic titration is as effective as standard manual titration in improving AHI, somnolence while maintaining sleep quality similar to the standard method. In addition, automatic titration has the same effect on the acceptance and compliance of CPAP treatment as manual titration. With the potential advantage

  20. Influence of kinetics on the determination of the surface reactivity of oxide suspensions by acid-base titration.

    Science.gov (United States)

    Duc, M; Adekola, F; Lefèvre, G; Fédoroff, M

    2006-11-01

    The effect of acid-base titration protocol and speed on pH measurement and surface charge calculation was studied on suspensions of gamma-alumina, hematite, goethite, and silica, whose size and porosity have been well characterized. The titration protocol has an important effect on surface charge calculation as well as on acid-base constants obtained by fitting of the titration curves. Variations of pH versus time after addition of acid or base to the suspension were interpreted as diffusion processes. Resulting apparent diffusion coefficients depend on the nature of the oxide and on its porosity.

  1. Modulated Temperature Differential Scanning Calorimetry Theoretical and Practical Applications in Polymer Characterisation

    CERN Document Server

    Reading, Mike

    2006-01-01

    MTDSC provides a step-change increase in the power of calorimetry to characterize virtually all polymer systems including curing systems, blends and semicrystalline polymers. It enables hidden transitions to be revealed, miscibility to be accurately assessed, and phases and interfaces in complex blends to be quantified. It also enables crystallinity in complex systems to be measured and provides new insights into melting behaviour. All of this is achieved by a simple modification of conventional DSC. In 1992 a new calorimetric technique was introduced that superimposed a small modulation on top of the conventional linear temperature program typically used in differential scanning calorimetry. This was combined with a method of data analysis that enabled the sample’s response to the linear component of the temperature program to be separated from its response to the periodic component. In this way, for the first time, a signal equivalent to that of conventional DSC was obtained simultaneously with a measure ...

  2. Application of isothermal calorimetry and uv spectroscopy for stability monitoring of pentaerythritol tetranitrate

    International Nuclear Information System (INIS)

    Dosser, L.R.; Pickard, J.M.

    1992-01-01

    Thermal stabilities for a series of pentaerythritol-tetranitrate (PETN) samples with variable surf ace areas were monitored by isothermal calorimetry and UV spectroscopy over the temperature range of 363 to 408 K. Isothermal induction times measured with constant volume calorimetry under an air atmosphere and No evolution rates monitored by UV absorbance at 213 nm under vacuum correlated with the PETN surface area at temperatures equal to or exceeding 383 K. Rate data measured at 383 K are in accord with predictions based on detailed kinetic modeling. Below 383 K, NO evolution data suggested that additional geometric factors may be significant in controlling PETN stability. Mechanisms for influencing surface area upon the rate-determining step are addressed

  3. Metabolic depression in fish measured by direct calorimetry: A review

    NARCIS (Netherlands)

    Ginneken, van V.J.T.; Thillart, van den G.

    2009-01-01

    In nature under adverse conditions like low oxygen conditions or starvation fish often lower their metabolism: `metabolic depression¿. This strategy of lowering the metabolic rate is a survival strategy and is used to save energy stores and diminish end-product accumulation. The overall metabolic

  4. Photothermal beam deflection calorimetry in solution photochemistry: recent progress and future prospects.

    Science.gov (United States)

    Falvey, D E

    1997-01-01

    Photothermal beam deflection (PBD) calorimetry is a technique that measures changes in the solvent's refractive index that accompanies photothermal heating. This method is capable of extracting both kinetic and thermodynamic information from photochemical reactions. A qualitative description of physical basis of time-resolved PBD is presented. Several recent examples of its application to photochemical and photobiological problems are discussed. Finally, the advantages and limitations of PBD are described.

  5. Determination of quaternary ammonium compounds by potentiometric titration with an ionic surfactant electrode: single-laboratory validation.

    Science.gov (United States)

    Price, Randi; Wan, Ping

    2010-01-01

    A potentiometric titration for determining the quaternary ammonium compounds (QAC) commonly found in antimicrobial products was validated by a single laboratory. Traditionally, QACs were determined by using a biphasic (chloroform and water) manual titration procedure. Because of safety considerations regarding chloroform, as well as the subjectivity of color indicator-based manual titration determinations, an automatic potentiometric titration procedure was tested with quaternary nitrogen product formulations. By using the Metrohm Titrando system coupled with an ionic surfactant electrode and an Ag/AgCl reference electrode, titrations were performed with various QAC-containing formulation products/matrixes; a standard sodium lauryl sulfate solution was used as the titrant. Results for the products tested are sufficiently reproducible and accurate for the purpose of regulatory product enforcement. The robustness of the method was measured by varying pH levels, as well as by comparing buffered versus unbuffered titration systems. A quantitation range of 1-1000 ppm quaternary nitrogen was established. Eight commercially available antimicrobial products covering a variety of matrixes were assayed; the results obtained were comparable to those obtained by the manual titration method. Recoveries of 94 to 104% were obtained for spiked samples.

  6. Clinical Outcomes of Continuation of Metformin Titration Instructions with Electronic Prescribing.

    Science.gov (United States)

    Delate, Thomas; Rader, Nathan; Rawlings, Julia E; Smith, Karen; Herner, Sheryl J

    2015-06-01

    Anecdotal evidence suggests that metformin titration instructions are not being updated and refill requests are approved without modification of the titration instructions such that the titration instructions is continued for patients newly initiated on metformin. This was a retrospective cohort analysis of adult patients who received newly initiated metformin pharmacotherapy. Patients were followed from their initial metformin purchase through two subsequent metformin refill purchases. Outcomes, including the 3-year incidence rate of patients with at least one set of continued titration instructions and proportions of patients with at least one gastrointestinal adverse effect (AE) and those with an elevated glucose measurement at follow-up, were assessed during the time period between patients' second and third metformin purchases. Analyses were performed comparing the exposure (i.e., patients with continued instructions) group to the control (i.e., patients without continued instructions) group. The exposure group had a higher mean age and chronic disease score but lower metformin starting dose than the control group (all p titration instructions was 60.3 % (95 % CI 58.3-62.3). Gastrointestinal AEs were rare with equivalent proportions of patients in each group experiencing an event (p > 0.05). Control patients (48.7 % of patients with a measurement) were more likely to have had poorly controlled glucose than exposure patients (35.7 % of patients with a measurement) (p titration instructions for patients newly initiated on metformin was observed; however, such continuation did not negatively affect clinical outcomes.

  7. Mathematical model of cycad cones' thermogenic temperature responses: inverse calorimetry to estimate metabolic heating rates.

    Science.gov (United States)

    Roemer, R B; Booth, D; Bhavsar, A A; Walter, G H; Terry, L I

    2012-12-21

    A mathematical model based on conservation of energy has been developed and used to simulate the temperature responses of cones of the Australian cycads Macrozamia lucida and Macrozamia. macleayi during their daily thermogenic cycle. These cones generate diel midday thermogenic temperature increases as large as 12 °C above ambient during their approximately two week pollination period. The cone temperature response model is shown to accurately predict the cones' temperatures over multiple days as based on simulations of experimental results from 28 thermogenic events from 3 different cones, each simulated for either 9 or 10 sequential days. The verified model is then used as the foundation of a new, parameter estimation based technique (termed inverse calorimetry) that estimates the cones' daily metabolic heating rates from temperature measurements alone. The inverse calorimetry technique's predictions of the major features of the cones' thermogenic metabolism compare favorably with the estimates from conventional respirometry (indirect calorimetry). Because the new technique uses only temperature measurements, and does not require measurements of oxygen consumption, it provides a simple, inexpensive and portable complement to conventional respirometry for estimating metabolic heating rates. It thus provides an additional tool to facilitate field and laboratory investigations of the bio-physics of thermogenic plants. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Indirect calorimetry in nutritional therapy. A position paper by the ICALIC study group.

    Science.gov (United States)

    Oshima, Taku; Berger, Mette M; De Waele, Elisabeth; Guttormsen, Anne Berit; Heidegger, Claudia-Paula; Hiesmayr, Michael; Singer, Pierre; Wernerman, Jan; Pichard, Claude

    2017-06-01

    This review aims to clarify the use of indirect calorimetry (IC) in nutritional therapy for critically ill and other patient populations. It features a comprehensive overview of the technical concepts, the practical application and current developments of IC. Pubmed-referenced publications were analyzed to generate an overview about the basic knowledge of IC, to describe advantages and disadvantages of the current technology, to clarify technical issues and provide pragmatic solutions for clinical practice and metabolic research. The International Multicentric Study Group for Indirect Calorimetry (ICALIC) has generated this position paper. IC can be performed in in- and out-patients, including those in the intensive care unit, to measure energy expenditure (EE). Optimal nutritional therapy, defined as energy prescription based on measured EE by IC has been associated with better clinical outcome. Equations based on simple anthropometric measurements to predict EE are inaccurate when applied to individual patients. An ongoing international academic initiative to develop a new indirect calorimeter aims at providing innovative and affordable technical solutions for many of the current limitations of IC. Indirect calorimetry is a tool of paramount importance, necessary to optimize the nutrition therapy of patients with various pathologies and conditions. Recent technical developments allow broader use of IC for in- and out-patients. Copyright © 2016 Elsevier Ltd and European Society for Clinical Nutrition and Metabolism. All rights reserved.

  9. Radiometric titration of thallium(III) with EDTA

    International Nuclear Information System (INIS)

    Rao, V.R.S.; Pulla Rao, Ch.; Tataiah, G.

    1978-01-01

    Radioactive solutions containing very small amounts of thallium(III) can be determined by radiometric titration using ammonia as hydrolysing agent. Aqueous solution of thallium(I) (both inactive and radioactive) is treated with bromine water till the appearance of the brown colour of bromine, and the solution is warmed to 80 deg C to expel the excess bromine. By this procedure all thallium(I) is quantitatively oxidised to thallium(III). An aqueous solution of ammonia is added to precipitate thallium(III) as thallic oxide. It is then filtered, washed with water to free it from bromide and then dissolved in 2N HCl and the solution is then standardised. 2 ml of this solution is transferred to a 20 ml volumetric flask, 1 ml of radioactive thallium(III) solution to be standardised is added as well as incremental amounts of EDTA solution and mixed thoroughly. Uncomplexed thallium(III) is then precipitated by the addition of an ammonia solution and diluted to 20 ml. Required amount of this mixture is centrifuged. The beta activity of the supernatant aliquot is measured using a GM counter. Quantitative determination of Tl(III) in the range of 1-10 μM can be carried out. The interference of cations such as Au(III), iron(III), Ga(III) can be eliminated by pretreatment of the Tl(III) solution before carrying out radiometric titration. The results obtained are reproducible and accurate to +-3%. (T.I.)

  10. Evaluation of the 5 and 8 pH point titration methods for monitoring anaerobic digesters treating solid waste.

    Science.gov (United States)

    Vannecke, T P W; Lampens, D R A; Ekama, G A; Volcke, E I P

    2015-01-01

    Simple titration methods certainly deserve consideration for on-site routine monitoring of volatile fatty acid (VFA) concentration and alkalinity during anaerobic digestion (AD), because of their simplicity, speed and cost-effectiveness. In this study, the 5 and 8 pH point titration methods for measuring the VFA concentration and carbonate system alkalinity (H2CO3*-alkalinity) were assessed and compared. For this purpose, synthetic solutions with known H2CO3*-alkalinity and VFA concentration as well as samples from anaerobic digesters treating three different kind of solid wastes were analysed. The results of these two related titration methods were verified with photometric and high-pressure liquid chromatography measurements. It was shown that photometric measurements lead to overestimations of the VFA concentration in the case of coloured samples. In contrast, the 5 pH point titration method provides an accurate estimation of the VFA concentration, clearly corresponding with the true value. Concerning the H2CO3*-alkalinity, the most accurate and precise estimations, showing very similar results for repeated measurements, were obtained using the 8 pH point titration. Overall, it was concluded that the 5 pH point titration method is the preferred method for the practical monitoring of AD of solid wastes due to its robustness, cost efficiency and user-friendliness.

  11. An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid.

    Science.gov (United States)

    van Staden, J F; Mashamba, Mulalo G; Stefan, Raluca I

    2002-09-01

    An on-line potentiometric sequential injection titration process analyser for the determination of acetic acid is proposed. A solution of 0.1 mol L(-1) sodium chloride is used as carrier. Titration is achieved by aspirating acetic acid samples between two strong base-zone volumes into a holding coil and by channelling the stack of well-defined zones with flow reversal through a reaction coil to a potentiometric sensor where the peak widths were measured. A linear relationship between peak width and logarithm of the acid concentration was obtained in the range 1-9 g/100 mL. Vinegar samples were analysed without any sample pre-treatment. The method has a relative standard deviation of 0.4% with a sample frequency of 28 samples per hour. The results revealed good agreement between the proposed sequential injection and an automated batch titration method.

  12. Thermodynamic study of the interaction between calcium and zoledronic acid by calorimetry

    International Nuclear Information System (INIS)

    Mostefa Side Larbi, Mohamed A.; Sauzet, Christophe; Piccerelle, Philippe; Cau, Pierre

    2016-01-01

    Bisphosphonates (BPs) are widely used to treat calcium disorders because of their structural and functional similarities with the organic pyrophosphates present in plasma and urine. BPs are well known for their strong interactions with calcium, and they have been shown to bind to hydroxyapatite or bone; however, no model exists for studying in greater detail how BPs and particularly amino-bisphosphonates (N-BPs) such as zolendronate (Zol) bind to free calcium. The aim of this work was to determine the effect of pH on Ca 2+ /Zol complex formation using isothermal titration calorimetry (ITC) because these effects might have important implications for the future development of a solid dosage form. In this study, using a predictive model, we can observe, the existence of three Ca 2+ /Zol complexes. Knowledge of the binding constant for each complex is helpful for predicting the predominance of the different species at different Ca 2+ /Zol ratios. Binding is due to ionic interaction between Ca 2+ and the negative charges formed by dissociated Zol as a function of the pKa. Ca 2+ fixation induces a strong rearrangement of the surrounding water molecules and causes proton release or uptake. The pH-dependent affinity of calcium for each site based on the model used in this work is proposed in detail, which might facilitate the development of new bisphosphonates and enable further elucidation of their mode of action.

  13. How to Measure Heat Capacity at Low Temperatures

    Science.gov (United States)

    Ventura, Guglielmo; Perfetti, Mauro

    This chapter is devoted to the description of calorimetric techniques used to measure heat capacity of solids: pulse heat calorimetry (Sect. 2.3), relaxation calorimetry (Sect. 2.4), dual slope calorimetry (Sect. 2.5), a.c. calorimetry (Sect. 2.6), differential scanning calorimetry (Sect. 2.7). Examples of measurements of heat capacity are reported in Sects. 2.3 and 2.4.

  14. Solution Calorimetry Experiments for Physical Chemistry.

    Science.gov (United States)

    Raizen, Deborah A.; And Others

    1988-01-01

    Presents two experiments: the first one measures the heat of an exothermic reaction by the reduction of permanganate by the ferris ion; the second one measures the heat of an endothermic process, the mixing of ethanol and cyclohexane. Lists tables to aid in the use of the solution calorimeter. (MVL)

  15. Liquid Argon Calorimetry with LHC-Performance Specifications

    CERN Multimedia

    2002-01-01

    % RD-3 Liquid Argon Calorimetry with LHC-Performance Specifications \\\\ \\\\Good electromagnetic and hadronic calorimetry will play a central role in an LHC detector. Among the techniques used so far, or under development, the liquid argon sampling calorimetry offers high radiation resistence, good energy resolution (electromagnetic and hadronic), excellent calibration stability and response uniformity. Its rate capabilities, however, do not yet match the requirements for LHC. \\\\ \\\\The aim of this proposal is to improve the technique in such a way that high granularity, good hermiticity and adequate rate capabilities are obtained, without compromising the above mentioned properties. To reach this goal, we propose to use a novel structure, the $^{\\prime\\prime}$accordion$^{\\prime\\prime}$, coupled to fast preamplifiers working at liquid argon temperature. Converter and readout electrodes are no longer planar and perpendicular to particles, as usual, but instead they are wiggled around a plane containing particles. ...

  16. Thermometric titration of some monoprotic and diprotic acids in aqueous and non-aqueous media.

    Science.gov (United States)

    Harries, R J

    1968-12-01

    Some mono- and diprotic acids have been titrated thermometrically with strong alkalis in aqueous and non-aqueous media. Thermograms with sharp arrest points were obtained, from which heats of neutralization were measured. Heats of neutralization in the media used were compared and an effect attributable to hydrogen bonding was found.

  17. Determination of oxygen nonstoichiometry and diffusivity in mixed conducting oxides by oxygen Coulometric titration

    NARCIS (Netherlands)

    Lankhorst, M.H.R.; Lankhorst, Martijn H.R.; Bouwmeester, Henricus J.M.

    1997-01-01

    Oxygen coulometric titration has been applied to measure chemical diffusion in La0.8Sr0.2CoO3-δ between 700 and 1000°C. The transient current response to a potentiostatic step has been transformed from the time domain to the frequency domain. The equivalent circuit used to fit the resulting

  18. Effects of pH, titratable acidity and calcium concentration of non ...

    African Journals Online (AJOL)

    Objective: Beverage acidity has been measured routinely using the pH value. However, titratable acidity is thought to be a true indicator of beverage erosive potential. It has also been reported that experimental addition of calcium in beverages can reduce the progression of erosion. This study was carried out to investigate ...

  19. Up-titration of allopurinol in patients with gout.

    Science.gov (United States)

    Jennings, Claudine G; Mackenzie, Isla S; Flynn, Rob; Ford, Ian; Nuki, George; De Caterina, Raffaele; Riches, Philip L; Ralston, Stuart H; MacDonald, Thomas M

    2014-08-01

    European League against Rheumatism (EULAR) gout management guidelines recommend achieving a target urate level titration in achieving the EULAR target levels. The Febuxostat versus Allopurinol Streamlined Trial (FAST) is an ongoing multi-centre study comparing the cardiovascular safety of febuxostat and allopurinol (target recruitment: 5706 patients). Recruited patients were already taking allopurinol and the protocol required up-titration of daily allopurinol dose, in 100 mg increments, to achieve the EULAR urate target level prior to randomisation. We reviewed pre-randomisation data from the first 400 recruited and subsequently randomised FAST patients. Of 400 patients, 144 (36%) had urate levels ≥357 µmol/L at screening and required allopurinol up-titration. Higher urate levels were significantly associated with lower allopurinol dose, male sex, increased BMI, increased alcohol intake and diuretic use. Mean fall in urate levels after a single 100-mg dose increase was 71 µmol/L. The number of up-titrations required ranged from one to five (median = 1) with 65% of patients controlled after one 100-mg up-titration. Overall, 97% of up-titrated patients achieved target urate levels with median final allopurinol dose of 300 mg daily. Side effects and complications of up-titration were minimal. Overall, 36% of FAST patients were not at target urate levels and required up-titration. Allopurinol up-titration was effective in achieving urate target levels and was generally well tolerated by patients. Copyright © 2014 Elsevier Inc. All rights reserved.

  20. Laboratory Automatic Titration of Chromium Plating and Electropolishing Solutions

    National Research Council Canada - National Science Library

    Sopok, Samuel

    2001-01-01

    .... The analytical chemistry literature lacks an adequate automatic titration method for the monitoring of chromic acid in chromium plating solutions and the monitoring of phosphoric and sulfuric acids...

  1. A computer controlled potentiometric titrator for quantitative determination of uranium

    International Nuclear Information System (INIS)

    Verdingh, V.; Michiels, A.

    1988-01-01

    The modified Davies and Gray methods is frequently used for the potentiometric titration of uranium. It is based upon the reduction of U(VI) to U(IV) with a reductant (e.g. Fe ++ ) followed by a selective oxidation of the excess of reductant and subsequent titration of U(IV) with potassium dichromate (K 2 Cr 2 O 7 ). Interference from other elements is low, but the method is rather cumbersome due to the number of reactants to be added before the titration is started. The timing of these additions also plays a role. In order to render the titration less dependent on human factors and with the aim of reaching high reproducibility, a computer controlled system has been designed and set-up. Reagents are added by five computer controlled burettes. A program allows the choice of volumes and waiting times, and commands the start of the final titration which is followed by the microprocessor of the automatic potentiometric titrator. In this way a routine uranium titration can be completed in about twelve minutes. Reproducibilities of the order of ±15% are achievable in routine operation. For high precision work, the titrator is used as an end-point detector. Titrant is added manually by mass, so as to react with > 99% of the uranium. The residual uranium is then titrated automatically by colume with diluted titrant. The precision can be improved by a factor of approximately ten. (orig.)

  2. PREFACE: XIV International Conference on Calorimetry in High Energy Physics

    Science.gov (United States)

    Wang, Yifang

    2011-03-01

    The International Conferences on Calorimetry in High Energy Physics (also known as the Calor Conference series, started in October 1990 at Fermilab) address all aspects of calorimetric particle detection and measurement, with an emphasis on high energy physics experiments. The XIV International Conference on Calorimetry in High Energy Physics (Calor 2010) was held at the campus of the Institute of High Energy Physics, Beijing, China, from May 10-14, 2010. This conference brought together more than 110 participants from 20 countries, including senior scientists and young physicists. During the five days of the conference, 98 presentations were given in seven plenary sessions. The attendees had in-depth discussions on the latest developments and innovations in calorimetry, including the exciting new LHC results. From the presentations, 83 papers were published in this proceedings. The success of the conference was due to the participants' enthusiasm and the excellent talks given by the speakers, and to the conveners for organizing the individual sessions. We would like to thank the International Advisory Committee for giving us the opportunity to host this Conference in Beijing. Finally we would like to thank all the people involved in the organization of the Conference, who have provided valuable local support. Yifang WangChair of Local Organizing Committee International Advisory Committee M DanilovITEP Moscow M DiemozINFN Roma I A EreditatoBern F L FabbriINFN Frascati T KobayashiICEPP Tokyo M LivanPavia University & INFN P LubranoINFN Perugia S MagillANL Argonne A MaioLIPP Lisbon H OberlackMPI Munich A ParaFermilab R WigmansTTU Lubbock R YoshidaANL Argonne R ZhuCaltech Local Organizing Committee Y WangIHEP (Chair) Y GaoTshinghua University T HuIHEP (Scientific secretary) C LiUSTC W LiIHEP J LuIHEP P WangIHEP T XuIHEP L ZhouIHEP Session Conveners 1) Materials and detectors - Junguang Lu (IHEP), Francesca Nessi (CERN) 2) Algorithm and simulation - Nural Akchurin

  3. Proton dosimetry comparison involving ionometry and calorimetry

    International Nuclear Information System (INIS)

    Delacroix, Sabine; Bridier, Andre; Mazal, Alexandre; Daures, Josiane; Ostrowsky, Aime; Nauraye, Catherine; Kacperek, Andre; Vynkier, Stephane; Brassard, Nicole; Habrand, Jean-Louis

    1997-01-01

    A comparison of the absorbed dose to tissue determined by various ionization chambers, Faraday cups, and an A-150 plastic calorimeter was performed in the 200 MeV proton beam of Orsay, France. Four European proton-therapy centers (Clatterbridge, UK, Louvain la Neuve, Belgium, and Nice and Orsay, France) participated in the comparison. An agreement of better than 1% was observed in the absorbed dose to A-150 measured with the different chambers of the participating groups. The mean ratio of the absorbed dose to A-150 determined with the calorimeter to that determined by the different ionization chambers in the different irradiation conditions was found to be 0.952 ± 0.007 [1 standard deviation (SD)] according to the code of practice used by all the participating centers, based on Janni's tables of stopping powers and a value of 35.2 J/Coulomb for (W air /e) p . A better agreement in the mean ratio calorimeter/chamber, 0.985 ± 0.007 (1 SD) is observed when using the proton stopping power ratio values recently published by the International Commission on Radiation Units and Measurements in Report no. 49. The mean ratio of these doses determined in accordance with the American Association of Physicists in Medicine protocol and using the new recommended stopping power tables becomes 1.002 ± 0.007 (1 SD). Two Faraday cups agree in measured charge to within 0.8%; however, the calculation of dose is underestimated by up to 17%; compared with ion chamber measurements and seems to be very sensitive to measurement conditions, particularly to the distance to the collimator

  4. Silk I and Silk II studied by fast scanning calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Cebe, Peggy; Partlow, Benjamin P.; Kaplan, David L.; Wurm, Andreas; Zhuravlev, Evgeny; Schick, Christoph

    2017-06-01

    Using fast scanning calorimetry (FSC), we investigated the glass transition and crystal melting of samples of B. mori silk fibroin containing Silk I and/or Silk II crystals. Due to the very short residence times at high temperatures during such measurements, thermal decomposition of silk protein can be significantly suppressed. FSC was performed at 2000 K/s using the Mettler Flash DSC1 on fibroin films with masses around 130–270 ng. Films were prepared with different crystalline fractions (ranging from 0.26 to 0.50) and with different crystal structures (Silk I, Silk II, or mixed) by varying the processing conditions. These included water annealing at different temperatures, exposure to 50% MeOH in water, or autoclaving. The resulting crystal structure was examined using wide angle X-ray scattering. Degree of crystallinity was evaluated from Fourier transform infrared (FTIR) spectroscopy and from analysis of the heat capacity increment at the glass transition temperature. Silk fibroin films prepared by water annealing at 25 °C were the least crystalline and had Silk I structure. FTIR and FSC studies showed that films prepared by autoclaving or 50% MeOH exposure were the most crystalline and had Silk II structure. Intermediate crystalline fraction and mixed Silk I/Silk II structures were found in films prepared by water annealing at 37 °C. FSC results indicate that Silk II crystals exhibit endotherms of narrower width and have higher mean melting temperature Tm(II) = 351 ± 2.6 °C, compared to Silk I crystals which melt at Tm(I) = 292 ± 3.8 °C. Films containing mixed Silk I/Silk II structure showed two clearly separated endothermic peaks. Evidence suggests that the two types of crystals melt separately and do not thermally interconvert on the extremely short time scale (0.065 s between onset and end of melting) of the FSC experiment.

  5. The acid-base titration of montmorillonite

    Science.gov (United States)

    Bourg, I. C.; Sposito, G.; Bourg, A. C.

    2003-12-01

    Proton binding to clay minerals plays an important role in the chemical reactivity of soils (e.g., acidification, retention of nutrients or pollutants). If should also affect the performance of clay barriers for waste disposal. The surface acidity of clay minerals is commonly modelled empirically by assuming generic amphoteric surface sites (>SOH) on a flat surface, with fitted site densities and acidity constant. Current advances in experimental methods (notably spectroscopy) are rapidly improving our understanding of the structure and reactivity of the surface of clay minerals (arrangement of the particles, nature of the reactive surface sites, adsorption mechanisms). These developments are motivated by the difficulty of modelling the surface chemistry of mineral surfaces at the macro-scale (e.g., adsorption or titration) without a detailed (molecular-scale) picture of the mechanisms, and should be progressively incorporated into surface complexation models. In this view, we have combined recent estimates of montmorillonite surface properties (surface site density and structure, edge surface area, surface electrostatic potential) with surface site acidities obtained from the titration of alpha-Al2O3 and SiO2, and a novel method of accounting for the unknown initial net proton surface charge of the solid. The model predictions were compared to experimental titrations of SWy-1 montmorillonite and purified MX-80 bentonite in 0.1-0.5 mol/L NaClO4 and 0.005-0.5 mol/L NaNO3 background electrolytes, respectively. Most of the experimental data were appropriately described by the model after we adjusted a single parameter (silanol sites on the surface of montmorillonite were made to be slightly more acidic than those of silica). At low ionic strength and acidic pH the model underestimated the buffering capacity of the montmorillonite, perhaps due to clay swelling or to the interlayer adsorption of dissolved aluminum. The agreement between our model and the experimental

  6. Thermodynamic characteristics of the acid-base equilibria of taurine in aqueous solutions, according to calorimetry data

    Science.gov (United States)

    Gridchin, S. N.; Shekhanov, R. F.; Pyreu, D. F.

    2015-02-01

    Enthalpies of the neutralization and protonation of taurine (HL) are measured by direct calorimetry at 298.15 K and ionic strengths of 0.3, 0.5, and 1.0 (KNO3). The standard thermodynamic characteristics of HL protolytic equilibria are calculated.

  7. Ultrasonic and densimetric titration applied for acid-base reactions.

    Science.gov (United States)

    Burakowski, Andrzej; Gliński, Jacek

    2014-01-01

    Classical acoustic acid-base titration was monitored using sound speed and density measurements. Plots of these parameters, as well as of the adiabatic compressibility coefficient calculated from them, exhibit changes with the volume of added titrant. Compressibility changes can be explained and quantitatively predicted theoretically in terms of Pasynski theory of non-compressible hydrates combined with that of the additivity of the hydration numbers with the amount and type of ions and molecules present in solution. It also seems that this development could be applied in chemical engineering for monitoring the course of chemical processes, since the applied experimental methods can be carried out almost independently on the medium under test (harmful, aggressive, etc.).

  8. Warm-up calorimetry of Dewar-Detector Assemblies

    Science.gov (United States)

    Veprik, A.; Shlomovich, B.; Tuito, A.

    2015-12-01

    Boil-off isothermal calorimetry of Dewar-Detector Assemblies (DDA) is a routine part of their Acceptance Testing Procedure. In this approach, the cryogenic liquid coolant (typically LN2) is allowed to naturally boil-off from the Dewar well to the atmosphere through a mass flow meter; the parasitic heat load is then evaluated as the product of the latent heat of vaporization and the "last drop" boil-off rate. An inherent major limitation of this technique is that it may be performed only at the fixed boiling temperature of the chosen liquid coolant. A further drawback is related to the explosive nature of "last drop" boiling, manifesting itself as an uneven flow rate. This especially holds true for advanced High Operational Temperature Dewar-Detector Assemblies, typically featuring short cold fingers and working at 150 K and above. In this work, we adapt the well-known technique of dual-slope calorimetry and show how accurate heat load evaluation may be performed by comparing the slopes of the warm-up thermal transients under different trial added heat loads. Because of the simplicity, accuracy and ability to perform calorimetry literally at any temperature of interest, this technique shows good potential for replacing traditional boil-off calorimetry.

  9. Particle flow calorimetry at the international linear collider

    Indian Academy of Sciences (India)

    Logo of the Indian Academy of Sciences. Indian Academy of Sciences. Home · About IASc · History · Memorandum of ... Home; Journals; Pramana – Journal of Physics; Volume 69; Issue 6. Particle flow calorimetry at the international linear collider. Mark A Thomson. Simulation and Reconstruction Volume 69 Issue 6 ...

  10. Particle flow calorimetry at the international linear collider

    Indian Academy of Sciences (India)

    jet energy resolution. It is widely believed that the particle flow approach to calorimetry is the key to achieving the goal of 0.3/. √. E(GeV). This paper describes the current performance of the PandoraPFA particle flow algorithm. For 45GeV jets in the Tesla. TDR detector concept, the ILC jet energy resolution goal is reached.

  11. Hadronic shower development in iron-scintillator tile calorimetry

    Czech Academy of Sciences Publication Activity Database

    Amaral, P.; Amorim, A.; Anderson, K.; Lokajíček, Miloš; Němeček, Stanislav

    2000-01-01

    Roč. 443, - (2000), s. 51-70 ISSN 0168-9002 R&D Projects: GA MPO RP-4210/69 Institutional research plan: CEZ:AV0Z1010920 Keywords : ATLAS Iron-Scintillator * hadron calorimeter * shower parametrisation * calorimetry * computer data analysis Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 0.964, year: 2000

  12. Fast sampling calorimetry with solid argon ionization chambers

    International Nuclear Information System (INIS)

    Clark, E.; Linn, S.; Piekarz, H.; Wahl, H.; Womersley, J.; Hansen, S.; Hurh, P.; Rivetta, C.; Sanders, R.; Schmitt, R.; Stanek, R.; Stefanik, A.

    1992-01-01

    A proposal for the fast sampling calorimetry with solid argon as active medium and the preliminary results from the solid argon test cell are presented. The proposed test calorimeter module structure, the signal routing and the mechanical and cryogenic arrangements are also discussed

  13. Optimization of crystals for applications in dual-readout calorimetry

    Czech Academy of Sciences Publication Activity Database

    Akchurin, N.; Bedeschi, F.; Cardini, A.; Carosi, R.; Ciapetti, G.; Fasoli, M.; Ferrari, R.; Franchino, S.; Fraternali, M.; Gaudio, G.; Hauptman, J.; Incagli, M.; Lacava, F.; La Rotonda, L.; Lee, S.; Livan, M.; Meoni, E.; Nikl, Martin; Pinci, D.; Policicchio, A.; Popescu, S.; Scuri, F.; Sill, A.; Susinno, G.; Vandelli, W.; Vedda, A.; Venturelli, T.; Voena, C.; Volobouev, I.; Wigmans, R.

    2010-01-01

    Roč. 621, 1-3 (2010), 212-221 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10100521 Keywords : calorimetry * Cherenkov light * High-Z scintillating crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.142, year: 2010

  14. Shower maximum detector for SDC calorimetry

    International Nuclear Information System (INIS)

    Ernwein, J.

    1994-01-01

    A prototype for the SDC end-cap (EM) calorimeter complete with a pre-shower and a shower maximum detector was tested in beams of electrons and Π's at CERN by an SDC subsystem group. The prototype was manufactured from scintillator tiles and strips read out with 1 mm diameter wave-length shifting fibers. The design and construction of the shower maximum detector is described, and results of laboratory tests on light yield and performance of the scintillator-fiber system are given. Preliminary results on energy and position measurements with the shower max detector in the test beam are shown. (authors). 4 refs., 5 figs

  15. Topics in calorimetry for high energy physics

    International Nuclear Information System (INIS)

    Hollebeek, R.

    1992-01-01

    These lectures focus on a series of topics now of interest or which have been of interest to designes of calorimeters in the past few years. The examples concentrate on calorimeters from DESY because its focus this year is on e-P physics, and on CDF and SDC because they are best known to the author. Calorimeters are, broadly speaking, devices to measure the total energy of particles. In general, no one device will be optimal for all types of particles. The two broadest classes of calorimeters in high energy physics are the electromagnetic calorimeters used primarily for photons and electrons, and the hadronic calorimeters used for most charged mesons and baryons. Most operate by absorbing and thereby measuring a significant amount of the incoming particles energy directly. Some particles may require special devices for their interactions and observation. Modern calorimeters are characterized by energy and position resolution, and cost and size. Calorimeter cost is often a trade-off between performance desired and money available. The optimum cost will require a careful choice of materials, reduction of the overall size of the detector, elimination of labor intensive construction techniques, and careful consideration of the cost of calibration systems. Since at least some of these requirements which optimize cost and resolution are contradictory, the ideal calorimeter in seldom what one ends up building

  16. A simplistic view of hadron calorimetry

    International Nuclear Information System (INIS)

    Groom, Donald E.

    2007-01-01

    All too often we rely on Monte Carlo simulations without worrying too much about basic physics. It is possible to start with a very simple calorimeter (a big cylinder) and learn the functional form of π/e by an induction argument. Monte Carlo simulations provide sanity checks and constants. A power-law functional form describes test beam results surprisingly well. The prediction that calorimeters respond differently to protons and pions of the same energy was unexpected. The effect was later demonstrated by the CMS forward calorimeter group, using the most noncompensating calorimeter ever built. Calorimeter resolution is dominated by fluctuations in π0 production and the energy deposit by neutrons. The DREAM collaboration has recently used a dual readout calorimeter to eliminate the first of these. Ultimate resolution depends on measuring neutrons on an event-by-event basis as well

  17. A simplistic view of hadron calorimetry

    International Nuclear Information System (INIS)

    Groom, Donald E.

    2006-01-01

    All too often we rely on Monte Carlo simulations without worrying too much about basic physics. It is possible to start with a very simple calorimeter (a big cylinder) and learn the functional form of pi e by an induction argument. Monte Carlo simulations provide sanity checks and constants. A power-law functional form describes test beam results surprisingly well. The prediction that calorimeters respond differently to protons and pions of the same energy was unexpected. The effect was later demonstrated by the CMS forward calorimeter group, using the most noncompensating calorimeter ever built. Calorimeter resolution is dominated by fluctuations in piz production and the energy deposit by neutrons. The DREAM collaboration has recently used a dual readout calorimeter to eliminate the first of these. Ultimate resolution depends on measuring neutrons on an event-by-event basis as well

  18. A Closer Look at Acid-Base Olfactory Titrations

    Science.gov (United States)

    Neppel, Kerry; Oliver-Hoyo, Maria T.; Queen, Connie; Reed, Nicole

    2005-01-01

    Olfactory titrations using raw onions and eugenol as acid-base indicators are reported. An in-depth investigation on olfactory titrations is presented to include requirements for potential olfactory indicators and protocols for using garlic, onions, and vanillin as acid-base olfactory indicators are tested.

  19. Titrated oral misoprostol solution- a new method of labour induction ...

    African Journals Online (AJOL)

    Titrated oral misoprostol solution- a new method of labour induction. ... To develop a new method of misoprostol use for labour induction using very small, frequent, titrated oral dosages, and to pilot effectiveness. Study design. Open clinical pilot ... A multicentre randomised trial of this method is underway. We emphasise the ...

  20. Automated proton titrations of pancreatic phospholipase A2

    NARCIS (Netherlands)

    Donné-Op den Kelder, G.M.; Haas, G.H. de; Egmond, M.R.

    1982-01-01

    A computer-controlled titration system has been developed, tested, and used for analysis of the proton-titration behavior of pancreatic phospholipase A2 from ox, horse, and pig. The results revealed an error in the reported amino acid composition of the equine enzyme. A simple interface for the

  1. a randomised trial comparing Foley catheter plus titrated oral ...

    African Journals Online (AJOL)

    Labour induction at term - a randomised trial comparing. Foley catheter plus titrated oral misoprostol solution, titrated oral misoprostol solution alone, and dinoprostone. Baron B Matonhodze, G Justus Hofmeyr, Jonathan Levin. Objectives. To compare three methods of labour induction. Design. Randomised controlled trial.

  2. The coulometric titration of acids and bases in dimethylsulfoxide media

    NARCIS (Netherlands)

    Bos, M.; IJpma, S.T.; Dahmen, E.A.M.F.

    1976-01-01

    The coulometric titration of 20–200 μeq of acids and bases in DMSO media is described. In the titration of bases, the electro-oxidation of hydrogen at a platinized platinum electrode is used as the source of protons. The conditions for 100 % current efficiency at this electrode are low current

  3. Electrophoretic separation of alginic sodium diester and sodium hexametaphosphate in chondroitin sulfate that interfere with the cetylpyridinium chloride titration assay.

    Science.gov (United States)

    Weiguo, Zhang; Giancaspro, Gabriel; Adams, Kristie M; Neal-Kababick, James; Hildreth, Jana; Li, Aishan; Roman, Mark C; Betz, Joseph M

    2014-01-01

    adulterants in CS and procedures to isolate ASD from CS matrixes containing these adulterants. The authors describe in this paper utilization of an orthogonal approach to establish the identity of Z1 as sodium hexametaphosphate and to confirm the identity of ASD, including ethanol fractionation, FTIR spectroscopy, differential scanning calorimetry, and NMR spectroscopy. The authors suggest that CAME is a cost-effective and easy to use methodfor detecting certain impurities in CS raw ingredients and recommend that CPC and CAME be used in combination by QC laboratories as a means of effectively deterring the practice of adulterating CS raw materials with the known adulterants ASD and Z1 and/or other non-chondroitin substances that can be separated from CSby CAME and that exhibit CPC titration behavior similar to CS.

  4. Conductivity, calorimetry and phase diagram of the NaHSO4–KHSO4 system

    DEFF Research Database (Denmark)

    Hind, Hamma-Cugny; Rasmussen, Søren Birk; Rogez, J.

    2006-01-01

    to polynomials of the form κ(X)=A(X)+B(X)(T-Tm)+C(X)(T-Tm)2, where Tm is the intermediate temperature of the measured temperature range and X, the mole fraction of KHSO4. The possible role of this binary system as a catalyst solvent is also discussed. (C) 2005 Elsevier B.V. All rights reserved.......Physico-chemical properties of the binary system NaHSO4-KHSO4 were studied by calorimetry and conductivity, The enthalpy of mixing has been measured at 505 K in the full composition range and the phase diagram calculated. The phase diagram has also been constructed from phase transition...

  5. A Fixed Flow is More Effective than Titrated Flow during Bubble Nasal CPAP for Respiratory Distress in Preterm Neonates.

    Science.gov (United States)

    Murki, Srinivas; Das, Ratan Kumar; Sharma, Deepak; Kumar, Praveen

    2015-01-01

    The clinical effects of a pre-fixed flow of air-oxygen versus a flow titrated according to visible bubbling are not well understood. To compare the effects of a fixed flow (5 L/min) and titrated flow (flow just enough to ensure bubbling) at different set pressures on delivered intra-prong pressure, gas exchange and clinical parameters in preterm infants on bubble CPAP for respiratory distress. Preterm infants rate, set pressure, FiO2, SpO2, Silverman retraction score, respiratory rate, abdominal girth, and blood gases were recorded. The delivered intra-prong pressure was measured by an electronic manometer. 69 recordings were made in 54 infants. For each of the set CPAP pressures (4, 5, and 6 cm H2O), the mean delivered pressure with a fixed flow of 5 L/min was higher than that delivered by the titrated flow. During the fixed flow epoch, the delivered pressure was closer to and higher than the set pressure resulting in higher PaO2 and lower PaCO2 as compared to titrated flow epoch. In the titrated flow period, the delivered pressure was consistently lower than the set pressure. In preterm infants on bubble CPAP with set pressures of 4-6 cm H2O, a fixed flow of 5 L/min is more effective than a flow titrated to ensure adequate visible bubbling. It achieves higher delivered pressures, better oxygenation and ventilation.

  6. ATLAS calorimetry: Trigger, simulation and jet calibration

    CERN Document Server

    Weber, Pavel

    2008-01-01

    The Pre-Processor system of the ATLAS Level-1 Calorimeter Trigger performs complex processing of analog trigger tower signals from electromagnetic and hadronic calorimeters. The main processing block of the Pre-Processor System is the Multi-Chip Module (MCM). The first part of this thesis describes MCM quality assurance tests that have been developed, their use in the MCM large scale production and the results that have been obtained. In the second part of the thesis a validation of a shower parametrisation model for the ATLAS fast simulation package ATLFAST based on QCD dijet events is performed. A detailed comparison of jet response and jet energy resolution between the fast and the full simulation is presented. The uniformity of the calorimeter response has a significant impact on the accuracy of the jet energy measurement. A study of the calorimeter intercalibration using QCD dijet events is presented in the last part of the thesis. The intercalibration study is performed in azimuth angle phi and in pseud...

  7. ATLAS calorimetry. Trigger, simulation and jet calibration

    Energy Technology Data Exchange (ETDEWEB)

    Weber, P.

    2007-02-06

    The Pre-Processor system of the ATLAS Level-1 Calorimeter Trigger performs complex processing of analog trigger tower signals from electromagnetic and hadronic calorimeters. The main processing block of the Pre-Processor System is the Multi-Chip Module (MCM). The first part of this thesis describes MCM quality assurance tests that have been developed, their use in the MCM large scale production and the results that have been obtained. In the second part of the thesis a validation of a shower parametrisation model for the ATLAS fast simulation package ATLFAST based on QCD dijet events is performed. A detailed comparison of jet response and jet energy resolution between the fast and the full simulation is presented. The uniformity of the calorimeter response has a significant impact on the accuracy of the jet energy measurement. A study of the calorimeter intercalibration using QCD dijet events is presented in the last part of the thesis. The intercalibration study is performed in azimuth angle {phi} and in pseudorapidity {eta}. The performance of the calibration methods including possible systematic and statistical effects is described. (orig.)

  8. Water calorimetry and ionization chamber dosimetry in an 85-MeV clinical proton beam.

    Science.gov (United States)

    Palmans, H; Seuntjens, J; Verhaegen, F; Denis, J M; Vynckier, S; Thierens, H

    1996-05-01

    In recent years, the increased use of proton beams for clinical purposes has enhanced the demand for accurate absolute dosimetry for protons. As calorimetry is the most direct way to establish the absorbed dose and because water has recently been accepted as standard material for this type of beam, the importance of water calorimetry is obvious. In this work we report water calorimeter operation in an 85-MeV proton beam and a comparison of the absorbed dose to water measured by ionometry with the dose resulting from water calorimetric measurements. To ensure a proper understanding of the heat defect for defined impurities in water for this type of radiation, a relative response study was first done in comparison with theoretical calculations of the heat defect. The results showed that pure hypoxic water and hydrogen-saturated water yielded the same response with practically zero heat defect, in agreement with the model calculations. The absorbed dose inferred from these measurements was then compared with the dose derived from ionometry by applying the European Charged Heavy Particle Dosimetry (ECHED) protocol. Restricting the comparison to chambers recommended in the protocol, the calorimeter dose was found to be 2.6% +/- 0.9% lower than the average ionometry dose. In order to estimate the significance of chamber-dependent effects in this deviation, measurements were performed using a set of ten ionization chambers of five different types. The maximum internal deviation in the ionometry results amounted to 1.1%. We detected no systematic chamber volume dependence, but observed a small but systematic effect of the chamber wall thickness. The observed deviation between calorimetry and ionometry can be attributed to a combination of the value of (Wair/e)p for protons, adopted in the ECHED protocol, the mass stopping power ratios of water to air for protons, and possibly small ionization chamber wall effects.

  9. Trace analysis of acids and bases by conductometric titration with multiparametric non-linear regression.

    Science.gov (United States)

    Coelho, Lúcia H G; Gutz, Ivano G R

    2006-03-15

    A chemometric method for analysis of conductometric titration data was introduced to extend its applicability to lower concentrations and more complex acid-base systems. Auxiliary pH measurements were made during the titration to assist the calculation of the distribution of protonable species on base of known or guessed equilibrium constants. Conductivity values of each ionized or ionizable species possibly present in the sample were introduced in a general equation where the only unknown parameters were the total concentrations of (conjugated) bases and of strong electrolytes not involved in acid-base equilibria. All these concentrations were adjusted by a multiparametric nonlinear regression (NLR) method, based on the Levenberg-Marquardt algorithm. This first conductometric titration method with NLR analysis (CT-NLR) was successfully applied to simulated conductometric titration data and to synthetic samples with multiple components at concentrations as low as those found in rainwater (approximately 10 micromol L(-1)). It was possible to resolve and quantify mixtures containing a strong acid, formic acid, acetic acid, ammonium ion, bicarbonate and inert electrolyte with accuracy of 5% or better.

  10. Development and validation of a simplified titration method for monitoring volatile fatty acids in anaerobic digestion.

    Science.gov (United States)

    Sun, Hao; Guo, Jianbin; Wu, Shubiao; Liu, Fang; Dong, Renjie

    2017-09-01

    The volatile fatty acids (VFAs) concentration has been considered as one of the most sensitive process performance indicators in anaerobic digestion (AD) process. However, the accurate determination of VFAs concentration in AD processes normally requires advanced equipment and complex pretreatment procedures. A simplified method with fewer sample pretreatment procedures and improved accuracy is greatly needed, particularly for on-site application. This report outlines improvements to the Nordmann method, one of the most popular titrations used for VFA monitoring. The influence of ion and solid interfering subsystems in titrated samples on results accuracy was discussed. The total solid content in titrated samples was the main factor affecting accuracy in VFA monitoring. Moreover, a high linear correlation was established between the total solids contents and VFA measurement differences between the traditional Nordmann equation and gas chromatography (GC). Accordingly, a simplified titration method was developed and validated using a semi-continuous experiment of chicken manure anaerobic digestion with various organic loading rates. The good fitting of the results obtained by this method in comparison with GC results strongly supported the potential application of this method to VFA monitoring. Copyright © 2017. Published by Elsevier Ltd.

  11. Equivalence of nasal and oronasal masks during initial CPAP titration for obstructive sleep apnea syndrome.

    Science.gov (United States)

    Teo, Ming; Amis, Terence; Lee, Sharon; Falland, Karina; Lambert, Stephen; Wheatley, John

    2011-07-01

    Continuous positive airway pressure (CPAP) titration studies are commonly performed using a nasal mask but some patients may prefer a full-face or oronasal mask. There is little evidence regarding the equivalence of different mask interfaces used to initiate treatment. We hypothesized that oronasal breathing when using an oronasal mask increases upper airway collapsibility and that a higher pressure may be required to maintain airway patency. We also assessed patient preferences for the 2 mask interfaces. Prospective, randomized, cross-over design with 2 consecutive CPAP titration nights. Accredited laboratory in a university hospital. Twenty-four treatment-naive subjects with obstructive sleep apnea syndrome and respiratory disturbance index of greater than 15 events per hour. CPAP titration was performed using an auto-titrating machine with randomization to a nasal or oronasal mask, followed by a second titration night using the alternate mask style. There was no significant difference in the mean pressures determined between nasal and oronasal masks, although 43% of subjects had nasal-to-oronasal mask-pressure differences of 2 cm H(2)O or more. Residual respiratory events, arousals, and measured leak were all greater with the oronasal mask. Seventy-nine percent of subjects preferred the nasal mask. Patients with obstructive sleep apnea syndrome can generally switch between nasal and oronasal masks without changing machine pressure, although there are individual differences that may be clinically significant. Measured leak is greater with the oronasal mask. Most patients with obstructive sleep apnea syndrome prefer a nasal mask as the interface for initiation of CPAP. Australian New Zealand Clinical Trials Registry (ANZCTR). ACTRN: ACTRN12611000243910. URL: http://www.ANZCTR.org.au/ACTRN12611000243910.aspx

  12. The Mobile Insulin Titration Intervention (MITI) for Insulin Glargine Titration in an Urban, Low-Income Population: Randomized Controlled Trial Protocol.

    Science.gov (United States)

    Levy, Natalie; Moynihan, Victoria; Nilo, Annielyn; Singer, Karyn; Bernik, Lidia S; Etiebet, Mary-Ann; Fang, Yixin; Cho, James; Natarajan, Sundar

    2015-03-13

    Patients on insulin glargine typically visit a clinician to obtain advice on how to adjust their insulin dose. These multiple clinic visits can be costly and time-consuming, particularly for low-income patients. It may be feasible to achieve insulin titration through text messages and phone calls with patients instead of face-to-face clinic visits. The objectives of this study are to (1) evaluate if the Mobile Insulin Titration Intervention (MITI) is clinically effective by helping patients reach their optimal dose of insulin glargine, (2) determine if the intervention is feasible within the setting and population, (3) assess patient satisfaction with the intervention, and (4) measure the costs associated with this intervention. This is a pilot study evaluating an approach to insulin titration using text messages and phone calls among patients with insulin-dependent type 2 diabetes in the outpatient medical clinic of Bellevue Hospital Center, a safety-net hospital in New York City. Patients will be randomized in a 1:1 ratio to either the MITI arm (texting/phone call intervention) or the usual-care arm (in-person clinic visits). Using a Web-based platform, weekday text messages will be sent to patients in the MITI arm, asking them to text back their fasting blood glucose values. In addition to daily reviews for alarm values, a clinician will rereview the texted values weekly, consult our physician-approved titration algorithm, and call the patients with advice on how to adjust their insulin dose. The primary outcome will be whether or not a patient reaches his/her optimal dose of insulin glargine within 12 weeks. Recruitment for this study occurred between June 2013 and December 2014. We are continuing to collect intervention and follow-up data from our patients who are currently enrolled. The results of our data analysis are expected to be available in 2015. This study explores the use of widely-available text messaging and voice technologies for insulin titration

  13. A single-beam titration method for the quantification of open-path Fourier transform infrared spectroscopy

    International Nuclear Information System (INIS)

    Sung, Lung-Yu; Lu, Chia-Jung

    2014-01-01

    This study introduced a quantitative method that can be used to measure the concentration of analytes directly from a single-beam spectrum of open-path Fourier Transform Infrared Spectroscopy (OP-FTIR). The peak shapes of the analytes in a single-beam spectrum were gradually canceled (i.e., “titrated”) by dividing an aliquot of a standard transmittance spectrum with a known concentration, and the sum of the squared differential synthetic spectrum was calculated as an indicator for the end point of this titration. The quantity of a standard transmittance spectrum that is needed to reach the end point can be used to calculate the concentrations of the analytes. A NIST traceable gas standard containing six known compounds was used to compare the quantitative accuracy of both this titration method and that of a classic least square (CLS) using a closed-cell FTIR spectrum. The continuous FTIR analysis of industrial exhausting stack showed that concentration trends were consistent between the CLS and titration methods. The titration method allowed the quantification to be performed without the need of a clean single-beam background spectrum, which was beneficial for the field measurement of OP-FTIR. Persistent constituents of the atmosphere, such as NH 3 , CH 4 and CO, were successfully quantified using the single-beam titration method with OP-FTIR data that is normally inaccurate when using the CLS method due to the lack of a suitable background spectrum. Also, the synthetic spectrum at the titration end point contained virtually no peaks of analytes, but it did contain the remaining information needed to provide an alternative means of obtaining an ideal single-beam background for OP-FTIR. - Highlights: • Establish single beam titration quantification method for OP-FTIR. • Define the indicator for the end-point of spectrum titration. • An ideal background spectrum can be obtained using single beam titration. • Compare the quantification between titration

  14. Particle flow calorimetry at the international linear collider

    Indian Academy of Sciences (India)

    For 45GeV jets in the Tesla. TDR detector concept, the ILC jet energy resolution goal is reached. At higher energies the jet energy resolution becomes worse and can be described by the empirical expression: σE /E ≈ 0.265/. √. E(GeV) + 1.2 × 10−4E(GeV). Keywords. Calorimetry; particle flow. PACS Nos 07.05.Kf; 29.40.

  15. The Philosophy and Feasibility of Dual Readout Calorimetry

    International Nuclear Information System (INIS)

    Hauptman, John

    2006-01-01

    I will discuss the general physical ideas behind dual-readout calorimetry, their implementation in DREAM (Dual REAdout Module) with exact separation of scintillation and Cerenkov light, implementation with mixed light in DREAM fibers, anticipated implementation in PbWO4 crystals with applications to the 4th Concept detector and to CMS, use in high energy gamma-ray and cosmic ray astrophysics with Cerenkov and N2 fluorescent light, and implementation in the 4th Concept detector for muon identification

  16. Accurate label-free reaction kinetics determination using initial rate heat measurements

    Science.gov (United States)

    Ebrahimi, Kourosh Honarmand; Hagedoorn, Peter-Leon; Jacobs, Denise; Hagen, Wilfred R.

    2015-01-01

    Accurate label-free methods or assays to obtain the initial reaction rates have significant importance in fundamental studies of enzymes and in application-oriented high throughput screening of enzyme activity. Here we introduce a label-free approach for obtaining initial rates of enzyme activity from heat measurements, which we name initial rate calorimetry (IrCal). This approach is based on our new finding that the data recorded by isothermal titration calorimetry for the early stages of a reaction, which have been widely ignored, are correlated to the initial rates. Application of the IrCal approach to various enzymes led to accurate enzyme kinetics parameters as compared to spectroscopic methods and enabled enzyme kinetic studies with natural substrate, e.g. proteases with protein substrates. Because heat is a label-free property of almost all reactions, the IrCal approach holds promise in fundamental studies of various enzymes and in use of calorimetry for high throughput screening of enzyme activity. PMID:26574737

  17. Test in a beam of large-area Micromegas chambers for sampling calorimetry

    CERN Document Server

    Adloff, C.; Dalmaz, A.; Drancourt, C.; Gaglione, R.; Geffroy, N.; Jacquemier, J.; Karyotakis, Y.; Koletsou, I.; Peltier, F.; Samarati, J.; Vouters, G.

    2014-06-11

    Application of Micromegas for sampling calorimetry puts specific constraints on the design and performance of this gaseous detector. In particular, uniform and linear response, low noise and stability against high ionisation density deposits are prerequisites to achieving good energy resolution. A Micromegas-based hadronic calorimeter was proposed for an application at a future linear collider experiment and three technologically advanced prototypes of 1$\\times$1 m$^{2}$ were constructed. Their merits relative to the above-mentioned criteria are discussed on the basis of measurements performed at the CERN SPS test-beam facility.

  18. Determination of magnetic characteristics of nanoparticles by low-temperature calorimetry methods

    Energy Technology Data Exchange (ETDEWEB)

    Ugulava, A.; Toklikishvili, Z. [Department of Physics, I.Javakhishvili Tbilisi State University,I.Chavchavadze av. 3, 0179 Tbilisi, Georgia (United States); Chkhaidze, S., E-mail: simon.chkhaidze@tsu.ge [Department of Physics, I.Javakhishvili Tbilisi State University,I.Chavchavadze av. 3, 0179 Tbilisi, Georgia (United States); Kekutia, Sh. [V. Chavchanidze Institute of Cybernetics, at the Technical State University, S. Euli str. 5, 0186 Tbilisi, Georgia (United States)

    2017-05-15

    At low temperatures, the heat capacity of a superparamagnetic “ideal gas” determined by magnetic degrees of freedom can greatly exceed the lattice heat capacity. It is shown that in the presence of an external magnetic field, the temperature dependence of the magnetic part of the heat capacity has two maxima. The relations between the temperature at which these maxima are achieved, the magnetic moment of the nanoparticles and the magnetic anisotropy constant have been obtained. Measuring the heat capacity maxima temperatures by low-temperature calorimetry methods and using the obtained relations, we can obtain the numerical values both of the magnetic moment of nanoparticles and the magnetic anisotropy constants.

  19. Titration and hysteresis in epigenetic chromatin silencing

    Science.gov (United States)

    Dayarian, Adel; Sengupta, Anirvan M.

    2013-06-01

    Epigenetic mechanisms of silencing via heritable chromatin modifications play a major role in gene regulation and cell fate specification. We consider a model of epigenetic chromatin silencing in budding yeast and study the bifurcation diagram and characterize the bistable and the monostable regimes. The main focus of this paper is to examine how the perturbations altering the activity of histone modifying enzymes affect the epigenetic states. We analyze the implications of having the total number of silencing proteins, given by the sum of proteins bound to the nucleosomes and the ones available in the ambient, to be constant. This constraint couples different regions of chromatin through the shared reservoir of ambient silencing proteins. We show that the response of the system to perturbations depends dramatically on the titration effect caused by the above constraint. In particular, for a certain range of overall abundance of silencing proteins, the hysteresis loop changes qualitatively with certain jump replaced by continuous merger of different states. In addition, we find a nonmonotonic dependence of gene expression on the rate of histone deacetylation activity of Sir2. We discuss how these qualitative predictions of our model could be compared with experimental studies of the yeast system under anti-silencing drugs.

  20. Titration and hysteresis in epigenetic chromatin silencing

    International Nuclear Information System (INIS)

    Dayarian, Adel; Sengupta, Anirvan M

    2013-01-01

    Epigenetic mechanisms of silencing via heritable chromatin modifications play a major role in gene regulation and cell fate specification. We consider a model of epigenetic chromatin silencing in budding yeast and study the bifurcation diagram and characterize the bistable and the monostable regimes. The main focus of this paper is to examine how the perturbations altering the activity of histone modifying enzymes affect the epigenetic states. We analyze the implications of having the total number of silencing proteins, given by the sum of proteins bound to the nucleosomes and the ones available in the ambient, to be constant. This constraint couples different regions of chromatin through the shared reservoir of ambient silencing proteins. We show that the response of the system to perturbations depends dramatically on the titration effect caused by the above constraint. In particular, for a certain range of overall abundance of silencing proteins, the hysteresis loop changes qualitatively with certain jump replaced by continuous merger of different states. In addition, we find a nonmonotonic dependence of gene expression on the rate of histone deacetylation activity of Sir2. We discuss how these qualitative predictions of our model could be compared with experimental studies of the yeast system under anti-silencing drugs. (paper)

  1. Comparison of NO titration and fiber optics catalytic probes for determination of neutral oxygen atom concentration in plasmas and postglows

    International Nuclear Information System (INIS)

    Mozetic, Miran; Ricard, Andre; Babic, Dusan; Poberaj, Igor; Levaton, Jacque; Monna, Virginie; Cvelbar, Uros

    2003-01-01

    A comparative study of two different absolute methods NO titration and fiber optics catalytic probe (FOCP) for determination of neutral oxygen atom density is presented. Both methods were simultaneously applied for measurements of O density in a postglow of an Ar/O 2 plasma created by a surfatron microwave generator with the frequency of 2.45 GHz an adjustable output power between 30 and 160 W. It was found that the two methods gave similar results. The advantages of FOCP were found to be as follows: it is a nondestructive method, it enables real time measuring of the O density, it does not require any toxic gas, and it is much faster than NO titration. The advantage of NO titration was found to be the ability to measure O density in a large range of dissociation of oxygen molecules

  2. A dipstick sensor for coulometric acid-base titrations

    OpenAIRE

    Olthuis, Wouter; van der Schoot, B.H.; Chavez, F.; Bergveld, Piet

    1989-01-01

    By performing an acid-base titration by coulometric generation of OH− or H+ ions at an inert electrode in close proximity to the pH-sensitive gate of an ISFET, it is possible to determine the acid or base concentration of a solution using the ISFET as an indicator device for the equivalence point in the titration curve. Typical values for the titration time are 0.1 to 10 s for acid or base concentrations ranging from 0.5 × 10−3 to 10 × 10−3 mol/l. By placing the counter electrode for the supp...

  3. The fluorimetric titration of zirconium in the ppm-range

    International Nuclear Information System (INIS)

    Linden, W.E. von der; Boef, G. den; Ozinga, W.

    1976-01-01

    A fluorimetric titration of zirconium(IV) with EDTA is proposed. The fluorescence intensity of the zirconium-morin complex is used to indicate the end-point. More than twenty other cations were investigated and it was found that they did not interfere, neither did common anions. Mercury(II) can only be tolerated in amount not exceeding that of zirconium. Bismuth(III) interferes and hafnium(IV0 is titrated together with zirconium. The relative standard deviation of the titration of 10ml of a solution containing 1 ppm of zirconium does not exceed 1.5%

  4. Determination of boron as boric acid by automatic potentiometric titration

    International Nuclear Information System (INIS)

    Midgley, D.

    1988-06-01

    Boron in PWR primary coolant and related waters may be determined as boric acid by titration with sodium hydroxide, using a glass electrode as a pH indicator. With a modern automatic titrator, the analysis is quick, convenient, accurate and precise. In the titration of 8 mg B (e.g. 4 ml of 2000 mg 1 -1 solution), no significant bias was observed and relative standard deviations were about 0.25%. With 0.8 g B, a bias of about 2% appears, although this could be reduced by restandardizing the titrant, but the relative standard deviation was still -1 B, depending on the stage of the fuel cycle. (author)

  5. Protofit: A program for determining surface protonation constants from titration data

    Science.gov (United States)

    Turner, Benjamin F.; Fein, Jeremy B.

    2006-11-01

    Determining the surface protonation behavior of natural adsorbents is essential to understand how they interact with their environments. ProtoFit is a tool for analysis of acid-base titration data and optimization of surface protonation models. The program offers a number of useful features including: (1) enables visualization of adsorbent buffering behavior; (2) uses an optimization approach independent of starting titration conditions or initial surface charge; (3) does not require an initial surface charge to be defined or to be treated as an optimizable parameter; (4) includes an error analysis intrinsically as part of the computational methods; and (5) generates simulated titration curves for comparison with observation. ProtoFit will typically be run through ProtoFit-GUI, a graphical user interface providing user-friendly control of model optimization, simulation, and data visualization. ProtoFit calculates an adsorbent proton buffering value as a function of pH from raw titration data (including pH and volume of acid or base added). The data is reduced to a form where the protons required to change the pH of the solution are subtracted out, leaving protons exchanged between solution and surface per unit mass of adsorbent as a function of pH. The buffering intensity function Qads* is calculated as the instantaneous slope of this reduced titration curve. Parameters for a surface complexation model are obtained by minimizing the sum of squares between the modeled (i.e. simulated) buffering intensity curve and the experimental data. The variance in the slope estimate, intrinsically produced as part of the Qads* calculation, can be used to weight the sum of squares calculation between the measured buffering intensity and a simulated curve. Effects of analytical error on data visualization and model optimization are discussed. Examples are provided of using ProtoFit for data visualization, model optimization, and model evaluation.

  6. Novel indirect calorimetry technology to analyze metabolism in individual neonatal rodent pups.

    Directory of Open Access Journals (Sweden)

    Jesus F Dominguez

    Full Text Available BACKGROUND: The ability to characterize the development of metabolic function in neonatal rodents has been limited due to technological constraints. Low respiratory volumes and flows at rest pose unique problems, making it difficult to reliably measure O(2 consumption, CO(2 production, respiratory quotient (RQ, and energy expenditure (EE. Our aim was to develop and validate a commercial-grade indirect calorimetry system capable of characterizing the metabolic phenotype of individual neonatal rodents. METHODOLOGY/PRINCIPAL FINDINGS: To address this research need, we developed a novel, highly sensitive open-circuit indirect calorimetry system capable of analyzing respiratory gas exchange in a single neonatal rodent pup. Additionally, we derived an equation from known metabolic relationships to estimate inlet flow rates, improving the efficiency of data collection. To validate the neonatal rodent indirect calorimetry system and evaluate the applicability of the derived equation for predicting appropriate flow rates, we conducted a series of experiments evaluating the impact of sex, litter size, time of day (during the light phase, and ambient temperature on neonatal rat metabolic parameters. Data revealed that the only metabolic parameter influenced by litter size is a neonatal rat's RQ, with rat pups reared in a small litter (5 pups having lower RQ's than rat pups reared in either medium (8 pups or large (11 pups litters. Furthermore, data showed that ambient temperature affected all metabolic parameters measured, with colder temperatures being associated with higher CO(2 production, higher O(2 consumption, and higher energy expenditure. CONCLUSION/SIGNIFICANCE: The results of this study demonstrate that the modified Panlab Oxylet system reliably assesses early postnatal metabolism in individual neonatal rodents. This system will be of paramount importance to further our understanding of processes associated with the developmental origins of adult

  7. Absolute determination of small samples of Pu and Am by calorimetry

    International Nuclear Information System (INIS)

    Tagziria, H.; Bagi, J.; Pedersen, B.; Schillebeeckx, P.

    2012-01-01

    An extensive measurement campaign has been carried in order to recalibrate and assess the performance of the small sample calorimeter (SSCAL) that was recently upgraded. The measurements have been performed in the Performance Laboratory of the Joint Research Centre's (JRC) Nuclear Security Unit in Ispra (Italy) using calibrated electric heat sources and standard reference nuclear materials. The SSCAL is a heat flow calorimeter which works by measuring the voltage generated by a heat-emitting sample across a thermal gap based on a thermopile cup technology. Results of calorimetry measurements carried out, both inside and outside a well-controlled environment of a climatic chamber, on reference Pu–Ga samples and well-characterised 241 Am samples are presented and discussed. The latter samples were produced at the JRC-ITU to be used by the JRC-IRMM for various cross-section measurements (total, neutron capture and 241 Am(n,2n) 240 Am).

  8. Thin-film calorimetry. In-situ characterization of materials for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Omelcenko, Alexander; Wulfmeier, Hendrik; Albrecht, Daniel; Fritze, Holger [Clausthal Univ. of Technology, Goslar (Germany). Inst. of Energy Research and Physical Technologies; El Mofid, Wassima; Ivanov, Svetlozar; Bund, Andreas [Ilmenau Univ. of Technology (Germany). Dept. of Electrochemistry

    2017-11-15

    Thin-film calorimetry allows for qualitative and quantitative in-situ analysis of thermodynamic properties of thin films and thin-film systems from room temperature up to 1000 C. It is based on highly sensitive piezoelectric langasite resonators which serve simultaneously as planar temperature sensors and substrates for the films of interest. Generation or consumption of heat during phase transformations of the films cause deviations from the regular course of the resonance frequency. Thermodynamic data such as phase transformation temperatures and enthalpies are extracted from these deviations. Thin-film calorimetry on Sn and Al thin films is performed to prove the concept. The results demonstrate high reproducibility of the measurement approach and are in agreement with literature data obtained by established calorimetric techniques. The calibration of the system is done in different atmospheres by application of defined heat pulses via heating structures. The latter replace the films of interest and simulate phase transformations to provide detailed analysis of the heat transfer mechanisms occurring in the measurement system. Based on this analysis, a data evaluation concept is developed. Application-relevant studies are performed on thin films of the lithium-ion battery materials NMC(A), NCA, LMO, and MoS{sub 2}. Their phase transformation temperatures and enthalpies are evaluated in oxidizing and reducing atmospheres. Furthermore, their thermodynamic stability ranges are presented. Finally, measurements on all-solid-state thin-film batteries during electrochemical cycling are performed. They demonstrate the suitability of the system for in-situ investigations.

  9. Green chemistry volumetric titration kit for pharmaceutical formulations: Econoburette

    Directory of Open Access Journals (Sweden)

    Man Singh

    2009-08-01

    Full Text Available Stopcock SC and Spring Sp models of Econoburette (Calibrated, RTC (NR, Ministry of Small Scale Industries, Government of India, developed for semimicro volumetric titration of pharmaceutical formulations are reported. These are economized and risk free titration where pipette is replaced by an inbuilt pipette and conical flask by inbuilt bulb. A step of pipetting of stock solution by mouth is deleted. It is used to allow solution exposure to user’s body. This risk is removed and even volatile and toxic solutions are titrated with full proof safety. Econoburette minimizes use of materials and time by 90 % and prevent discharge of polluting effluent to environment. Few acid and base samples are titrated and an analysis of experimental expenditure is described in the papers.

  10. Spectrophotometric titration of sulfates in the presence of zirconium

    International Nuclear Information System (INIS)

    Kuznetsov, V.V.; Kotova, S.S.; Molokanova, L.G.; Chekmarev, A.M.; Yagodin, G.A.

    1978-01-01

    The procedure has been proposed for express determination of sulphate ions in the presence of zirconium by spectrophotometric titration with the use of barium chloride and nitrochromazo as an indicator. The procedure is based on bonding zirconium into a more stable complex with EDTA (ethylenediaminotetraacetic acid). The presence of excess of EDTA and zirconium (4) complexonate in the solution being titrated does not affect the titration curve shape and the character of break on the curve in the equivalence point. A complete demasking of SO 4 2- is observed in the case of 1O-fold excess of EDTA with respect to zirconium (4). Statistic evaluation of the method has shown that the results of titration can be distorted by chance errors only

  11. Coulometric titration of niobium in 1F sulfuric acid

    International Nuclear Information System (INIS)

    Pannu, S.S.

    1975-01-01

    A coulometric titration at constant current has been devised for Nb in 1F sulfuric acid. The titration was based on the oxidation of Nb(III) to Nb(V) by Fe(III) electrogenerated at a graphite anode. Both potentiometric and amperometric end points were used. The Nb(V) was prior reduced at a mercury cathode by exhaustive electrolysis at a current density of 15 ma/mc 2 for at least 10 hr. Ta,V,Ti and a working platinum anode interfered, but the separation of the potentials of Nb(V)/Nb(III) and Ti(IV)/Ti(III) permitted the titration of first Nb and then Ti. The average error for the titration of 0.30 to 13.00 mg of niobium in 100 ml of 1F sulfuric acid was + 0.57%. (author)

  12. Coulometric titration of niobium in EDTA complexing solution

    International Nuclear Information System (INIS)

    Pannu, S.S.

    1976-01-01

    Constant current coulometry of Nb in EDTA was studied employing both potentiometric and amperometric end-point techniques. The titrations were based on the oxidation of Nb(IV)-EDTA with electrogenerated Fe(III) at a graphite anode. The rate of disproportionation of Nb(IV)-EDTA was found to be slow enough not to effect the accuracy sought for the titration. The coulometric titration of Nb in EDTA was found to be more accurate than in 1F sulfuric acid. The mean error in the titrations of 4.76 to 19.65 of Nb in a volume of about 100 ml of 0.02 to 0.04F EDTA was 0.13%. It was found that Ta may be tolerated to a ratio of 1:4, Ta:Nb, in a solution containing 13 mg of Nb. (author)

  13. Potentiometric titration of free acid in uranium solutions

    Energy Technology Data Exchange (ETDEWEB)

    Suh, M. Y.; Kim, W. H.; Kim, J. S.; Sohn, S. C.; Eom, T. Y.; Lee, C. H.; Jeon, Y. S.; Han, S. H.

    1998-02-01

    Hydrolysis properties of metal cations and fundamental principles of the potentiometric titration of free acid in aqueous solutions containing metal cations were described. The published papers and reports for the alkalimetric and acidimetric titration of free acid were surveyed, and the applicability of these titration methods to the uranium and/or plutonium solutions were discussed. This technical report also includes the various results obtained from the authors` researches to establish the alkalimetric and acidimetric titration methods for the determination of free acid in nitric acid solutions containing uranium and/or oxalic acid, and aluminum. The procedure manuals used in chemical processes and the newly prepared manuals based on the authors` researches are appended. (author). 26 refs., 54 figs.

  14. Microscope Titration and Extraction of DNA from Liver.

    Science.gov (United States)

    Mayo, Lois T.; And Others

    1993-01-01

    Describes a simple and inexpensive, one-period activity to extract DNA to make the study of DNA less abstract. A microscope titration is used to determine when cells are ready for DNA extraction. (PR)

  15. A microcomputer-controlled system for titration analysis

    NARCIS (Netherlands)

    Boelema, Gerrit Jan

    1982-01-01

    This thesis deals with the results of the implementation of microprocessor technology in automatic titration equipment to obtain a versatile system for pharmaceutical, chemical analytical and optimization research purposes. ... Zie: Summary

  16. Analysis of the Purity of Cetrimide by Titrations

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov; Rasmussen, Claus/Dallerup; Nielsen, Hans/Boye

    2006-01-01

    The purity of cetrimide, trimethyl tetradecyl ammonium bromide (TTAB), that is an important preservative of many cosmetic and pharmaceutical products, was determined by three independent methods of titration. Traditionally, cetrimide was analysed by an assay method of the European Pharmacopoeia (Ph....... Eur.), which showed consistently a low purity of cetrimide with large standard deviations associated, however. A systematic 3% bias of the Ph. Eur. assay method was identified by comparing the result with results of two alternative methods of titration that exhibited high precision and high accuracy....... Titration by perchloric acid showed a 99.69 ± 0.05 % purity of cetrimide and titration by silver nitrate showed a 99.85% ± 0.05 % purity while the traditional assay method predicted a purity of only 97.1 ± 0.4. It was found that the discrepancy could be identified as differences in selectivity during...

  17. Plutonium volumetric titration after reduction on a Jones' column

    International Nuclear Information System (INIS)

    Description of a plutonium analysis method, in hydrochloric or sulfuric solution, for plutonium content over 2 mg, by reduction from plutonium IV to plutonium III in a Jones' column. Volumetic titration by ceric sulfate with ferrous orthophenanthroline [fr

  18. Amperometric titration of indium with edta solution in propanol

    International Nuclear Information System (INIS)

    Gevorgyan, A.M.; Talipov, Sh.T.; Khadeev, V.A.; Kostylev, V.S.; Khadeeva, L.A.

    1980-01-01

    Optimum conditions have been chosen for titration of indium with EDTA solution in anhydrous propanol and its mixtures with some aprotic solvents using amperometric and point detection. A procedure is suggested of determining indium microcontents in the presence of large amounts of other elements. The procedure is based on its extraction preseparation followed by direct titration in the extract with a standard EDTA solution [ru

  19. Potentiometric and coulometric titration of 2-thiobarbituric acid.

    Science.gov (United States)

    Ciesielski, W; Kowalska, J; Zakrzewski, R

    1995-05-01

    A new method for the determination of 2-thiobarbituric acid, using its reaction with iodine in an alkaline medium is presented. In the volumetric titration with potentiometric end-point detection, the determinability range is 10-400 micromol (1.4-58 mg). In coulometric titration using the biamperometric end-point detection, 0.1-20 micromol (1.4 x 10(-2)-2.9 mg) of 2-thiobarbituric acid was successfully determined.

  20. Gran method for end point anticipation in monosegmented flow titration

    Directory of Open Access Journals (Sweden)

    Aquino Emerson V

    2004-01-01

    Full Text Available An automatic potentiometric monosegmented flow titration procedure based on Gran linearisation approach has been developed. The controlling program can estimate the end point of the titration after the addition of three or four aliquots of titrant. Alternatively, the end point can be determined by the second derivative procedure. In this case, additional volumes of titrant are added until the vicinity of the end point and three points before and after the stoichiometric point are used for end point calculation. The performance of the system was assessed by the determination of chloride in isotonic beverages and parenteral solutions. The system employs a tubular Ag2S/AgCl indicator electrode. A typical titration, performed according to the IUPAC definition, requires only 60 mL of sample and about the same volume of titrant (AgNO3 solution. A complete titration can be carried out in 1 - 5 min. The accuracy and precision (relative standard deviation of ten replicates are 2% and 1% for the Gran and 1% and 0.5% for the Gran/derivative end point determination procedures, respectively. The proposed system reduces the time to perform a titration, ensuring low sample and reagent consumption, and full automatic sampling and titrant addition in a calibration-free titration protocol.

  1. Percent relative cumulative frequency analysis in indirect calorimetry: application to studies of transgenic mice.

    Science.gov (United States)

    Riachi, Marc; Himms-Hagen, Jean; Harper, Mary-Ellen

    2004-12-01

    Indirect calorimetry is commonly used in research and clinical settings to assess characteristics of energy expenditure. Respiration chambers in indirect calorimetry allow measurements over long periods of time (e.g., hours to days) and thus the collection of large sets of data. Current methods of data analysis usually involve the extraction of only a selected small proportion of data, most commonly the data that reflects resting metabolic rate. Here, we describe a simple quantitative approach for the analysis of large data sets that is capable of detecting small differences in energy metabolism. We refer to it as the percent relative cumulative frequency (PRCF) approach and have applied it to the study of uncoupling protein-1 (UCP1) deficient and control mice. The approach involves sorting data in ascending order, calculating their cumulative frequency, and expressing the frequencies in the form of percentile curves. Results demonstrate the sensitivity of the PRCF approach for analyses of oxygen consumption (.VO2) as well as respiratory exchange ratio data. Statistical comparisons of PRCF curves are based on the 50th percentile values and curve slopes (H values). The application of the PRCF approach revealed that energy expenditure in UCP1-deficient mice housed and studied at room temperature (24 degrees C) is on average 10% lower (p lower environmental temperature, there were no differences in .VO2 between groups. The latter is likely due to augmented shivering thermogenesis in UCP1-deficient mice compared with controls. With the increased availability of murine models of metabolic disease, indirect calorimetry is increasingly used, and the PRCF approach provides a novel and powerful means for data analysis.

  2. Comparison of 3 titration methods of positive airway pressure for obstructive sleep apnea syndrome: a random, single-blind and self-control clinical study

    Directory of Open Access Journals (Sweden)

    Yan LI

    2013-05-01

    APAP titration are effective in treatment with moderate or severe simple OSAS, the measured mean pressure may be used to define the optimal therapeutic pressure of CPAP.

  3. Silk I and Silk II studied by fast scanning calorimetry.

    Science.gov (United States)

    Cebe, Peggy; Partlow, Benjamin P; Kaplan, David L; Wurm, Andreas; Zhuravlev, Evgeny; Schick, Christoph

    2017-06-01

    Using fast scanning calorimetry (FSC), we investigated the glass transition and crystal melting of samples of B. mori silk fibroin containing Silk I and/or Silk II crystals. Due to the very short residence times at high temperatures during such measurements, thermal decomposition of silk protein can be significantly suppressed. FSC was performed at 2000K/s using the Mettler Flash DSC1 on fibroin films with masses around 130-270ng. Films were prepared with different crystalline fractions (ranging from 0.26 to 0.50) and with different crystal structures (Silk I, Silk II, or mixed) by varying the processing conditions. These included water annealing at different temperatures, exposure to 50%MeOH in water, or autoclaving. The resulting crystal structure was examined using wide angle X-ray scattering. Degree of crystallinity was evaluated from Fourier transform infrared (FTIR) spectroscopy and from analysis of the heat capacity increment at the glass transition temperature. Silk fibroin films prepared by water annealing at 25°C were the least crystalline and had Silk I structure. FTIR and FSC studies showed that films prepared by autoclaving or 50%MeOH exposure were the most crystalline and had Silk II structure. Intermediate crystalline fraction and mixed Silk I/Silk II structures were found in films prepared by water annealing at 37°C. FSC results indicate that Silk II crystals exhibit endotherms of narrower width and have higher mean melting temperature T m (II)=351±2.6°C, compared to Silk I crystals which melt at T m (I)=292±3.8°C. Films containing mixed Silk I/Silk II structure showed two clearly separated endothermic peaks. Evidence suggests that the two types of crystals melt separately and do not thermally interconvert on the extremely short time scale (0.065s between onset and end of melting) of the FSC experiment. Silkworm silk is a naturally occurring biomaterial. The fibroin component of silk forms two types of crystals. Silk properties depend upon the

  4. A custom floating point format ADC for LHC calorimetry

    International Nuclear Information System (INIS)

    Hermel, V.; Lecoq, J.; Bohner, G.

    1996-01-01

    Due to their large dynamic range (in excess of 16 bits) signals from LHC calorimetry poses severe problems to the shaping and digitizing circuits. We are investigating a solution for an ADC based on a custom floating point format. Since the calorimeter precision is limited, the full dynamic range can be split into 8 positive sub-ranges and 5 negative ones, each with an 8 bits dynamic. The reduced number of bits (8 for the mantissa, 4 for the exponent and 1 for the sign) translates itself into a reduction of the power consumption both of the ADC and of the following digital filtering stages. (authors)

  5. Applications of modulated differential scanning calorimetry in preformulation studies.

    Science.gov (United States)

    Rabel, S R; Jona, J A; Maurin, M B

    1999-11-01

    Characterization of the thermal properties of active pharmaceutical ingredients is critical in the selection of appropriate physical forms for development and defining proper manufacturing, handling and storage conditions of those chemical entities. Modulated differential scanning calorimetry (MDSC) has proven to be an effective tool in the thorough characterization of thermal behavior of compounds in preformulation studies. Selected applications of MDSC for various preclinical compounds are presented, thereby demonstrating the utility of this analytical method in the determination of glass transitions, characterization of desolvation and degradation processes as well as in the study of polymorphic transformations and crystallizations.

  6. Successful management of a difficult cancer pain patient by appropriate adjuvant and morphine titration

    Directory of Open Access Journals (Sweden)

    Shiv PS Rana

    2011-01-01

    Full Text Available Morphine has been used for many years to relieve cancer pain. Oral morphine (in either immediate release or modified release form remains the analgesic of choice for moderate or severe cancer pain. The dose of oral morphine is titrated up to achieve adequate relief from pain with minimal side effects. Antidepressant and anticonvulsant drugs, when used in addition to conventional analgesics, give excellent relief from cancer pain. Most cancer pain responds to pharmacological measures with oral morphine but some pain like neuropathic and bony pain, pain in children and elderly age group, and advanced malignancy pain are very difficult to treat. Here, we report the management of a similar patient of severe cancer pain and the difficulty that we came across during dose titration of oral morphine and adjuvant analgesic.

  7. Effect of a stirring process in an isothermal titration microcalorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Socorro, F.; Nuez, I. de la; Alvarez, L.; Rodriguez de Rivera, M

    2004-10-01

    In this paper, it is analysed the way in which the thermodynamic results obtained in an isothermal titration microcalorimeter, with continuous injection of a liquid and a variable mass are affected. Two aspects are presented, the first one refers to a variation in the baseline that takes place when the liquid mass is increased in the laboratory cell, this variation is due to the change in the thermal coupling between the stirrer and its contact with the thermostat. The second aspect is the analysis of the effect of the stirring process and the injection velocity on the homogenization of the remaining mixture in the laboratory cell. The aim of the study of these two previous aspects is to increase the accuracy of the thermodynamic measures carried out. The variation of the baseline affects in a percentage from 1 to 2% of the total energy developed. It is also shown the necessity of a stirring process according to the injection velocity in order to obtain a homogeneous mixture at every instant. This fact allows to carry out a deconvolution of the calorimetric signal and to obtain directly the power developed in the mixture process in terms of the amount of mixed substance [Meas. Sci. Technol. 1 (1990) pp. 1285-1290; J. Thermal Analysis 41 (1994) pp. 1385-1392].

  8. Rapid clozapine titration in treatment-refractory bipolar disorder.

    Science.gov (United States)

    Ifteni, Petru; Correll, Christoph U; Nielsen, Jimmi; Burtea, Victoria; Kane, John M; Manu, Peter

    2014-09-01

    Clozapine is effective in treatment-refractory bipolar disorder (BD). Guidelines recommend slow titration to prevent seizures, hypotension and myocarditis, but this stance is not supported by comparative data. To evaluate the safety and effectiveness of rapid clozapine titration in BD. Analysis of a consecutive cohort of treatment-refractory BD patients with mixed/manic episode admitted on alternate days to one of two units of a psychiatric hospital. On one unit, clozapine was started at 25mg followed by 25-50mg as needed every 6h (maximum=100mg/day) on day 1, followed by increases of 25-100mg/day. On the other unit, clozapine was initiated with 25mg in day 1, followed by increases of 25-50mg/day. The primary outcome was the number of days from starting clozapine until readiness for discharge, adjusted in logistic regression for the number of antipsychotics tried during the hospitalization, psychotropic co-treatments and presence of psychotic features. Patients subject to rapid (N=44) and standard (N=23) titration were similar in age, gender, smoking status, body mass index, illness severity at baseline and discharge, and highest clozapine dose. Clozapine was discontinued due to hypotension (N=1) and pneumonia (N=1) during rapid titration, and for excessive sedation (N=1) in each titration group. The number of hospital days from starting clozapine until readiness for discharge was 3.8 days shorter in the rapid titration group (12.7±6.3 vs. 16.5±5.8, p=0.0077). Rapid clozapine titration appeared safe and effective for treatment-refractory BD. The potential for shorter hospital stays justifies prospective trials of this method. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. High-precision gravimetric coulometry using the silver-perchloric acid coulometer: Titration of arsenious oxide with electrogenerated iodine.

    Science.gov (United States)

    Newton, C M

    1977-06-01

    High-precision gravimetric coulometry with a silver-perchloric acid coulometer is evaluated as an alternative to the conventional titrimetric method. The loss of weight (caused by electrolytic dissolution) of a highly pure silver anode in series with the cathode of a conventional constant-current titration system is measured and related to the number of equivalents of substance titrated. The precision of the method is determined by titrations of the Standard Reference Material 83C arsenious oxide (99.99% pure) with electrogenerated iodine, using biamperometric end-point detection. Depending on the size of the sample, an ultimate precision of 25 ppm is obtained. The assay for 0.5-g samples of the SRM material is 99.993(9) +/- 0.002(5)% purity.

  10. Control of OSA during automatic positive airway pressure titration in a clinical case series: predictors and accuracy of device download data.

    Science.gov (United States)

    Huang, Hsin-Chia Carol; Hillman, David R; McArdle, Nigel

    2012-09-01

    To investigate the factors associated with physiologic control of obstructive sleep apnea (OSA) during automatic positive airway pressure (APAP) titration in a clinical series. To also assess the usefulness of apnea-hypopnea index (AHI) data downloaded from the APAP device (Dev AHI). Retrospective review of a consecutive series of patients with OSA who underwent APAP titration (Autoset Spirit, ResMed, Bella Vista, New South Wales, Australia ) with simultaneous polysomnographic (PSG) monitoring in the sleep laboratory. Tertiary sleep clinic. There were 190 consecutive patients with OSA referred for APAP titration. There were 58% of patients who achieved optimal or good control of OSA (titration PSG AHI titration. The independent predictors of titration PSG AHI were a history of cardiac disease and elevated central apnea and arousal indices during the diagnostic study. Although the median and interquartile range (IQR) AHI from the device (7.0, 3.9-11.6 events/hr) was only slightly less than the PSG AHI (7.8, 3.9-14.4 events/hr, P = 0.04) during titration, case-by-case agreement between the two measures was poor (chi-square titration is often poor, and close clinical follow-up is particularly needed in patients with a history of cardiac disease or with high arousal or central apnea indices on the diagnostic study. Device AHI does not reliably assess control during APAP titration, and PSG assessment may be required if clinical response to treatment is poor. The findings relate to the ResMed AutoSet device and may not apply to other devices.

  11. Dissecting electrostatic interactions in Bacillus circulans xylanase through NMR-monitored pH titrations

    Energy Technology Data Exchange (ETDEWEB)

    McIntosh, Lawrence P., E-mail: mcintosh@chem.ubc.ca; Naito, Daigo; Baturin, Simon J.; Okon, Mark; Joshi, Manish D. [University of British Columbia, Department of Biochemistry and Molecular Biology, Department of Chemistry, and Michael Smith Laboratories, Life Sciences Centre (Canada); Nielsen, Jens E. [University College Dublin, School of Biomolecular and Biomedical Science, Centre for Synthesis and Chemical Biology, UCD Conway Institute (Ireland)

    2011-09-15

    NMR-monitored pH titration curves of proteins provide a rich source of structural and electrostatic information. Although relatively straightforward to measure, interpreting pH-dependent chemical shift changes to obtain site-specific acid dissociation constants (pK{sub A} values) is challenging. In order to analyze the biphasic titrations exhibited by the side chain {sup 13}C{sup {gamma}} nuclei of the nucleophilic Glu78 and general acid/base Glu172 in Bacillus circulans xylanase, we have revisited the formalism for the ionization equilibria of two coupled acidic residues. In general, fitting NMR-monitored pH titration curves for such a system will only yield the two macroscopic pK{sub A} values that reflect the combined effects of both deprotonation reactions. However, through the use of mutations complemented with ionic strength-dependent measurements, we are able to extract the four microscopic pK{sub Ai} values governing the branched acid/base equilibria of Glu78 and Glu172 in BcX. These data, confirmed through theoretical calculations, help explain the pH-dependent mechanism of this model GH11 xylanase by demonstrating that the kinetically determined pK{sub A} values and hence catalytic roles of these two residues result from their electrostatic coupling.

  12. Dissecting electrostatic interactions in Bacillus circulans xylanase through NMR-monitored pH titrations

    International Nuclear Information System (INIS)

    McIntosh, Lawrence P.; Naito, Daigo; Baturin, Simon J.; Okon, Mark; Joshi, Manish D.; Nielsen, Jens E.

    2011-01-01

    NMR-monitored pH titration curves of proteins provide a rich source of structural and electrostatic information. Although relatively straightforward to measure, interpreting pH-dependent chemical shift changes to obtain site-specific acid dissociation constants (pK A values) is challenging. In order to analyze the biphasic titrations exhibited by the side chain 13 C γ nuclei of the nucleophilic Glu78 and general acid/base Glu172 in Bacillus circulans xylanase, we have revisited the formalism for the ionization equilibria of two coupled acidic residues. In general, fitting NMR-monitored pH titration curves for such a system will only yield the two macroscopic pK A values that reflect the combined effects of both deprotonation reactions. However, through the use of mutations complemented with ionic strength-dependent measurements, we are able to extract the four microscopic pK Ai values governing the branched acid/base equilibria of Glu78 and Glu172 in BcX. These data, confirmed through theoretical calculations, help explain the pH-dependent mechanism of this model GH11 xylanase by demonstrating that the kinetically determined pK A values and hence catalytic roles of these two residues result from their electrostatic coupling.

  13. Automated spectrophotometric bicarbonate analysis in duodenal juice compared to the back titration method.

    Science.gov (United States)

    Erchinger, Friedemann; Engjom, Trond; Gudbrandsen, Oddrun Anita; Tjora, Erling; Gilja, Odd H; Dimcevski, Georg

    2016-01-01

    We have recently evaluated a short endoscopic secretin test for exocrine pancreatic function. Bicarbonate concentration in duodenal juice is an important parameter in this test. Measurement of bicarbonate by back titration as the gold standard method is time consuming, expensive and technically difficult, thus a simplified method is warranted. We aimed to evaluate an automated spectrophotometric method in samples spanning the effective range of bicarbonate concentrations in duodenal juice. We also evaluated if freezing of samples before analyses would affect its results. Patients routinely examined with short endoscopic secretin test suspected to have decreased pancreatic function of various reasons were included. Bicarbonate in duodenal juice was quantified by back titration and automatic spectrophotometry. Both fresh and thawed samples were analysed spectrophotometrically. 177 samples from 71 patients were analysed. Correlation coefficient of all measurements was r = 0.98 (p titration gold standard. This is a major simplification of direct pancreas function testing, and allows a wider distribution of bicarbonate testing in duodenal juice. Extreme values for Bicarbonate concentration achieved by the autoanalyser method have to be interpreted with caution. Copyright © 2016 IAP and EPC. Published by Elsevier India Pvt Ltd. All rights reserved.

  14. Evaluation of aluminosilicate glass sintering during differential scanning calorimetry

    International Nuclear Information System (INIS)

    Souza, Juliana Pereira de

    2015-01-01

    In this work a difference in the baseline in differential scanning calorimetry analyses, observed in a work where aluminosilicate glasses microspheres containing Ho were studied for application in selective internal radiotherapy as hepatocellular carcinoma treatment, was studied. The glasses with nominal composition 53,7 SiO 2 .10,5 Al 2 O 3 . 35,8 MgO in %mol were produced from traditional melting. The first obtained were milled and sieved in the range of 45 a 63 μm. The material was used to produce glass microspheres by the gravitational fall method. The glass powder and the microspheres were characterized by X ray fluorescence spectrometry, laser diffraction, X ray diffraction, differential scanning calorimetry, differential thermal analysis, thermogravimetry, mass spectrometry, and scanning electron microscopy. After the thermal analyses, pellets were formed in the crucibles and were analyzed by scanning electron microscopy, X ray diffraction, and He pycnometry. The difference in the baseline was associated to the viscous flow sintering process and happens because of the decrease in the detected heat flow due to the sample shrinkage. Other events as concurrent crystallization with the sintering process were also studied. (author)

  15. Impact of Uniform Methods on Interlaboratory Antibody Titration Variability: Antibody Titration and Uniform Methods.

    Science.gov (United States)

    Bachegowda, Lohith S; Cheng, Yan H; Long, Thomas; Shaz, Beth H

    2017-01-01

    -Substantial variability between different antibody titration methods prompted development and introduction of uniform methods in 2008. -To determine whether uniform methods consistently decrease interlaboratory variation in proficiency testing. -Proficiency testing data for antibody titration between 2009 and 2013 were obtained from the College of American Pathologists. Each laboratory was supplied plasma and red cells to determine anti-A and anti-D antibody titers by their standard method: gel or tube by uniform or other methods at different testing phases (immediate spin and/or room temperature [anti-A], and/or anti-human globulin [AHG: anti-A and anti-D]) with different additives. Interlaboratory variations were compared by analyzing the distribution of titer results by method and phase. -A median of 574 and 1100 responses were reported for anti-A and anti-D antibody titers, respectively, during a 5-year period. The 3 most frequent (median) methods performed for anti-A antibody were uniform tube room temperature (147.5; range, 119-159), uniform tube AHG (143.5; range, 134-150), and other tube AHG (97; range, 82-116); for anti-D antibody, the methods were other tube (451; range, 431-465), uniform tube (404; range, 382-462), and uniform gel (137; range, 121-153). Of the larger reported methods, uniform gel AHG phase for anti-A and anti-D antibodies had the most participants with the same result (mode). For anti-A antibody, 0 of 8 (uniform versus other tube room temperature) and 1 of 8 (uniform versus other tube AHG), and for anti-D antibody, 0 of 8 (uniform versus other tube) and 0 of 8 (uniform versus other gel) proficiency tests showed significant titer variability reduction. -Uniform methods harmonize laboratory techniques but rarely reduce interlaboratory titer variance in comparison with other methods.

  16. [Titration comparative study of TOPINA Tablets in patients with localization related epilepsy: double-blind comparative study by rapid and slow titration methods].

    Science.gov (United States)

    Kaneko, Sunao; Inoue, Yushi; Sasagawa, Mutsuo; Kato, Masaaki

    2012-04-01

    To compare the tolerability and efficacy of two titration methods (rapid and slow titration) for TOPINA Tablets with different dosages and periods of escalation, a double-blind comparative study was conducted in patients with localization-related epilepsy. A total of 183 patients were randomized to either rapid titration (initial dosage 100 mg/day increased by 100-200 mg at weekly intervals) or to slow titration (initial dosage 50 mg/day increased in 50 mg/day increments at weekly intervals). TOPINA Tablets were administered for 12 weeks to the maximum dosage of 400 mg/day. The incident of adverse events leading to treatment interruptions or withdrawals was 18.9% in rapid titration and 14.8% in slow titration, with no statistical significance (p = 0.554). The incident of adverse events and adverse reactions of slow titration was slightly lower than that of rapid titration. The common adverse events and adverse reactions reported in the two titration methods were comparable and were well tolerated. On the other hand, the efficacy of slow titration, percent reduction in seizure rate and responder rate, was comparable with that of rapid titration. In conclusion, there were no significant differences of therapeutic response to TOPINA Tablets between the two titration methods.

  17. Potentiometric titration and equivalent weight of humic acid

    Science.gov (United States)

    Pommer, A.M.; Breger, I.A.

    1960-01-01

    The "acid nature" of humic acid has been controversial for many years. Some investigators claim that humic acid is a true weak acid, while others feel that its behaviour during potentiometric titration can be accounted for by colloidal adsorption of hydrogen ions. The acid character of humic acid has been reinvestigated using newly-derived relationships for the titration of weak acids with strong base. Re-interpreting the potentiometric titration data published by Thiele and Kettner in 1953, it was found that Merck humic acid behaves as a weak polyelectrolytic acid having an equivalent weight of 150, a pKa of 6.8 to 7.0, and a titration exponent of about 4.8. Interdretation of similar data pertaining to the titration of phenol-formaldehyde and pyrogallol-formaldehyde resins, considered to be analogs for humic acid by Thiele and Kettner, leads to the conclusion that it is not possible to differentiate between adsorption and acid-base reaction for these substances. ?? 1960.

  18. An interaction of the functionalized closo-borates with albumins: The protein fluorescence quenching and calorimetry study

    International Nuclear Information System (INIS)

    Losytskyy, Mykhaylo Yu.; Kovalska, Vladyslava B.; Varzatskii, Oleg A.; Kuperman, Marina V.; Potocki, Slawomir; Gumienna-Kontecka, Elzbieta; Zhdanov, Andrey P.; Yarmoluk, Sergiy M.; Voloshin, Yan Z.; Zhizhin, Konstantin Yu.; Kuznetsov, Nikolai T.; Elskaya, Anna V.

    2016-01-01

    An interaction of the boron clusters closo-borates K 2 [B 10 H 10 ], K 2 [B 12 H 12 ] and their functionalized derivatives with serum proteins human (HSA) and bovine (BSA) albumins and immonoglobulin IgG as well as globular proteins β-lactoglobulin and lysozyme was characterized. The steady state and time resolved protein fluorescence quenching studies point on the binding of the closo-borate arylamine derivatives to serum albumins and discrimination of other proteins. The mechanism of the albumin fluorescence quenching by the closo-borate arylamine derivatives was proposed. The complex formation between albumin and the closo-borate molecules has been confirmed by isothermal titration calorimetry (ITC). The compound (K 2 [B 10 H 10 ]) and its arylamine derivative both interact with HSA, have close values of K a (1.4 and 1.2×10 3 M −1 respectively) and Gibbs energy (−17.9 and −17.5 kJ/mol respectively). However, the arylamine derivative forms complex with the higher guest/host binding ratio (4:1) comparing to the parent closo-borate (2:1). - Highlights: • Complex formation between boron clusters closo-borates and albumins was confirmed. • Functional substituent of closo-borate strongly affects its complex with albumins. • Binding of arylamine closo-borates essentially quench the albumin fluorescence. • Mechanism of tryptophan emission quenching by arylamine closo-borates was proposed.

  19. Reference method for total water in lint cotton by automated oven drying combined with volumetric Karl Fischer titration

    Science.gov (United States)

    In a preliminary study to measure total water in lint cotton we demonstrated that volumetric Karl Fischer Titration of moisture transported by a carrier gas from an attached small oven is more accurate than standard oven drying in air. The objective of the present study was to assess the measuremen...

  20. Automated Methods Of Corrosion Measurements

    DEFF Research Database (Denmark)

    Bech-Nielsen, Gregers; Andersen, Jens Enevold Thaulov; Reeve, John Ch

    1997-01-01

    The chapter describes the following automated measurements: Corrosion Measurements by Titration, Imaging Corrosion by Scanning Probe Microscopy, Critical Pitting Temperature and Application of the Electrochemical Hydrogen Permeation Cell.......The chapter describes the following automated measurements: Corrosion Measurements by Titration, Imaging Corrosion by Scanning Probe Microscopy, Critical Pitting Temperature and Application of the Electrochemical Hydrogen Permeation Cell....

  1. Detectors for Linear Colliders: Calorimetry at a Future Electron-Positron Collider (3/4)

    CERN Multimedia

    CERN. Geneva

    2010-01-01

    Calorimetry will play a central role in determining the physics reach at a future e+e- collider. The requirements for calorimetry place the emphasis on achieving an excellent jet energy resolution. The currently favoured option for calorimetry at a future e+e- collider is the concept of high granularity particle flow calorimetry. Here granularity and a high pattern recognition capability is more important than the single particle calorimetric response. In this lecture I will describe the recent progress in understanding the reach of high granularity particle flow calorimetry and the related R&D efforts which concentrate on test beam demonstrations of the technological options for highly granular calorimeters. I will also discuss alternatives to particle flow, for example the technique of dual readout calorimetry.

  2. Study of phase changing characteristics of granular composites using differential scanning calorimetry

    International Nuclear Information System (INIS)

    Rady, Mohamed

    2009-01-01

    Characterization of the phase changing behavior of granular materials is an important issue for design and optimization of latent heat thermal energy storage (LHTES) systems. In the present work, differential scanning calorimetry (DSC) has been used to study the phase changing behavior of granular composites consisting of ceramic encapsulated phase change material (EPCM) with particle diameters of 1-3 mm. The obtained DSC curves characterizing melting and solidification of the composite material are shown to be dependent upon the values of heating and cooling rates. Direct utilization of the measured DSC curves could result in an inexact representation of the sample enthalpy change. A simple procedure has been advised to obtain accurate quantitative results from the DSC measurements based on the estimation of the thermal resistance between the sample and its enclosure. Analysis of the evolution of latent heat of EPCM with temperature at different values of cooling/heating rates is presented.

  3. Acid-base titration of melanocortin peptides: evidence of Trp rotational conformers interconversion.

    Science.gov (United States)

    Fernandez, Roberto M; Vieira, Renata F F; Nakaie, Clóvis R; Lamy, M Teresa; Ito, Amando S

    2005-01-01

    Tryptophantime-resolved fluorescence was used to monitor acid-base titration properties of alpha-melanocyte stimulating hormone (alpha-MSH) and the biologically more potent analog [Nle4, D-Phe7]alpha -MSH (NDP-MSH), labeled or not with the paramagnetic amino acid probe 2,2,6,6-tetramthylpiperidine-N-oxyl-4-amino-4-carboxylic acid (Toac). Global analysis of fluorescence decay profiles measured in the pH range between 2.0 and 11.0 showed that, for each peptide, the data could be well fitted to three lifetimes whose values remained constant. The less populated short lifetime component changed little with pH and was ascribed to Trp g+ chi1 rotamer, in which electron transfer deactivation predominates over fluorescence. The long and intermediate lifetime preexponential factors interconverted along that pH interval and the result was interpreted as due to interconversion between Trp g- and trans chi1 rotamers, driven by conformational changes promoted by modifications in the ionization state of side-chain residues. The differences in the extent of interconversion in alpha-MSH and NDP-MSH are indicative of structural differences between the peptides, while titration curves suggest structural similarities between each peptide and its Toac-labeled species, in aqueous solution. Though less sensitive than fluorescence, the Toac electron spin resonance (ESR) isotropic hyperfine splitting parameter can also monitor the titration of side-chain residues located relatively far from the probe. Copyright (c) 2005 Wiley Periodicals, Inc.

  4. Automated sample-processing and titration system for determining uranium in nuclear materials

    International Nuclear Information System (INIS)

    Harrar, J.E.; Boyle, W.G.; Breshears, J.D.; Pomernacki, C.L.; Brand, H.R.; Kray, A.M.; Sherry, R.J.; Pastrone, J.A.

    1977-01-01

    The system is designed for accurate, precise, and selective determination of from 10 to 180 mg of uranium in 2 to 12 cm 3 of solution. Samples, standards, and their solutions are handled on a weight basis. These weights, together with their appropriate identification numbers, are stored in computer memory and are used automatically in the assay calculations after each titration. The measurement technique (controlled-current coulometry) is based on the Davies-Gray and New Brunswick Laboratory method, in which U(VI) is reduced to U(IV) in strong H 3 PO 4 , followed by titration of the U(IV) with electrogenerated V(V). Solution pretreatment and titration are automatic. The analyzer is able to process 44 samples per loading of the sample changer, at a rate of 4 to 9 samples per hour. The system includes a comprehensive fault-monitoring system that detects analytical errors, guards against abnormal conditions which might cause errors, and prevents unsafe operation. A detailed description of the system, information on the reliability of the component subsystems, and a summary of its evaluation by the New Brunswick Laboratory are presented

  5. Quantitative RT-PCR for titration of replication-defective recombinant Semliki Forest virus.

    Science.gov (United States)

    Puglia, Ana L P; Rezende, Alexandre G; Jorge, Soraia A C; Wagner, Renaud; Pereira, Carlos A; Astray, Renato M

    2013-11-01

    Virus titration may constitute a drawback in the development and use of replication-defective viral vectors like Semliki Forest virus (SFV). The standardization and validation of a reverse transcription quantitative PCR (qRT-PCR) method for SFV titration is presented here. The qRT-PCR target is located within the nsp1 gene of the non-structural polyprotein SFV region (SFV RNA), which allows the strategy to be used for several different recombinant SFV constructs. Titer determinations were carried out by performing virus titration and infection assays with SFVs containing an RNA coding region for the rabies virus glycoprotein (RVGP) or green fluorescent protein (GFP). Results showed that the standardized qRT-PCR is applicable for different SFV constructs, and showed good reproducibility. To evaluate the correlation between the amount of functional SFV RNA in a virus lot and its infectivity in BHK-21 cell cultures, a temperature mediated titer decrease was performed and successfully quantitated by qRT-PCR. When used for cell infection at the same multiplicity of infection (MOI), the temperature treated SFV-RVGP samples induced the same levels of RVGP expression. Similarly, when different SFV-GFP lots with different virus titers, as accessed by qRT-PCR, were used for cell infection at the same MOI, the cultures showed comparable amounts of fluorescent cells. The data demonstrate a good correlation between the amount of virus used for infection, as measured by its SFV RNA, and the protein synthesis in the cells. In conclusion, the qRT-PCR method developed here is accurate and enables the titration of replication-defective SFV vectors, an essential aid for viral vector development as well as for establishment of production bioprocesses. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Determination of uranium by direct titration with dipicolinic acid

    International Nuclear Information System (INIS)

    Baumann, E.W.

    1984-01-01

    Direct titration of uranium with dipicolinic acid, in the presence of Arsenazo I, is a simple, precise, and accurate method for uranium determination. The method is particularly attractive because it can be totally automated. Detecting the end point (color change from blue to pink) depends on the concentration range. For the Micro Method (1 to 20 ppM U in the solution titrated), the gradual color change is monitored spectrophotometrically. For the Macro Method (20 to 300 ppM), the end point is determined either visually or spectrophotometrically. The spectrophotometric end point is computed by fitting the titration curve. The relative standard deviation is +-1 to 3% for the Micro Method and +-0.3% for the Macro Method

  7. Coulometric titration of D(+)-glucose using its enzymatic oxidation.

    Science.gov (United States)

    Tanaka, T; Shutto, E; Mizoguchi, T; Fukushima, K

    2001-02-01

    A definitive method is described for the indirect assay of milligram quantities of D(+)-glucose by coulometric titration. D(+)-Glucose was aerobically oxidized by glucose oxidase in an acetate buffer solution (pH 5.1). Subsequently, the enzymatically formed hydrogen peroxide was titrated coulometrically with electrogenerated hypobromite in sodium bromide-sodium tetraborate medium of pH 8.6, with biamperometric end-point detection. Parameters affecting the enzymatically catalyzed oxidation and coulometric titration were evaluated. The optimized conditions for the oxidation of up to 20 mg of D(+)-glucose include the addition of 4500 U of glucose oxidase and stirring over a 10-min interval at 25 degrees C. Under proposed conditions, the assay values of several commercial D(+)-glucose reagents were somewhat lower than the guaranteed minimum values, with RSDs (n = 5) of 0.071 - 0.106%.

  8. Determination of tungsten by amperometric redox titration with dichromate

    Energy Technology Data Exchange (ETDEWEB)

    Wuensch, G.; Aupers, R.; Kranich, R.

    1985-11-01

    Tungsten is reduced by an excess of Cr(II) in about 10 M HCl. This is technically simpler than the use of reductor columns or liquid amalgams. Titration with Fe(III) or Cr(VI) first consumes the excess of Cr(II) and then oxidizes W(V) to W(VI). The potentiometric response of metal electrodes to W(V) is slow but biamperometric indication at Esub(pol) = 0.2 V applies well. A mixture of W, Fe and Mo can be analyzed in a consecutive titration. Only Ti interferes. As compared to the reductometric titration of W(VI) with Cr(II) the method uses a stable titrant and avoids deairating of the sample solution. Sample preparations for ferrotungsten, steel and wolframite ore are described. (orig.).

  9. Improved methylene blue two-phase titration method for determining cationic surfactant concentration in high-salinity brine.

    Science.gov (United States)

    Cui, Leyu; Puerto, Maura; López-Salinas, José L; Biswal, Sibani L; Hirasaki, George J

    2014-11-18

    The methylene blue (MB) two-phase titration method is a rapid and efficient method for determining the concentrations of anionic surfactants. The point at which the aqueous and chloroform phases appear equally blue is called Epton's end point. However, many inorganic anions, e.g., Cl(-), NO3(-), Br(-), and I(-), can form ion pairs with MB(+) and interfere with Epton's end point, resulting in the failure of the MB two-phase titration in high-salinity brine. Here we present a method to extend the MB two-phase titration method for determining the concentration of various cationic surfactants in both deionized water and high-salinity brine (22% total dissolved solid). A colorless end point, at which the blue color is completely transferred from the aqueous phase to the chloroform phase, is proposed as titration end point. Light absorbance at the characteristic wavelength of MB is measured using a spectrophotometer. When the absorbance falls below a threshold value of 0.04, the aqueous phase is considered colorless, indicating that the end point has been reached. By using this improved method, the overall error for the titration of a permanent cationic surfactant, e.g., dodecyltrimethylammonium bromide, in deionized (DI) water and high-salinity brine is 1.274% and 1.322% with limits of detection (LOD) of 0.149 and 0.215 mM, respectively. Compared to the traditional acid-base titration method, the error of this improved method for a switchable cationic surfactant, e.g., tertiary amine surfactant (Ethomeen C12), is 2.22% in DI water and 0.106% with LOD of 0.369 and 0.439 mM, respectively.

  10. Error assessment in recombinant baculovirus titration: evaluation of different methods.

    Science.gov (United States)

    Roldão, António; Oliveira, Rui; Carrondo, Manuel J T; Alves, Paula M

    2009-07-01

    The success of baculovirus/insect cells system in heterologous protein expression depends on the robustness and efficiency of the production workflow. It is essential that process parameters are controlled and include as little variability as possible. The multiplicity of infection (MOI) is the most critical factor since irreproducible MOIs caused by inaccurate estimation of viral titers hinder batch consistency and process optimization. This lack of accuracy is related to intrinsic characteristics of the method such as the inability to distinguish between infectious and non-infectious baculovirus. In this study, several methods for baculovirus titration were compared. The most critical issues identified were the incubation time and cell concentration at the time of infection. These variables influence strongly the accuracy of titers and must be defined for optimal performance of the titration method. Although the standard errors of the methods varied significantly (7-36%), titers were within the same order of magnitude; thus, viral titers can be considered independent of the method of titration. A cost analysis of the baculovirus titration methods used in this study showed that the alamarblue, real time Q-PCR and plaque assays were the most expensive techniques. The remaining methods cost on average 75% less than the former methods. Based on the cost, time and error analysis undertaken in this study, the end-point dilution assay, microculture tetrazolium assay and flow cytometric assay were found to be the techniques that combine all these three main factors better. Nevertheless, it is always recommended to confirm the accuracy of the titration either by comparison with a well characterized baculovirus reference stock or by titration using two different methods and verification of the variability of results.

  11. A titration method for determining individual oxidant concentration in the dual sodium persulfate and hydrogen peroxide oxidation system.

    Science.gov (United States)

    Liang, Chenju; He, Boyu

    2018-05-01

    The use of a dual oxidation system, which combines sodium persulfate (Na 2 S 2 O 8 , SPS) and hydrogen peroxide (H 2 O 2 , HP) is increasing as an in-situ chemical oxidation (ISCO) process for soil and groundwater remediation. An analytical method was assessed in this study for determining individual oxidant concentration in order to understand the interactions, and variations in the concentrations, of SPS and HP in aqueous systems containing both SPS and HP. The iodometric titration method was demonstrated to be capable of measuring total oxidant (SPS + HP) concentration; while the ceric sulfate titration method can be used specifically for measuring HP in the dual oxidation system without interfering with the iodometric titration. Therefore, SPS concentration can be deduced by subtraction of the HP concentration from the total oxidant concentration. Direct iodometric titration for determination of total oxidant at concentration above 20 mM exhibited <8% concentration. Based on the results of indirect determination of SPS in the dual oxidation system, an approximate 10% concentration variation was expected. This research may serve as a reference for measuring oxidant variations in this ISCO dual oxidant application. Copyright © 2018. Published by Elsevier Ltd.

  12. Experimental Techniques for Thermodynamic Measurements of Ceramics

    Science.gov (United States)

    Jacobson, Nathan S.; Putnam, Robert L.; Navrotsky, Alexandra

    1999-01-01

    Experimental techniques for thermodynamic measurements on ceramic materials are reviewed. For total molar quantities, calorimetry is used. Total enthalpies are determined with combustion calorimetry or solution calorimetry. Heat capacities and entropies are determined with drop calorimetry, differential thermal methods, and adiabatic calorimetry . Three major techniques for determining partial molar quantities are discussed. These are gas equilibration techniques, Knudsen cell methods, and electrochemical techniques. Throughout this report, issues unique to ceramics are emphasized. Ceramic materials encompass a wide range of stabilities and this must be considered. In general data at high temperatures is required and the need for inert container materials presents a particular challenge.

  13. Hadronic shower development in Iron-Scintillator Tile Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Amaral, P.; Amorim, A.; Anderson, K.; Barreira, G.; Benetta, R.; Berglund, S.; Biscarat, C.; Blanchot, G.; Blucher, E.; Bogush, A.; Bohm, C.; Boldea, V.; Borisov, O.; Bosman, M.; Bromberg, C.; Budagov, J.; Burdin, S.; Caloba, L.; Carvalho, J.; Casado, P.; Castillo, M.V.; Cavalli-Sforza, M.; Cavasinni, V.; Chadelas, R.; Chirikov-Zorin, I.; Chlachidze, G.; Cobal, M.; Cogswell, F.; Colaco, F.; Cologna, S.; Constantinescu, S.; Costanzo, D.; Crouau, M.; Daudon, F.; David, J.; David, M.; Davidek, T.; Dawson, J.; De, K.; Del Prete, T.; De Santo, A.; Di Girolamo, B.; Dita, S.; Dolejsi, J.; Dolezal, Z.; Downing, R.; Efthymiopoulos, I.; Engstroem, M.; Errede, D.; Errede, S.; Evans, H.; Fenyuk, A.; Ferrer, A.; Flaminio, V.; Gallas, E.; Gaspar, M.; Gil, I.; Gildemeister, O.; Glagolev, V.; Gomes, A.; Gonzalez, V.; Gonzalez De La Hoz, S.; Grabski, V.; Grauges, E.; Grenier, P.; Hakopian, H.; Haney, M.; Hansen, M.; Hellman, S.; Henriques, A.; Hebrard, C.; Higon, E.; Holmgren, S.; Huston, J.; Ivanyushenkov, Yu.; Jon-And, K.; Juste, A.; Kakurin, S.; Karapetian, G.; Karyukhin, A.; Kopikov, S.; Kukhtin, V.; Kulchitsky, Y.; Kurzbauer, W.; Kuzmin, M.; Lami, S.; Lapin, V.; Lazzeroni, C.; Lebedev, A.; Leitner, R.; Li, J.; Lomakin, Yu.; Lomakina, O.; Lokajicek, M.; Lopez Amengual, J.M.; Maio, A.; Malyukov, S.; Marroquin, F.; Martins, J.P.; Mazzoni, E.; Merritt, F.; Miller, R.; Minashvili, I.; Miralles, Ll.; Montarou, G.; Munar, A.; Nemecek, S.; Nessi, M. E-mail: marzio.nessi@cern.ch; Onofre, A.; Orteu, S.; Park, I.C.; Pallin, D.; Pantea, D.; Paoletti, R.; Patriarca, J.; Pereira, A.; Perlas, J.A.; Petit, P.; Pilcher, J.; Pinhao, J.; Poggioli, L.; Price, L.; Proudfoot, J.; Pukhov, O.; Reinmuth, G.; Renzoni, G.; Richards, R.; Roda, C.; Romance, J.B.; Romanov, V.; Ronceux, B.; Rosnet, P.; Rumyantsev, V.; Russakovich, N.; Sanchis, E.; Sanders, H.; Santoni, C.; Santos, J.; Sawyer, L.; Says, L.-P.; Seixas, J.M.; Sellden, B.; Semenov, A.; Shchelchkov, A.; Shochet, M.; Simaitis, V. [and others

    2000-03-21

    The lateral and longitudinal profiles of hadronic showers detected by a prototype of the ATLAS Iron-Scintillator Tile Hadron Calorimeter have been investigated. This calorimeter presents a unique longitudinal configuration of scintillator tiles. Using a fine-grained pion beam scan at 100 GeV, a detailed picture of transverse shower behaviour is obtained. The underlying radial energy densities for the four depth segments and for the entire calorimeter have been reconstructed. A three-dimensional hadronic shower parametrisation has been developed. The results presented here are useful for understanding the performance of iron-scintillator calorimeters, for developing fast simulations of hadronic showers, for many calorimetry problems requiring the integration of a shower energy deposition in a volume and for future calorimeters design.

  14. On the Interpretation of Low Temperature Calorimetry Data

    DEFF Research Database (Denmark)

    Kjeldsen, Ane Mette; Geiker, Mette Rica

    2008-01-01

    The effect of selected factors and phenomena on Low Temperature Calorimetry (LTC) results has been investigated, in order to determine the possibilities and limitations of using LTC for characterisation of the porosity of cement-based materials. LTC was carried out on a model material with mono......-sized pores of approximately 14 nm saturated with either distilled water or a sodium chloride solution, as well as on water, the salt solution, and an artificial pore solution, alone. It was found that supercooling is unavoidable during the liquid-solid phase transition, and that even at low temperature...... to limit transport of liquid, whereas heating should be undertaken at a low rate to limit the effect of non-equilibrium....

  15. Present status of CMS HF quartz fiber calorimetry

    CERN Document Server

    Önel, Y M

    2002-01-01

    The experiments at the Large Hadron Collider will have to deal with unprecedented radiation levels. The design of the CMS forward calorimetry detector (HF) is now finalized. The present design of CMS calls for the HF calorimeter to be based on quartz fiber technology. It consists of two modules, located symmetrically at about 11 meters from either side of interaction point. They cover the pseudorapidity range 3-5. The length along the beam is 1.65 m or 10 nuclear interaction lengths. Each calorimeter consists of a large steel block that serves as the absorber. Embedded quartz fibers in the steel absorber run parallel to the beam and constitute the active component of the detector. In order to optimize energy resolution for E and E /sup T/ flows and forward jets, the calorimeter is effectively segmented longitudinally by using two different fiber lengths. The present status will be discussed. (6 refs).

  16. Review of MEMS differential scanning calorimetry for biomolecular study

    Science.gov (United States)

    Yu, Shifeng; Wang, Shuyu; Lu, Ming; Zuo, Lei

    2017-12-01

    Differential scanning calorimetry (DSC) is one of the few techniques that allow direct determination of enthalpy values for binding reactions and conformational transitions in biomolecules. It provides the thermodynamics information of the biomolecules which consists of Gibbs free energy, enthalpy and entropy in a straightforward manner that enables deep understanding of the structure function relationship in biomolecules such as the folding/unfolding of protein and DNA, and ligand bindings. This review provides an up to date overview of the applications of DSC in biomolecular study such as the bovine serum albumin denaturation study, the relationship between the melting point of lysozyme and the scanning rate. We also introduce the recent advances of the development of micro-electro-mechanic-system (MEMS) based DSCs.

  17. Hadronic Shower Development in Iron-Scintillator Tile Calorimetry

    CERN Document Server

    Amaral, P; Anderson, K; Barreira, G; Benetta, R; Berglund, S; Biscarat, C; Blanchot, G; Blucher, E; Bogush, A A; Bohm, C; Boldea, V; Borisov, O; Bosman, M; Bromberg, C; Budagov, Yu A; Burdin, S; Caloba, L; Carvalho, J; Casado, M P; Castillo, M V; Cavalli-Sforza, M; Cavasinni, V; Chadelas, R; Chirikov-Zorin, I E; Chlachidze, G; Cobal, M; Cogswell, F; Colaço, F; Cologna, S; Constantinescu, S; Costanzo, D; Crouau, M; Daudon, F; David, J; David, M; Davidek, T; Dawson, J; De, K; Del Prete, T; De Santo, A; Di Girolamo, B; Dita, S; Dolejsi, J; Dolezal, Z; Downing, R; Efthymiopoulos, I; Engström, M; Errede, D; Errede, S; Evans, H; Fenyuk, A; Ferrer, A; Flaminio, V; Gallas, E; Gaspar, M; Gil, I; Gildemeister, O; Glagolev, V; Gomes, A; González, V; González de la Hoz, S; Grabskii, V; Graugès-Pous, E; Grenier, P; Hakopian, H H; Haney, M; Hansen, M; Hellman, S; Henriques, A; Hébrard, C; Higón, E; Holmgren, S O; Huston, J; Ivanyushenkov, Yu M; Jon-And, K; Juste, A; Kakurin, S; Karapetian, G V; Karyukhin, A N; Kopikov, S; Kukhtin, V; Kulchitskii, Yu A; Kurzbauer, W; Kuzmin, M; Lami, S; Lapin, V; Lazzeroni, C; Lebedev, A; Leitner, R; Li, J; Lomakin, Yu F; Lomakina, O V; Lokajícek, M; López-Amengual, J M; Maio, A; Malyukov, S; Marroquin, F; Martins, J P; Mazzoni, E; Merritt, F S; Miller, R; Minashvili, I A; Miralles, L; Montarou, G; Munar, A; Némécek, S; Nessi, Marzio; Onofre, A; Orteu, S; Park, I C; Pallin, D; Pantea, D; Paoletti, R; Patriarca, J; Pereira, A; Perlas, J A; Petit, P; Pilcher, J E; Pinhão, J; Poggioli, L; Price, L; Proudfoot, J; Pukhov, O; Reinmuth, G; Renzoni, G; Richards, R; Roda, C; Romance, J B; Romanov, V; Ronceux, B; Rosnet, P; Rumyantsev, V; Rusakovich, N; Sanchis, E; Sanders, H; Santoni, C; Santos, J; Sawyer, L; Says, L P; Seixas, J M; Selldén, B; Semenov, A; Shchelchkov, A S; Shochet, M; Simaitis, V; Sissakian, A N; Solodkov, A; Solovyanov, O; Sonderegger, P; Sosebee, M; Soustruznik, K; Spanó, F; Stanek, R; Starchenko, E A; Stephens, R; Suk, M; Tang, F; Tas, P; Thaler, J; Tokar, S; Topilin, N; Trka, Z; Turcot, A S; Turcotte, M; Valkár, S; Varandas, M J; Vartapetian, A H; Vazeille, F; Vichou, I; Vinogradov, V; Vorozhtsov, S B; Wagner, D; White, A; Wolters, H; Yamdagni, N; Yarygin, G; Yosef, C; Zaitsev, A; Zdrazil, M; Zúñiga, J

    2000-01-01

    The lateral and longitudinal profiles of hadronic showers detected by a prototype of the ATLAS Iron-Scintillator Tile Hadron Calorimeter have been investigated. This calorimeter uses a unique longitudinal configuration of scintillator tiles. Using a fine-grained pion beam scan at 100 GeV, a detailed picture of transverse shower behavior is obtained. The underlying radial energy densities for four depth segments and for the entire calorimeter have been reconstructed. A three-dimensional hadronic shower parametrization has been developed. The results presented here are useful for understanding the performance of iron-scintillator calorimeters, for developing fast simulations of hadronic showers, for many calorimetry problems requiring the integration of a shower energy deposition in a volume and for future calorimeter design.

  18. Determination of the thermodynamic properties of complexation and extraction by micro-calorimetry; Determination de grandeurs thermodynamiques de complexation et d'extraction d'ions lanthanide(3) par microcalorimetrie

    Energy Technology Data Exchange (ETDEWEB)

    Charbonnel, M.Ch.; Flandin, J.L. [CEA Valrho, (DCC/DRRV/SEMP), 30 - Marcoule (France)

    2000-07-01

    The CEA is currently developing the DIAMEX process, the first step in the strategy for the separation of minor actinides from high-level radioactive waste. The extractant belongs to the diamide family of molecules and is able to co-extract trivalent actinides and lanthanides. This study focuses on the thermodynamic properties ({delta}H, {delta}G, {delta}S) of lanthanide extraction by malonamide in order to better understand the mechanisms involved and to account for differences in the behavior of various diamide extractants. The main technique used is microcalorimetric titration. The Thermal Activity Monitor (TAM) microcalorimeter is a modular system with a highly stable ({+-} 0.1 mK) temperature-controlled bath containing up to four calorimetry vessel units. The sensor bulbs inserted in the reaction vessel can measure heat flows in static or dynamic conditions. Micro-calorimetry, and calorimetric titration in particular, is a fast growing field due to technical improvements in both hardware and software. In the case of an equilibrium reaction, titration allows both {delta}{sub r}G and {delta}{sub r}H (and thus {delta}{sub r}S) to be determined simultaneously. It was decided to initiate this thermochemical investigation with a homogeneous phase reaction, and the first study concerned the aqueous phase complexation of a trivalent lanthanide ion by a water-soluble diamide, tetraethyl-malonamide (TEMA: (C{sub 2}H{sub 5}){sub 2}NCO-CH{sub 2}CON(C{sub 2}H{sub 5}){sub 2}). In the test system, the heat of dilution of the diamide in water is preponderant over the heat arising from the complexation reaction; the result is a positive value corresponding to an endothermic reaction. However, the equilibration constant K and {delta} H are both very small, and cannot be calculated from the resulting Q{sub v}f(n{sub TEMA}) curves. Moreover, in aqueous phase, the reactions involved are different from those observed when neodymium(III) is extracted into an organic phase, and the

  19. Potentiometric and coulometric titration of 6-propyl-2-thiouracil.

    Science.gov (United States)

    Ciesielski, W; Zakrzewski, R

    1997-05-01

    A method for the determination of 6-propyl-2-thiouracil involving its reaction with iodine in an alkaline medium is presented. In volumetric titration with potentiometric end-point detection, the range of determination is 125-500 mumol (21-85 mg). In coulometric titration using biamperometric end-point detection, 0.5-5.0 mumol (0.085-0.85 mg) of 6-propyl-2-thiouracil was successfully determined. The RSD in all applied techniques was < 1%. The methods developed were applied to the determination of 6-propyl-2-thiouracil in tablets.

  20. The importance of calorimetry for highly-boosted jet substructure

    Energy Technology Data Exchange (ETDEWEB)

    Coleman, Evan [Brown U.; Freytsis, Marat [Oregon U.; Hinzmann, Andreas [Hamburg U.; Narain, Meenakshi [Brown U.; Thaler, Jesse [MIT, Cambridge, CTP; Tran, Nhan [Fermilab; Vernieri, Caterina [Fermilab

    2017-09-25

    Jet substructure techniques are playing an essential role in exploring the TeV scale at the Large Hadron Collider (LHC), since they facilitate the efficient reconstruction and identification of highly-boosted objects. Both for the LHC and for future colliders, there is a growing interest in using jet substructure methods based only on charged-particle information. The reason is that silicon-based tracking detectors offer excellent granularity and precise vertexing, which can improve the angular resolution on highly-collimated jets and mitigate the impact of pileup. In this paper, we assess how much jet substructure performance degrades by using track-only information, and we demonstrate physics contexts in which calorimetry is most beneficial. Specifically, we consider five different hadronic final states - W bosons, Z bosons, top quarks, light quarks, gluons - and test the pairwise discrimination power with a multi-variate combination of substructure observables. In the idealized case of perfect reconstruction, we quantify the loss in discrimination performance when using just charged particles compared to using all detected particles. We also consider the intermediate case of using charged particles plus photons, which provides valuable information about neutral pions. In the more realistic case of a segmented calorimeter, we assess the potential performance gains from improving calorimeter granularity and resolution, comparing a CMS-like detector to more ambitious future detector concepts. Broadly speaking, we find large performance gains from neutral-particle information and from improved calorimetry in cases where jet mass resolution drives the discrimination power, whereas the gains are more modest if an absolute mass scale calibration is not required.

  1. Construction and use of an optical semi-automatic titrator employing the technique of reflectance photometry

    International Nuclear Information System (INIS)

    Hwang, Hoon

    2001-01-01

    An optical semi-automatic titrator was constructed employing the technique of the reflectance spectrometry and was tested for the determination of the end points of the acid-base, precipitation, and EDTA titrations. And since the current optical semi-automatic titrator built on the principle of the reflectance spectrometry could be successfully used even for the determination of the end of the end point in the precipitation titration where the solid particles are formed during the titration process, it was found to be feasible that a completely automated optical titrator would be designed and built based on the current findings

  2. Titration of digoxin through radio-immunology in the solid phase

    International Nuclear Information System (INIS)

    Hersh, L.S.; Yaverbaum, Sidney.

    1975-01-01

    The invention relates to biological titrations. It refers to a method for determining the digoxin concentration in a solution, characterized in that it comprises the steps of: causing the solution (a known amount of labelled digoxin and a composite substance constituted by anti-digoxin antibodies chemically coupled through the medium of a silane coupling agent) to react with magnetically-sensitive inorganic particles, so as to generate immuno-chemical complex; magnetically separating the composite substance from the reaction solution; measuring the radioactivity of the thus separated composite substance or of the remaining solution; and comparing the measurements of step with a reference curve so as to determine the digoxin concentration [fr

  3. Analysis of the microbial growth in 60Co γ-irradiated foods by calorimetry

    International Nuclear Information System (INIS)

    Furuta, Masakazu; Hayashi, Toshio; Hamasaki, Koji; Wirkner, Sandra; Constantinoiu, Elena; Takahashi, Katsutada

    2002-01-01

    Using a heat conduction calorimeter equipped with 24 sample units the heat evolutions from growing 60 Co γ-irradiated bioburden of black pepper seeds and frozen beef were detected in the form of growth thermograms. 60 Co γ-irradiation affected the growth pattern in which a dose-dependent reduction of the growth rate constant was observed together with the retardation in growth, indicating a combination of bactericidal and bacteriostatic effects. We successfully determined the minimal inactivation doses for the two food samples using the relationship between the irradiation dose and the retardation in growth t α , or the growth rate constant μ obtained from the growth thermograms. These results strongly suggested the possibility of calorimetry as measure of predictive microbiology in food irradiation. (author)

  4. Analysis of the microbial growth in 60Co gamma-irradiated foods by calorimetry

    International Nuclear Information System (INIS)

    Furuta, M.; Hamasaki, K.; Wirkner, S.; Constantinoiu, E.; Takahashi, K.; Hayashi, T.

    2002-01-01

    Using a heat conduction calorimeter equipped with 24 sample units the heat evolutions from growing 60Co gamma-irradiated bioburden of black pepper seeds and frozen beef were detected in the form of growth thermograms. 60Co gamma-irradiation affected the growth pattern in which a dose-dependent reduction of the growth rate constant was observed together with the retardation in growth, indicating a combination of bactericidal and bacteriostatic effects. We successfully determined the minimal inactivation doses for the two food samples using the relationship between the irradiation dose and the retardation in growth talpha, or the growth rate constant mu obtained from the growth thermograms. These results strongly suggested the possibility of calorimetry as a measure of predictive microbiology in food irradiation

  5. Relaxation calorimetry at very low temperatures for systems with internal relaxation

    Science.gov (United States)

    Matsumoto, Yosuke; Nakatsuji, Satoru

    2018-03-01

    We present the detailed introduction of our relaxation calorimetry designed for tiny samples down to very low temperatures of 0.03 K. In particular, we discuss how to analyze the data that are modified by an internal thermal relaxation in the sample or in the sample stage of the specific heat cell. We demonstrate that the correct heat capacity is obtained even when the relaxation curve has a triple exponential decay, rather than a double exponential decay which has usually been discussed. As an example, we discuss the measurements performed for α-YbAlB4 in a magnetic field of 5 T, where we found the triple exponential decay due to a thermal relaxation between electron and nuclear contributions at relatively high temperature well above 0.1 K. Our modified analysis provides the best solution in such a case.

  6. DETERMINATION OF HYDROGEN DESORBED THROUGH THERMAL CALORIMETRY IN A HIGH STRENGTH STEEL

    Directory of Open Access Journals (Sweden)

    Carolina A. Asmus

    2014-03-01

    Full Text Available The following study aims to quantify the release activation energy (Ea of hydrogen (H from lattice sites, reversible or irreversible, where the H can be trapped. Moreover, enthalpy changes associated with the main hydrogen (H trapping sites can be analyzed by means of differential scanning calorimetry (DSC. In this technique, the peak temperature measurement is determined at two different heating rates, 3ºC/min y 5ºC/min, from ambient temperature to 500°C. In order to simulate severe conditions of hydrogen income into resulfurized high strength steel, electrolytic permeation tests were performed on test tubes suitable for fatigue tests. Sometimes during charging, H promoters were aggregated to electrolytic solution. Subsequently, the test tubes were subjected to flow cycle fatigue tests. Finally, irreversible trap which anchor more strongly H atoms are MnS inclusions. Its role on hydrogen embrittlement during fatigue tests is conclusive.

  7. Characterization of lipid nanoparticles by differential scanning calorimetry, X-ray and neutron scattering.

    Science.gov (United States)

    Bunjes, Heike; Unruh, Tobias

    2007-07-10

    Differential scanning calorimetry and X-ray diffraction play a prominent role in the characterization of lipid nanoparticle (LNP) dispersions. This review shortly outlines the measurement principles of these two techniques and summarizes their applications in the field of nanodispersions of solid lipids. These methods are particularly useful for the characterization of the matrix state, polymorphism and phase behavior of the nanoparticles which may be affected by, for example, the small particle size and the composition of the dispersions. The basics of small angle X-ray and neutron scattering which are also very promising methods for the characterization of LNPs are explained in some more detail. Examples for their use in the area of solid LNPs regarding the evaluation of particle size effects and the formation of superstructures in the nanoparticle dispersions are given. Some technical questions concerning the use of the different characterization techniques in the field of LNP research are also addressed.

  8. New methodology developed for the differential scanning calorimetry analysis of polymeric matrixes incorporating phase change materials

    International Nuclear Information System (INIS)

    Barreneche, Camila; Solé, Aran; Miró, Laia; Martorell, Ingrid; Cabeza, Luisa F; Fernández, A Inés

    2012-01-01

    Nowadays, thermal comfort needs in buildings have led to an increase in energy consumption of the residential and service sectors. For this reason, thermal energy storage is shown as an alternative to achieve reduction of this high consumption. Phase change materials (PCM) have been studied to store energy due to their high storage capacity. A polymeric material capable of macroencapsulating PCM was developed by the authors of this paper. However, difficulties were found while measuring the thermal properties of these materials by differential scanning calorimetry (DSC). The polymeric matrix interferes in the detection of PCM properties by DSC. To remove this interfering effect, a new methodology which replaces the conventional empty crucible used as a reference in the DSC analysis by crucibles composed of the polymeric matrix was developed. Thus, a clear signal from the PCM is obtained by subtracting the new full crucible signal from the sample signal. (paper)

  9. Energetics of methanol and formic acid oxidation on Pt(111): Mechanistic insights from adsorption calorimetry

    Science.gov (United States)

    Silbaugh, Trent L.; Karp, Eric M.; Campbell, Charles T.

    2016-08-01

    The catalytic and electrocatalytic oxidation and reforming of methanol and formic acid have received intense interest due to potential use in direct fuel cells and as prototype models for understanding electrocatalysis. Consequently, the reaction energy diagram (energies of all the adsorbed intermediates and activation energies of all the elementary steps) have been estimated for these reactions on Pt(111) by density functional theory (DFT) in several studies. However, no experimental measurement of these energy diagrams have been reported, nor is there a consensus on the mechanisms. Here, we use energies of key intermediates on Pt(111) from single crystal adsorption calorimetry (SCAC) and temperature programmed desorption (TPD) to build a combined energy diagram for these reactions. It suggests a new pathway involving monodentate formate as a key intermediate, with bidentate formate only being a spectator species that slows the rate. This helps reconcile conflicting proposed mechanisms.

  10. Calorimetry of the Pd-D2O system: from simplicity via complications to simplicity

    International Nuclear Information System (INIS)

    Fleischmann, M.; Pons, S.

    1993-01-01

    We present here one aspect of our recent research on the calorimetry of the Pd-D 2 O system which has been concerned with high rates of specific excess enthalpy generation (> 1 kW cm -3 ) at temperatures close to (or at) the boiling point of the elctrolyte solution. This has led to a particularly simple method of deriving the rate of excess enthalpy production based on measuring the times required to boil the cells to dryness, this process being followed by using time-lapse video recordings. Our use of this simple method as well as our investigations for the results of other research groups prompts us to present also other simple methods of data analysis which we have used in the preliminary evaluations of these systems. (orig.)

  11. FLUKA studies of hadron-irradiated scintillating crystals for calorimetry at the High-Luminosity LHC

    CERN Document Server

    Quittnat, Milena Eleonore

    2015-01-01

    Calorimetry at the High-Luminosity LHC (HL-LHC) will be performed in a harsh radiation environment with high hadron fluences. The upgraded CMS electromagnetic calorimeter design and suitable scintillating materials are a focus of current research. In this paper, first results using the Monte Carlo simulation program FLUKA are compared to measurements performed with proton-irradiated LYSO, YSO and cerium fluoride crystals. Based on these results, an extrapolation to the behavior of an electromagnetic sampling calorimeter, using one of the inorganic scintillators above as an active medium, is performed for the upgraded CMS experiment at the HL-LHC. Characteristic parameters such as the induced ambient dose, fluence spectra for different particle types and the residual nuclei are studied, and the suitability of these materials for a future calorimeter is surveyed. Particular attention is given to the creation of isotopes in an LYSO-tungsten calorimeter that might contribute a prohibitive background to the measu...

  12. Kinetics of Enzymatic High-Solid Hydrolysis of Lignocellulosic Biomass Studied by Calorimetry

    DEFF Research Database (Denmark)

    Olsen, Søren Nymand; Rasmussen, Erik Lumby; McFarland, K.C.

    2011-01-01

    Enzymatic hydrolysis of high-solid biomass (>10% w/w dry mass) has become increasingly important as a key step in the production of second-generation bioethanol. To this end, development of quantitative real-time assays is desirable both for empirical optimization and for detailed kinetic analysis....... In the current work, we have investigated the application of isothermal calorimetry to study the kinetics of enzymatic hydrolysis of two substrates (pretreated corn stover and Avicel) at high-solid contents (up to 29% w/w). It was found that the calorimetric heat flow provided a true measure of the hydrolysis...... analysis of the interrelationships of enzyme load and the rate, time, and extent of the reaction. The results suggest that the hydrolysis rate of pretreated corn stover is limited initially by available attack points on the substrate surface (

  13. Effects of positive end-expiratory pressure titration and recruitment maneuver on lung inflammation and hyperinflation in experimental acid aspiration-induced lung injury.

    Science.gov (United States)

    Ambrosio, Aline M; Luo, Rubin; Fantoni, Denise T; Gutierres, Claudia; Lu, Qin; Gu, Wen-Jie; Otsuki, Denise A; Malbouisson, Luiz M S; Auler, Jose O C; Rouby, Jean-Jacques

    2012-12-01

    In acute lung injury positive end-expiratory pressure (PEEP) and recruitment maneuver are proposed to optimize arterial oxygenation. The aim of the study was to evaluate the impact of such a strategy on lung histological inflammation and hyperinflation in pigs with acid aspiration-induced lung injury. Forty-seven pigs were randomly allocated in seven groups: (1) controls spontaneously breathing; (2) without lung injury, PEEP 5 cm H2O; (3) without lung injury, PEEP titration; (4) without lung injury, PEEP titration + recruitment maneuver; (5) with lung injury, PEEP 5 cm H2O; (6) with lung injury, PEEP titration; and (7) with lung injury, PEEP titration + recruitment maneuver. Acute lung injury was induced by intratracheal instillation of hydrochloric acid. PEEP titration was performed by incremental and decremental PEEP from 5 to 20 cm H2O for optimizing arterial oxygenation. Three recruitment maneuvers (pressure of 40 cm H2O maintained for 20 s) were applied to the assigned groups at each PEEP level. Proportion of lung inflammation, hemorrhage, edema, and alveolar wall disruption were recorded on each histological field. Mean alveolar area was measured in the aerated lung regions. Acid aspiration increased mean alveolar area and produced alveolar wall disruption, lung edema, alveolar hemorrhage, and lung inflammation. PEEP titration significantly improved arterial oxygenation but simultaneously increased lung inflammation in juxta-diaphragmatic lung regions. Recruitment maneuver during PEEP titration did not induce additional increase in lung inflammation and alveolar hyperinflation. In a porcine model of acid aspiration-induced lung injury, PEEP titration aimed at optimizing arterial oxygenation, substantially increased lung inflammation. Recruitment maneuvers further improved arterial oxygenation without additional effects on inflammation and hyperinflation.

  14. potentiometric titration curves of aluminium salt solutions and its

    African Journals Online (AJOL)

    a

    species, which set up a base to study on the hydrolysis-polymerization of Al3+. At the same time, significant effects of total aluminum concentration, temperature, halide ion, silicate radical, and organic acid radical on the titration curves and its critical points were observed. Given the three critical points which demarcating the ...

  15. Potentiometric titration curves of aluminium salt solutions and its ...

    African Journals Online (AJOL)

    At the same time, significant effects of total aluminum concentration, temperature, halide ion, silicate radical, and organic acid radical on the titration curves and its critical points were observed. Given the three critical points which demarcating the aluminum forms, we carry out a through investigation into the fundamental ...

  16. A dipstick sensor for coulometric acid-base titrations

    NARCIS (Netherlands)

    Olthuis, Wouter; van der Schoot, B.H.; Chavez, F.; Bergveld, Piet

    1989-01-01

    By performing an acid-base titration by coulometric generation of OH− or H+ ions at an inert electrode in close proximity to the pH-sensitive gate of an ISFET, it is possible to determine the acid or base concentration of a solution using the ISFET as an indicator device for the equivalence point in

  17. Using Spreadsheets to Produce Acid-Base Titration Curves.

    Science.gov (United States)

    Cawley, Martin James; Parkinson, John

    1995-01-01

    Describes two spreadsheets for producing acid-base titration curves, one uses relatively simple cell formulae that can be written into the spreadsheet by inexperienced students and the second uses more complex formulae that are best written by the teacher. (JRH)

  18. Determination of Acidity Constants by Gradient Flow-Injection Titration

    Science.gov (United States)

    Conceicao, Antonio C. L.; Minas da Piedade, Manuel E.

    2006-01-01

    A three-hour laboratory experiment, designed for an advanced undergraduate course in instrumental analysis that illustrates the application of the gradient chamber flow-injection titration (GCFIT) method with spectrophotometric detection to determine acidity constants is presented. The procedure involves the use of an acid-base indicator to obtain…

  19. A General Simulator for Acid-Base Titrations

    Science.gov (United States)

    de Levie, Robert

    1999-07-01

    General formal expressions are provided to facilitate the automatic computer calculation of acid-base titration curves of arbitrary mixtures of acids, bases, and salts, without and with activity corrections based on the Davies equation. Explicit relations are also given for the buffer strength of mixtures of acids, bases, and salts.

  20. Developing and Demonstrating an Augmented Reality Colorimetric Titration Tool

    Science.gov (United States)

    Tee, Nicholas Yee Kwang; Gan, Hong Seng; Li, Jonathan; Cheong, Brandon Huey-Ping; Tan, Han Yen; Liew, Oi Wah; Ng, Tuck Wah

    2018-01-01

    The handling of chemicals in the laboratory presents a challenge in instructing large class sizes and when students are relatively new to the laboratory environment. In this work, we describe and demonstrate an augmented reality colorimetric titration tool that operates out of the smartphone or tablet of students. It allows multiple students to…

  1. Electroconvulsive therapy stimulus titration: Not all it seems.

    Science.gov (United States)

    Rosenman, Stephen J

    2018-05-01

    To examine the provenance and implications of seizure threshold titration in electroconvulsive therapy. Titration of seizure threshold has become a virtual standard for electroconvulsive therapy. It is justified as individualisation and optimisation of the balance between efficacy and unwanted effects. Present day threshold estimation is significantly different from the 1960 studies of Cronholm and Ottosson that are its usual justification. The present form of threshold estimation is unstable and too uncertain for valid optimisation or individualisation of dose. Threshold stimulation (lowest dose that produces a seizure) has proven therapeutically ineffective, and the multiples applied to threshold to attain efficacy have never been properly investigated or standardised. The therapeutic outcomes of threshold estimation (or its multiples) have not been separated from simple dose effects. Threshold estimation does not optimise dose due to its own uncertainties and the different short-term and long-term cognitive and memory effects. Potential harms of titration have not been examined. Seizure threshold titration in electroconvulsive therapy is not a proven technique of dose optimisation. It is widely held and practiced; its benefit and harmlessness assumed but unproven. It is a prematurely settled answer to an unsettled question that discourages further enquiry. It is an example of how practices, assumed scientific, enter medicine by obscure paths.

  2. Comparison of a Handheld Indirect Calorimetry Device and Predictive Energy Equations Among Individuals on Maintenance Hemodialysis.

    Science.gov (United States)

    Morrow, Ellis A; Marcus, Andrea; Byham-Gray, Laura

    2017-11-01

    Practical methods for determining resting energy expenditure (REE) among individuals on maintenance hemodialysis (MHD) are needed because of the limitations of indirect calorimetry. Two disease-specific predictive energy equations (PEEs) have been developed for this metabolically complex population. The aim of this study was to compare estimated REE (eREE) by PEEs to measured REE (mREE) with a handheld indirect calorimetry device (HICD). A prospective pilot study of adults on MHD (N = 40) was conducted at 2 dialysis clinics in Houston and Texas City, Texas. mREE by an HICD was compared with eREE determined by 6 PEEs using Bland-Altman analysis with a band of acceptable agreement of ±10% of the group mean mREE. Paired t-test and the intraclass correlation coefficient were also used to compare the alternate methods of measuring REE. A priori alpha was set at P Maintenance Hemodialysis Equation-Creatinine version (MHCD-CR) was the most accurate PEE with 52.5% of values within the band of acceptable agreement, followed by the Mifflin-St. Jeor Equation and the Vilar et al. Equation at 45.0% and 42.5%, respectively. When compared with mREE by the HICD, the MHDE-CR was more accurate and precise than other PEEs evaluated; however, this must be interpreted with caution as mREE was consistently lower than eREE from all PEEs. Further research is needed to validate the MHDE-CR and other practical methods for determining REE among individuals on MHD. Copyright © 2017 National Kidney Foundation, Inc. Published by Elsevier Inc. All rights reserved.

  3. Accuracy and precision of protein–ligand interaction kinetics determined from chemical shift titrations

    International Nuclear Information System (INIS)

    Markin, Craig J.; Spyracopoulos, Leo

    2012-01-01

    NMR-monitored chemical shift titrations for the study of weak protein–ligand interactions represent a rich source of information regarding thermodynamic parameters such as dissociation constants (K D ) in the micro- to millimolar range, populations for the free and ligand-bound states, and the kinetics of interconversion between states, which are typically within the fast exchange regime on the NMR timescale. We recently developed two chemical shift titration methods wherein co-variation of the total protein and ligand concentrations gives increased precision for the K D value of a 1:1 protein–ligand interaction (Markin and Spyracopoulos in J Biomol NMR 53: 125–138, 2012). In this study, we demonstrate that classical line shape analysis applied to a single set of 1 H– 15 N 2D HSQC NMR spectra acquired using precise protein–ligand chemical shift titration methods we developed, produces accurate and precise kinetic parameters such as the off-rate (k off ). For experimentally determined kinetics in the fast exchange regime on the NMR timescale, k off ∼ 3,000 s −1 in this work, the accuracy of classical line shape analysis was determined to be better than 5 % by conducting quantum mechanical NMR simulations of the chemical shift titration methods with the magnetic resonance toolkit GAMMA. Using Monte Carlo simulations, the experimental precision for k off from line shape analysis of NMR spectra was determined to be 13 %, in agreement with the theoretical precision of 12 % from line shape analysis of the GAMMA simulations in the presence of noise and protein concentration errors. In addition, GAMMA simulations were employed to demonstrate that line shape analysis has the potential to provide reasonably accurate and precise k off values over a wide range, from 100 to 15,000 s −1 . The validity of line shape analysis for k off values approaching intermediate exchange (∼100 s −1 ), may be facilitated by more accurate K D measurements from NMR

  4. Insulin degludec once-daily in type 2 diabetes: simple or step-wise titration (BEGIN: once simple use).

    Science.gov (United States)

    Philis-Tsimikas, Athena; Brod, Meryl; Niemeyer, Marcus; Ocampo Francisco, Ann Marie; Rothman, Jeffrey

    2013-06-01

    Insulin degludec (IDeg) is a new basal insulin in development with a flat, ultra-long action profile that may permit dosing using a simplified titration algorithm with less frequent self-measured blood glucose (SMBG) measurements and more simplified titration steps than currently available basal insulins. This 26-week, multi-center, open-label, randomized, treat-to-target study compared the efficacy and safety of IDeg administered once-daily in combination with metformin in insulin-naïve subjects with type 2 diabetes using two different patient-driven titration algorithms: a "Simple" algorithm, with dose adjustments based on one pre-breakfast SMBG measurement (n = 111) versus a "Step-wise" algorithm, with adjustments based on three consecutive pre-breakfast SMBG values (n = 111). IDeg was administered using the FlexTouch® insulin pen (Novo Nordisk A/S, Bagsværd, Denmark), with once-weekly dose titration in both groups. Glycosylated hemoglobin (HbA1c) decreased from baseline to week 26 in both groups (-1.09%, IDegSimple; -0.93%, IDegStep-wise). IDegSimple was non-inferior to IDegStep-wise in lowering HbA1c [estimated treatment difference (IDegSimple - IDegStep-wise): -0.16% points (-0.39; 0.07)95% CI]. Fasting plasma glucose was reduced (-3.27 mmol/L, IDegSimple; -2.68 mmol/L, IDegStep-wise) with no significant difference between groups. Rates of confirmed hypoglycemia [1.60, IDegSimple; 1.17, IDegStep-wise events/patient year of exposure (PYE)] and nocturnal confirmed hypoglycemia (0.21, IDegSimple; 0.10, IDegStep-wise events/PYE) were low, with no significant differences between groups. Daily insulin dose after 26 weeks was 0.61 U/kg (IDegSimple) and 0.50 U/kg (IDegStep-wise). No significant difference in weight change was seen between groups by week 26 (+1.6 kg, IDegSimple; +1.1 kg, IDegStep-wise), and there were no clinically relevant differences in adverse event profiles. IDeg was effective and well tolerated using either the Simple or Step-wise titration

  5. Evaluation of modified boehm titration methods for use with biochars.

    Science.gov (United States)

    Fidel, Rivka B; Laird, David A; Thompson, Michael L

    2013-11-01

    The Boehm titration, originally developed to quantify organic functional groups of carbon blacks and activated carbons in discrete pK ranges, has received growing attention for analyzing biochar. However, properties that distinguish biochar from carbon black and activated carbon, including greater carbon solubility and higher ash content, may render the original Boehm titration method unreliable for use with biochars. Here we use seven biochars and one reference carbon black to evaluate three Boehm titration methods that use (i) acidification followed by sparging (sparge method), (ii) centrifugation after treatment with BaCl (barium method), and (iii) a solid-phase extraction cartridge followed by acidification and sparging (cartridge method) to remove carbonates and dissolved organic compounds (DOC) from the Boehm extracts before titration. Our results for the various combinations of Boehm reactants and methods indicate that no one method was free of bias for all three Boehm reactants and that the cartridge method showed evidence of bias for all pK ranges. By process of elimination, we found that a combination of the sparge method for quantifying functional groups in the lowest pK range (∼5 to 6.4), and the barium method for quantifying functional groups in the higher pK ranges (∼6.4 to 10.3 and ∼10.3 to 13) to be free of evidence for bias. We caution, however, that further testing is needed and that all Boehm titration results for biochars should be considered suspect unless efforts were undertaken to remove ash and prevent interference from DOC. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

  6. Evaluation of the performance of a metrohm titrator titrando-836 in potentiometric analysis of uranium for safeguards purposes

    International Nuclear Information System (INIS)

    Cristiano, Barbara Fernandes; Silva, Jose Wanderley S. da; Barros, Pedro Dionisio de; Araujo, Radier Mario S. de

    2009-01-01

    To achieve the requirements of the Brazilian State System of Accounting for and Control of Nuclear Materials - SSAC the Safeguards Laboratory of Brazilian Nuclear Energy Commission, LASAL, has been applying the 'Davies and Gray/NBL' method for Potentiometric determination of total uranium concentration in several forms of nuclear materials since 1984. To improve the accuracy and the repeatability the method uses as titrant, standard reference potassium dichromate NIST SRM 136e and the results are also corrected for bias with NBL CRM 112A uranium metal assay standard. This work describes the assays performed for validation of a Metrohm 836 potentiometric titrator acquired by LASAL in order to improve the analytical methodology of the laboratory. The titrator is attached to a Pt:Rh (90:10) as indicator electrode and a mercurous sulfate as the reference electrode. The evaluation of accuracy and repeatability were made by comparison, the results provided by the titrator with the certified value of standards and also by the participation in round robin program sponsored by New Brunswick Laboratory - NBL. The validation was done by a comparison of the performance between the Metrohm 836 and a Mettler - DL67 titrator which has currently been used by the laboratory. It included evaluation of the results of both equipment, the repeatability of the measurement, any systematic contributions and its uncertainties. (author)

  7. A modified two-point titration method for the determination of volatile fatty acids in anaerobic systems.

    Science.gov (United States)

    Mu, Zhe-Xuan; He, Chuan-Shu; Jiang, Jian-Kai; Zhang, Jie; Yang, Hou-Yun; Mu, Yang

    2018-04-10

    The volatile fatty acids (VFA) concentration plays important roles in the rapid start-up and stable operation of anaerobic reactors. It's essential to develop a simple and accurate method to monitor the VFA concentration in the anaerobic systems. In present work, a modified two-point titration method was developed to determine the VFA concentration. The results show that VFA concentration in standard solutions estimated by the titration method coincided well with that measured by gas chromatograph, where all relative errors were lower than 5.5%. Compared with the phosphate, ammonium and sulfide subsystems, the effect of bicarbonate on the accuracy of the developed method was relatively significant. When the bicarbonate concentration varied from 0 to 8 mmol/L, the relative errors increased from 1.2% to 30% for VFA concentration at 1 mmol/L, but were within 2.0% for that at 5 mmol/L. In addition, the VFA composition affected the accuracy of the titration method to some extent. This developed titration method was further proved to be effective with practical effluents from a lab-scale anaerobic reactor under organic shock loadings and an unstable full-scale anaerobic reactor. Copyright © 2018 Elsevier Ltd. All rights reserved.

  8. ASSESSMENT OF ATTENTION THRESHOLD IN RATS BY TITRATION OF VISUAL CUE DURATION DURING THE FIVE CHOICE SERIAL REACTION TIME TASK

    Science.gov (United States)

    Martin, Thomas J.; Grigg, Amanda; Kim, Susy A.; Ririe, Douglas G.; Eisenach, James C.

    2014-01-01

    Background The 5 choice serial reaction time task (5CSRTT) is commonly used to assess attention in rodents. We sought to develop a variant of the 5CSRTT that would speed training to objective success criteria, and to test whether this variant could determine attention capability in each subject. New Method Fisher 344 rats were trained to perform a variant of the 5CSRTT in which the duration of visual cue presentation (cue duration) was titrated between trials based upon performance. The cue duration was decreased when the subject made a correct response, or increased with incorrect responses or omissions. Additionally, test day challenges were provided consisting of lengthening the intertrial interval and inclusion of a visual distracting stimulus. Results Rats readily titrated the cue duration to less than 1 sec in 25 training sessions or less (mean ± SEM, 22.9 ± 0.7), and the median cue duration (MCD) was calculated as a measure of attention threshold. Increasing the intertrial interval increased premature responses, decreased the number of trials completed, and increased the MCD. Decreasing the intertrial interval and time allotted for consuming the food reward demonstrated that a minimum of 3.5 sec is required for rats to consume two food pellets and successfully attend to the next trial. Visual distraction in the form of a 3 Hz flashing light increased the MCD and both premature and time out responses. Comparison with existing method The titration variant of the 5CSRTT is a useful method that dynamically measures attention threshold across a wide range of subject performance, and significantly decreases the time required for training. Task challenges produce similar effects in the titration method as reported for the classical procedure. Conclusions The titration 5CSRTT method is an efficient training procedure for assessing attention and can be utilized to assess the limit in performance ability across subjects and various schedule manipulations. PMID

  9. Hydrogen concentration determination in pressure tube samples using differential scanning calorimetry (dsc)

    International Nuclear Information System (INIS)

    Marinescu, R.; Mincu, M.

    2015-01-01

    Zirconium alloys are widely used as a structural material in nuclear reactors. It is known that zirconium based cladding alloys absorb hydrogen as a result of service in a pressurized water reactor. Hydrogen absorbed (during operation of the reactor) in the zirconium alloy, out of which the pressure tube is made, is one of the major factors determining the life time of the pressure tube. For monitoring the hydrides, samples of the pressure tube are periodically taken and analyzed. At normal reactor operating temperature, hydrogen has limited solubility in the zirconium lattice and precipitates out of solid solution as zirconium hydride when the solid solubility is exceeded. As a consequences material characterization of Zr-2.5Nb CANDU pressure tubes is required after manufacturing but also during the operation to assess its structural integrity and to predict its behavior until the next in-service inspection. Hydrogen and deuterium concentration determination is one of the most important parameters to be evaluated during the experimental tests. Hydrogen present in zirconium alloys has a strong effect of weakening. Following the zirconium-hydrogen reaction, the resulting zirconium hydride precipitates in the mass of material. Weakening of the material, due to the presence of 10 ppm of precipitated hydrogen significantly affects some of its properties. The concentration of hydrogen in a sample can be determined by several methods, one of them being the differential scanning calorimetry (DSC). The principle of the method consists in measuring the difference between the amount of heat required to raise the temperature of a sample and a reference to a certain value. The experiments were made using a TA Instruments DSC Q2000 calorimeter. This paper contains experimental work for hydrogen concentration determination by Differential Scanning Calorimetry (DSC) method. Also, the reproducibility and accuracy of the method used at INR Pitesti are presented. (authors)

  10. Pyrolysis Combustion Flow Calorimetry Studies on Some Reactively Modified Polymers

    Directory of Open Access Journals (Sweden)

    Svetlana Tretsiakova-McNally

    2015-03-01

    Full Text Available As a part of our continuing work to improve the flame retardance of some chain-growth polymers, by employing a reactive route, we have synthesized several unsaturated compounds containing either phosphorus (P, or both phosphorus (P and nitrogen (N, bearing groups in different chemical environments. They included: diethyl(acryloyloxymethylphosphonate (DEAMP; diethyl(1-acryloyloxyethylphosphonate (DE1AEP; diethyl-2-(acryloyloxyethyl phosphate (DEAEP; diethyl-2-(metharyloyloxyethyl phosphate (DEMEP; acrylic acid-2-(diethoxyphosphorylaminoethyl ester (ADEPAE; acrylic acid-2-[(diethoxyphosphorylmethyl amino]ethyl ester (ADEPMAE. Acrylonitrile (AN, methyl methacrylate (MMA and styrene (S were free radically copolymerised with the above mentioned comonomers. The recovered polymers were subjected to routine spectroscopic and thermo-gravimetric analyses. In addition, the combustion behaviours of homopolymers as well as the copolymers containing nominal loadings of P-, or P/N-, groups were, primarily, evaluated using pyrolysis combustion flow calorimetry (PCFC. PCFC has been found to be a very useful screening technique, especially, in establishing the efficacies of the different modifying groups towards flame retarding some base polymeric materials. Values of the heat release capacity (HRC values normalised to the P contents (wt% can be considered as useful tool in ranking the various P-containing modifying groups in terms of their efficacies to flame-retard non-halogenated chain-growth polymers considered in the present work.

  11. An investigation of calibration methods for solution calorimetry.

    Science.gov (United States)

    Yff, Barbara T S; Royall, Paul G; Brown, Marc B; Martin, Gary P

    2004-01-28

    Solution calorimetry has been used in a number of varying applications within pharmaceutical research as a technique for the physical characterisation of pharmaceutical materials, such as quantifying small degrees of amorphous content, identifying polymorphs and investigating interactions between drugs and carbohydrates or proteins and carbohydrates. A calibration test procedure is necessary to validate the instrumentation; a few of the suggested calibration reactions are the enthalpies of solution associated with dissolving Tris in 0.1 M HCl or NaCl, KCl or propan-1-ol in water. In addition, there are a number of different methods available to determine enthalpies of solution from the experimental data provided by the calorimeter, for example, the Regnault-Pfaundler's method, a graphical extrapolation based on the Dickinson method, or a manual integration-based method. Thus, the aim of the study was to investigate how each of these methods influences the values for the enthalpy of solution. Experiments were performed according to the method outlined by Hogan and Buckton [Int. J. Pharm. 207 (2000) 57] using KCl (samples of 50, 100 and 200 mg), Tris and sucrose as calibrants. For all three materials the manual integration method was found to be the most consistent with the KCl in water (sample mass of 200 mg) being the most precise. Thus, this method is recommended for the validation of solution calorimeters.

  12. Study of Liquid Argon Dopants for LHC Hadron Calorimetry

    CERN Multimedia

    2002-01-01

    Hadron calorimetry based on the Liquid Argon Ionisation Chamber technique is one of the choice techniques for LHC-experimentation. A systematic study of the effect of selected dopants on Liquid Argon (LAr) will be carried out with the aim to achieve an improvement on: \\item (i)~``Fast Liquid Argon'' search and study of dopants to increase the drift velocity. It has been already shown that CH&sub4. added at a fraction of one percent increases the drift velocity by a factor of two or more. \\item (ii)~``Compensated Liquid Argon'' search and study of dopants to increase the response to densely ionising particles, resulting in improved compensation, such as photosensitive dopants. \\end{enumerate}\\\\ \\\\ Monitoring of the parameters involved in understanding the response of a calorimeter is essential. In case of doped LAr, the charge yield, the non-saturated drift velocity and the electron lifetime in the liquid should be precisely and simultaneously monitored as they all vary with the level of dopant concentrati...

  13. Colloid Titration--A Rapid Method for the Determination of Charged Colloid.

    Science.gov (United States)

    Ueno, Keihei; Kina, Ken'yu

    1985-01-01

    "Colloid titration" is a volumetric method for determining charged polyelectrolytes in aqueous solutions. The principle of colloid titration, reagents used in the procedure, methods of endpoint detection, preparation of reagent solutions, general procedure used, results obtained, and pH profile of colloid titration are considered. (JN)

  14. The Acid-Base Titration of a Very Weak Acid: Boric Acid

    Science.gov (United States)

    Celeste, M.; Azevedo, C.; Cavaleiro, Ana M. V.

    2012-01-01

    A laboratory experiment based on the titration of boric acid with strong base in the presence of d-mannitol is described. Boric acid is a very weak acid and direct titration with NaOH is not possible. An auxiliary reagent that contributes to the release of protons in a known stoichiometry facilitates the acid-base titration. Students obtain the…

  15. Acidity titration curves - a versatile tool for the characterisation of acidic mine waste water

    International Nuclear Information System (INIS)

    Fyson, A.

    2000-01-01

    Acidity titrations with NaOH are valuable tools for characterisation of acidic mine waters. - Titrations can be used to estimate metal concentrations. - Titrations can be carried out in the field, minimising changes in water chemistry due to sample handling time and procedure. (orig.)

  16. The Mobile Insulin Titration Intervention (MITI) for Insulin Adjustment in an Urban, Low-Income Population: Randomized Controlled Trial.

    Science.gov (United States)

    Levy, Natalie; Moynihan, Victoria; Nilo, Annielyn; Singer, Karyn; Bernik, Lidia S; Etiebet, Mary-Ann; Fang, Yixin; Cho, James; Natarajan, Sundar

    2015-07-17

    Diabetes patients are usually started on a low dose of insulin and their dose is adjusted or "titrated" according to their blood glucose levels. Insulin titration administered through face-to-face visits with a clinician can be time consuming and logistically burdensome for patients, especially those of low socioeconomic status (SES). Given the wide use of mobile phones among this population, there is the potential to use short message service (SMS) text messaging and phone calls to perform insulin titration remotely. The goals of this pilot study were to (1) evaluate if our Mobile Insulin Titration Intervention (MITI) intervention using text messaging and phone calls was effective in helping patients reach their optimal insulin glargine dose within 12 weeks, (2) assess the feasibility of the intervention within our clinic setting and patient population, (3) collect data on the cost savings associated with the intervention, and (4) measure patient satisfaction with the intervention. This was a pilot study evaluating an intervention for patients requiring insulin glargine titration in the outpatient medical clinic of Bellevue Hospital Center in New York City. Patients in the intervention arm received weekday SMS text messages from a health management platform requesting their fasting blood glucose values. The clinic's diabetes nurse educator monitored the texted responses on the platform website each weekday for alarm values. Once a week, the nurse reviewed the glucose values, consulted the MITI titration algorithm, and called patients to adjust their insulin dose. Patients in the usual care arm continued to receive their standard clinic care for insulin titration. The primary outcome was whether a patient reached his/her optimal insulin glargine dose within 12 weeks. A total of 61 patients consented and were randomized into the study. A significantly greater proportion of patients in the intervention arm reached their optimal insulin glargine dose than patients in

  17. Effect of temperature on the acid-base properties of the alumina surface: microcalorimetry and acid-base titration experiments.

    Science.gov (United States)

    Morel, Jean-Pierre; Marmier, Nicolas; Hurel, Charlotte; Morel-Desrosiers, Nicole

    2006-06-15

    Sorption reactions on natural or synthetic materials that can attenuate the migration of pollutants in the geosphere could be affected by temperature variations. Nevertheless, most of the theoretical models describing sorption reactions are at 25 degrees C. To check these models at different temperatures, experimental data such as the enthalpies of sorption are thus required. Highly sensitive microcalorimeters can now be used to determine the heat effects accompanying the sorption of radionuclides on oxide-water interfaces, but enthalpies of sorption cannot be extracted from microcalorimetric data without a clear knowledge of the thermodynamics of protonation and deprotonation of the oxide surface. However, the values reported in the literature show large discrepancies and one must conclude that, amazingly, this fundamental problem of proton binding is not yet resolved. We have thus undertaken to measure by titration microcalorimetry the heat effects accompanying proton exchange at the alumina-water interface at 25 degrees C. Based on (i) the surface sites speciation provided by a surface complexation model (built from acid-base titrations at 25 degrees C) and (ii) results of the microcalorimetric experiments, calculations have been made to extract the enthalpic variations associated respectively to first and second deprotonation of the alumina surface. Values obtained are deltaH1 = 80+/-10 kJ mol(-1) and deltaH2 = 5+/-3 kJ mol(-1). In a second step, these enthalpy values were used to calculate the alumina surface acidity constants at 50 degrees C via the van't Hoff equation. Then a theoretical titration curve at 50 degrees C was calculated and compared to the experimental alumina surface titration curve. Good agreement between the predicted acid-base titration curve and the experimental one was observed.

  18. Characterization of molecularly imprinted polymers using a new polar solvent titration method.

    Science.gov (United States)

    Song, Di; Zhang, Yagang; Geer, Michael F; Shimizu, Ken D

    2014-07-01

    A new method of characterizing molecularly imprinted polymers (MIPs) was developed and tested, which provides a more accurate means of identifying and measuring the molecular imprinting effect. In the new polar solvent titration method, a series of imprinted and non-imprinted polymers were prepared in solutions containing increasing concentrations of a polar solvent. The polar solvent additives systematically disrupted the templation and monomer aggregation processes in the prepolymerization solutions, and the extent of disruption was captured by the polymerization process. The changes in binding capacity within each series of polymers were measured, providing a quantitative assessment of the templation and monomer aggregation processes in the imprinted and non-imprinted polymers. The new method was tested using three different diphenyl phosphate imprinted polymers made using three different urea functional monomers. Each monomer had varying efficiencies of templation and monomer aggregation. The new MIP characterization method was found to have several advantages. To independently verify the new characterization method, the MIPs were also characterized using traditional binding isotherm analyses. The two methods appeared to give consistent conclusions. First, the polar solvent titration method is less susceptible to false positives in identifying the imprinting effect. Second, the method is able to differentiate and quantify changes in binding capacity, as measured at a fixed guest and polymer concentration, arising from templation or monomer aggregation processes in the prepolymerization solution. Third, the method was also easy to carry out, taking advantage of the ease of preparing MIPs. Copyright © 2014 John Wiley & Sons, Ltd.

  19. Determination of uranium by a gravimetric-volumetric titration method

    International Nuclear Information System (INIS)

    Krtil, J.

    1998-01-01

    A volumetric-gravimetric modification of a method for the determination of uranium based on the reduction of uranium to U (IV) in a phosphoric acid medium and titration with a standard potassium dichromate solution is described. More than 99% of the stoichiometric amount of the titrating solution is weighed and the remainder is added volumetrically by using the Mettler DL 40 RC Memotitrator. Computer interconnected with analytical balances collects continually the data on the analyzed samples and evaluates the results of determination. The method allows to determine uranium in samples of uranium metal, alloys, oxides, and ammonium diuranate by using aliquot portions containing 30 - 100 mg of uranium with the error of determination, expressed as the relative standard deviation, of 0.02 - 0.05%. (author)

  20. Analysis of the Purity of Cetrimide by Titrations

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov; Rasmussen, Claus/Dallerup; Nielsen, Hans/Boye

    2006-01-01

    The purity of cetrimide, trimethyl tetradecyl ammonium bromide (TTAB), that is an important preservative of many cosmetic and pharmaceutical products, was determined by three independent methods of titration. Traditionally, cetrimide was analysed by an assay method of the European Pharmacopoeia (Ph...... the extraction step of the Ph. Eur.-assay method. The distribution coefficients between chloroform and water of cetrimide and the corresponding iodide species (TTAI) were thus determined as 2150 ± 50 M-1 and 68000 ± 4000 M-1, respectively....

  1. Calorimetry at the international linear collider. From simulation to reality

    International Nuclear Information System (INIS)

    Wattimena, Nanda

    2010-02-01

    Calorimetry plays a crucial role in ongoing and upcoming high-energy physics experiments. To build a powerful calorimetric system with a performance tailored to the expected physics signatures, demands dedicated research and development of new readout technologies as well as dedicated reconstruction algorithms. The presented design of a calorimetric system which meets the high demands of precision physics at the future linear collider ILC, follows the paradigm of particle ow. Particle ow is a reconstruction principle that relies on a calorimetric system with high spatial granularity. In the detector optimisation process, the development of hardware and software are interlinked and cannot be judged independently. This thesis addresses two different aspects of detector optimisation, a test of the detector design against one example physics scenario and the development of a stable calibration procedure. In the rst part, a gauge-mediated Supersymmetry breaking scenario is used to test the design of the electromagnetic calorimeter in a full detector simulation study. The reconstruction of the neutralino properties, each decaying into a photon and a gravitino, requires a good energy resolution, as well as excellent position and angular resolution. The error bounds on the neutralino mass is strongly linked to the energy resolution, while the position and angular reconstruction of neutral particles is essential for the determination of the neutralino lifetime. The second part of this thesis focuses on the calibration procedure for a prototype of the hadron calorimeter. 7608 novel photodetectors are operated and tested in this prototype. They are exposed to beams of well de ned particle type and energy. The calibration is tested with a detailed study of electromagnetic showers inside the cubic-metre-sized prototype, with special attention paid towards the non-linearity correction. (orig.)

  2. Calorimetry at the international linear collider. From simulation to reality

    Energy Technology Data Exchange (ETDEWEB)

    Wattimena, Nanda

    2010-02-15

    Calorimetry plays a crucial role in ongoing and upcoming high-energy physics experiments. To build a powerful calorimetric system with a performance tailored to the expected physics signatures, demands dedicated research and development of new readout technologies as well as dedicated reconstruction algorithms. The presented design of a calorimetric system which meets the high demands of precision physics at the future linear collider ILC, follows the paradigm of particle ow. Particle ow is a reconstruction principle that relies on a calorimetric system with high spatial granularity. In the detector optimisation process, the development of hardware and software are interlinked and cannot be judged independently. This thesis addresses two different aspects of detector optimisation, a test of the detector design against one example physics scenario and the development of a stable calibration procedure. In the rst part, a gauge-mediated Supersymmetry breaking scenario is used to test the design of the electromagnetic calorimeter in a full detector simulation study. The reconstruction of the neutralino properties, each decaying into a photon and a gravitino, requires a good energy resolution, as well as excellent position and angular resolution. The error bounds on the neutralino mass is strongly linked to the energy resolution, while the position and angular reconstruction of neutral particles is essential for the determination of the neutralino lifetime. The second part of this thesis focuses on the calibration procedure for a prototype of the hadron calorimeter. 7608 novel photodetectors are operated and tested in this prototype. They are exposed to beams of well de ned particle type and energy. The calibration is tested with a detailed study of electromagnetic showers inside the cubic-metre-sized prototype, with special attention paid towards the non-linearity correction. (orig.)

  3. Interaction of molybdenum (6) with potassium benzyldithiocarbaminate during amperometric titration

    International Nuclear Information System (INIS)

    Galushko, S.V.; Usatenko, Yu.I.

    1975-01-01

    The paper is an amperometric study of the mechanism of interaction between molybdenum (VI) and potassium benzyl dithiocarbamate [BDTC] which was based on the use of voltamperometry, electron paramagnetic resonance, infrared spectroscopy, potentiometry and elemental analysis. In amperometric titration Mo(VI) with BDTC (pH 4-2) forms a red compound of low solubility. In more acidic media the intensity of coloration is increased and a violet hue develops. On the basis of the data obtained it is concluded that in the amperometric titration of Mo(VI) with potassium BDTC there is first formation of a Mo(VI) compound, which subsequently acquires a red colour as a result of the reduction of Mo(VI) to Mo(V). It was also established that the degree of reduction is small where titration is carried out in the range pH 4.8-0.1. Quantitative determination of Mo is performed most effectively in slightly acidic media. Mo reacts with potassium BDTC in a ratio of 1:2. (E.P.)

  4. Titratable acidity of beverages influences salivary pH recovery.

    Science.gov (United States)

    Tenuta, Livia Maria Andaló; Fernández, Constanza Estefany; Brandão, Ana Carolina Siqueira; Cury, Jaime Aparecido

    2015-01-01

    A low pH and a high titratable acidity of juices and cola-based beverages are relevant factors that contribute to dental erosion, but the relative importance of these properties to maintain salivary pH at demineralizing levels for long periods of time after drinking is unknown. In this crossover study conducted in vivo, orange juice, a cola-based soft drink, and a 10% sucrose solution (negative control) were tested. These drinks differ in terms of their pH (3.5 ± 0.04, 2.5 ± 0.05, and 5.9 ± 0.1, respectively) and titratable acidity (3.17 ± 0.06, 0.57 ± 0.04 and buffering capacity kept 15 mL of each beverage in their mouth for 10 s, expectorated it, and their saliva was collected after 15, 30, 45, 60, 90, and 120 s. The salivary pH, determined using a mini pH electrode, returned to the baseline value at 30 s after expectoration of the cola-based soft drink, but only at 90 s after expectoration of the orange juice. The salivary pH increased to greater than 5.5 at 15 s after expectoration of the cola drink and at 30 s after expectoration of the orange juice. These findings suggest that the titratable acidity of a beverage influences salivary pH values after drinking acidic beverages more than the beverage pH.

  5. A rapid method for titration of ascovirus infectivity.

    Science.gov (United States)

    Han, Ningning; Chen, Zishu; Wan, Hu; Huang, Guohua; Li, Jianhong; Jin, Byung Rae

    2018-05-01

    Ascoviruses are a recently described family and the traditional plaque assay and end-point PCR assay have been used for their titration. However, these two methods are time-consuming and inaccurate to titrate ascoviruses. In the present study, a quick method for the determination of the titer of ascovirus stocks was developed based on ascovirus-induced apoptosis in infected insect cells. Briefly, cells infected with serial dilutions of virus (10 -2 -10 -10 ) for 24 h were stained with trypan blue. The stained cells were counted, and the percentage of nonviable cells was calculated. The stained cell rate was compared between virus-infected and control cells. The minimum-dilution group that had a significant difference compared with control and the maximum-dilution group that had no significant difference were selected and then compared each well of the two groups with the average stained cell rate of control. The well was marked as positive well if the stained cell rate was higher than the average stained cell rate of control wells; otherwise, the well was marked as negative wells. The percentage of positive wells were calculated according to the number of positive. Subsequently, the virus titer was calculated through the method of Reed and Muench. This novel method is rapid, simple, reproducible, accurate, and less material-consuming and eliminates the subjectivity of the other procedures for titrating ascoviruses. Copyright © 2018 Elsevier B.V. All rights reserved.

  6. An interaction of the functionalized closo-borates with albumins: The protein fluorescence quenching and calorimetry study

    Energy Technology Data Exchange (ETDEWEB)

    Losytskyy, Mykhaylo Yu., E-mail: mlosytskyy@gmail.com [Institute of Molecular Biology and Genetics, NASU, 150 Zabolotnogo Street, 03143 Kyiv (Ukraine); Kovalska, Vladyslava B. [Institute of Molecular Biology and Genetics, NASU, 150 Zabolotnogo Street, 03143 Kyiv (Ukraine); Varzatskii, Oleg A. [V. I. Vernadsky Institute of General and Inorganic Chemistry, 32/34 Palladin Avenue, 03080 Kyiv (Ukraine); Kuperman, Marina V. [Institute of Molecular Biology and Genetics, NASU, 150 Zabolotnogo Street, 03143 Kyiv (Ukraine); Potocki, Slawomir; Gumienna-Kontecka, Elzbieta [Faculty of Chemistry, Wroclaw University, 14F. Joliot-Curie Street, 50-383 Wroclaw (Poland); Zhdanov, Andrey P. [Kurnakov Institute of General and Inorganic Chemistry, 31 Leninskii Avenue, 119991 Moscow (Russian Federation); Yarmoluk, Sergiy M. [Institute of Molecular Biology and Genetics, NASU, 150 Zabolotnogo Street, 03143 Kyiv (Ukraine); Voloshin, Yan Z. [Nesmeyanov Institute of Organoelement Compounds, 28 Vavilova Street, 119991 Moscow (Russian Federation); Zhizhin, Konstantin Yu.; Kuznetsov, Nikolai T. [Kurnakov Institute of General and Inorganic Chemistry, 31 Leninskii Avenue, 119991 Moscow (Russian Federation); Elskaya, Anna V. [Institute of Molecular Biology and Genetics, NASU, 150 Zabolotnogo Street, 03143 Kyiv (Ukraine)

    2016-01-15

    An interaction of the boron clusters closo-borates K{sub 2}[B{sub 10}H{sub 10}], K{sub 2}[B{sub 12}H{sub 12}] and their functionalized derivatives with serum proteins human (HSA) and bovine (BSA) albumins and immonoglobulin IgG as well as globular proteins β-lactoglobulin and lysozyme was characterized. The steady state and time resolved protein fluorescence quenching studies point on the binding of the closo-borate arylamine derivatives to serum albumins and discrimination of other proteins. The mechanism of the albumin fluorescence quenching by the closo-borate arylamine derivatives was proposed. The complex formation between albumin and the closo-borate molecules has been confirmed by isothermal titration calorimetry (ITC). The compound (K{sub 2}[B{sub 10}H{sub 10}]) and its arylamine derivative both interact with HSA, have close values of K{sub a} (1.4 and 1.2×10{sup 3} M{sup −1} respectively) and Gibbs energy (−17.9 and −17.5 kJ/mol respectively). However, the arylamine derivative forms complex with the higher guest/host binding ratio (4:1) comparing to the parent closo-borate (2:1). - Highlights: • Complex formation between boron clusters closo-borates and albumins was confirmed. • Functional substituent of closo-borate strongly affects its complex with albumins. • Binding of arylamine closo-borates essentially quench the albumin fluorescence. • Mechanism of tryptophan emission quenching by arylamine closo-borates was proposed.

  7. Using differential scanning calorimetry, laser refractometry, electrical conductivity and spectrophotometry for discrimination of different types of Bulgarian honey

    International Nuclear Information System (INIS)

    Vlaeva, I; Nikolova, K; Tsankova, D; Bodurov, I; Marudova, M; Viraneva, A; Yovcheva, T; Lekova, S

    2017-01-01

    The potential of several physical methods for investigation of the botanical origin of honey has been discussed. Samples from the three most prevalent types of honey in Bulgaria (acacia, linden and honeydew) have been used. They have been examined by laser refractometry, UV, VIS and FTIR spectroscopy, electric conductivity measurement and differential scanning calorimetry. The purpose of this study was to reveal the physical characterizations of honeys from different flora produced in Bulgaria and to identify honeys with a high apitherapy potential for future studies. (paper)

  8. Ionic liquids: differential scanning calorimetry as a new indirect method for determination of vaporization enthalpies.

    Science.gov (United States)

    Verevkin, Sergey P; Emel'yanenko, Vladimir N; Zaitsau, Dzmitry H; Ralys, Ricardas V; Schick, Christoph

    2012-04-12

    Differential scanning calorimetry (DSC) has been used to measure enthalpies of synthesis reactions of the 1-alkyl-3-methylimidazolium bromide [C(n)mim][Br] ionic liquids from 1-methylimidazole and n-alkyl bromides (with n = 4, 5, 6, 7, and 8). The optimal experimental conditions have been elaborated. Enthalpies of formation of these ionic liquids in the liquid state have been determined using the DSC results according to the Hess Law. The ideal-gas enthalpies of formation of [C(n)mim][Br] were calculated using the methods of quantum chemistry. They were used together with the DSC results to derive indirectly the enthalpies of vaporization of the ionic liquids under study. In order to validate the indirect determination, the experimental vaporization enthalpy of [C(4)mim][Br] was measured by using a quartz crystal microbalance (QCM). The combination of reaction enthalpy measurements by DSC with modern high-level first-principles calculations opens valuable indirect thermochemical options to obtain values of vaporization enthalpies of ionic liquids.

  9. Microcalorimetric and potentiometric titration studies on the adsorption of copper by P. putida and B. thuringiensis and their composites with minerals

    International Nuclear Information System (INIS)

    Fang Linchuan; Cai Peng; Li Pengxiang; Wu Huayong; Liang Wei; Rong Xingmin; Chen Wenli; Huang Qiaoyun

    2010-01-01

    In order to have a better understanding of the interactions of heavy metals with bacteria and minerals in soil and associated environments, isothermal titration calorimetry (ITC), potentiometric titration and equilibrium sorption experiments were conducted to investigate the adsorption behavior of Cu(II) by Bacillus thuringiensis, Pseudomonas putida and their composites with minerals. The interaction of montmorillonite with bacteria increased the reactive sites and resulted in greater adsorption for Cu(II) on their composites, while decreased adsorption sites and capacities for Cu(II) were observed on goethite-bacteria composites. A gram-positive bacterium B. thuringiensis played a more important role than a gram-negative bacterium P. putida in determining the properties of the bacteria-minerals interfaces. The enthalpy changes (ΔH ads ) from endothermic (6.14 kJ mol -1 ) to slightly exothermic (-0.78 kJ mol -1 ) suggested that Cu(II) is complexed with the anionic oxygen ligands on the surface of bacteria-mineral composites. Large entropies (32.96-58.89 J mol -1 K -1 ) of Cu(II) adsorption onto bacteria-mineral composites demonstrated the formation of inner-sphere complexes in the presence of bacteria. The thermodynamic data implied that Cu(II) mainly bound to the carboxyl and phosphoryl groups as inner-sphere complexes on bacteria and mineral-bacteria composites.

  10. Microcalorimetric and potentiometric titration studies on the adsorption of copper by P. putida and B. thuringiensis and their composites with minerals

    Energy Technology Data Exchange (ETDEWEB)

    Fang Linchuan [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Cai Peng; Li Pengxiang; Wu Huayong; Liang Wei; Rong Xingmin [Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China); Chen Wenli [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Huang Qiaoyun, E-mail: qyhuang@mail.hzau.edu.cn [State Key Laboratory of Agricultural Microbiology, Huazhong Agricultural University, Wuhan 430070 (China); Key Laboratory of Subtropical Agriculture and Environment, Ministry of Agriculture, College of Resources and Environment, Huazhong Agricultural University, Wuhan 430070 (China)

    2010-09-15

    In order to have a better understanding of the interactions of heavy metals with bacteria and minerals in soil and associated environments, isothermal titration calorimetry (ITC), potentiometric titration and equilibrium sorption experiments were conducted to investigate the adsorption behavior of Cu(II) by Bacillus thuringiensis, Pseudomonas putida and their composites with minerals. The interaction of montmorillonite with bacteria increased the reactive sites and resulted in greater adsorption for Cu(II) on their composites, while decreased adsorption sites and capacities for Cu(II) were observed on goethite-bacteria composites. A gram-positive bacterium B. thuringiensis played a more important role than a gram-negative bacterium P. putida in determining the properties of the bacteria-minerals interfaces. The enthalpy changes ({Delta}H{sub ads}) from endothermic (6.14 kJ mol{sup -1}) to slightly exothermic (-0.78 kJ mol{sup -1}) suggested that Cu(II) is complexed with the anionic oxygen ligands on the surface of bacteria-mineral composites. Large entropies (32.96-58.89 J mol{sup -1} K{sup -1}) of Cu(II) adsorption onto bacteria-mineral composites demonstrated the formation of inner-sphere complexes in the presence of bacteria. The thermodynamic data implied that Cu(II) mainly bound to the carboxyl and phosphoryl groups as inner-sphere complexes on bacteria and mineral-bacteria composites.

  11. Isothermal titration calorimetric and computational studies on the binding of chitooligosaccharides to pumpkin (Cucurbita maxima) phloem exudate lectin.

    Science.gov (United States)

    Narahari, Akkaladevi; Singla, Hitesh; Nareddy, Pavan Kumar; Bulusu, Gopalakrishnan; Surolia, Avadhesha; Swamy, Musti J

    2011-04-14

    The interaction of chitooligosaccharides [(GlcNAc)(2-6)] with pumpkin phloem exudate lectin (PPL) was investigated by isothermal titration calorimetry and computational methods. The dimeric PPL binds to (GlcNAc)(3-5) with binding constants of 1.26-1.53 × 10(5) M(-1) at 25 °C, whereas chitobiose exhibits approximately 66-fold lower affinity. Interestingly, chitohexaose shows nearly 40-fold higher affinity than chitopentaose with a binding constant of 6.16 × 10(6) M(-1). The binding stoichiometry decreases with an increase in the oligosaccharide size from 2.26 for chitobiose to 1.08 for chitohexaose. The binding reaction was essentially enthalpy driven with negative entropic contribution, suggesting that hydrogen bonds and van der Waals' interactions are the main factors that stabilize PPL-saccharide association. The three-dimensional structure of PPL was predicted by homology modeling, and binding of chitooligosaccharides was investigated by molecular docking and molecular dynamics simulations, which showed that the protein binding pocket can accommodate up to three GlcNAc residues, whereas additional residues in chitotetraose and chitopentaose did not exhibit any interactions with the binding pocket. Docking studies with chitohexaose indicated that the two triose units of the molecule could interact with different protein binding sites, suggesting formation of higher order complexes by the higher oligomers of GlcNAc by their simultaneous interaction with two protein molecules.

  12. A new approach to flow-batch titration. A monosegmented flow titrator with coulometric reagent generation and potentiometric or biamperometric detection.

    Science.gov (United States)

    de Aquino, Emerson Vidal; Rohwedder, Jarbas José Rodrigues; Pasquini, Celio

    2006-11-01

    Monosegmented flow analysis (MSFA) has been used as a flow-batch system to produce a simple, robust, and mechanized titrator that enables true titrations to be performed without the use of standards. This paper also introduces the use of coulometry with monosegmented titration by proposing a versatile flow cell. Coulometric generation of the titrand is attractive for titrations performed in monosegmented systems, because the reagent can be added without increasing the volume of sample injected. Also, biamperomeric and potentiometric detection of titration end-points can increase the versatility of the monosegmented titrator. The cell integrates coulometric generation of the titrand with detection of end-point by potentiometry or biamperometry. The resulting titrator is a flow-batch system in which the liquid monosegment, constrained by the interfaces of the gaseous carrier stream, plays the role of a sample of known volume to be titrated. The system has been used for determination of ascorbic acid, by coulometric generation of I2 with biamperometric detection, and for determination of Fe(II), by coulometric generation of Ce(IV) with potentiometric detection of the end-point, both in feed supplements.

  13. Determination of iodide by volumetric titration in support of the oil eletrolabeling with {sup 123}I

    Energy Technology Data Exchange (ETDEWEB)

    Kenup-Cantuaria, Hericka O.H.; Brandao, Luis E.B., E-mail: hkenup@ien.gov.br, E-mail: brandao@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil); Silva, Ademir X., E-mail: ademir@nuclear.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (PEN/COPPE/UFRJ), Rio de Janeiro, RJ (Brazil). Programa de Engenharia Nuclear

    2015-07-01

    The accuracy in measuring flow rate in pipelines is essential task to control various technical parameters in an industrial plant in oil industry and its derivatives. For this reason, it becomes increasingly widespread the uses of organic molecules labeled with radioactive isotopes mainly because of the wide possibility in use of different radioisotopes also due to the new labeling techniques. This paper presents a study to develop an electrochemical technique for oil labeling with iodine -123 and to determine the yield of production by measuring the concentration of iodide (I{sup -}) during this process. The volumetric titration technique was applied as a basis for quantitative and qualitative measures to monitor the labeling process. The results indicate the technical proposal as a viable alternative for monitoring electro labeling process of lubricating oils with iodine -123. (author)

  14. Charge characteristics of humic and fulvic acids: comparative analysis by colloid titration and potentiometric titration with continuous pK-distribution function model.

    Science.gov (United States)

    Bratskaya, S; Golikov, A; Lutsenko, T; Nesterova, O; Dudarchik, V

    2008-09-01

    Charge characteristics of humic and fulvic acids of a different origin (inshore soils, peat, marine sediments, and soil (lysimetric) waters) were evaluated by means of two alternative methods - colloid titration and potentiometric titration. In order to elucidate possible limitations of the colloid titration as an express method of analysis of low content of humic substances we monitored changes in acid-base properties and charge densities of humic substances with soil depth, fractionation, and origin. We have shown that both factors - strength of acidic groups and molecular weight distribution in humic and fulvic acids - can affect the reliability of colloid titration. Due to deviations from 1:1 stoichiometry in interactions of humic substances with polymeric cationic titrant, the colloid titration can underestimate total acidity (charge density) of humic substances with domination of weak acidic functional groups (pK>6) and high content of the fractions with molecular weight below 1kDa.

  15. Determination of net energy content of soybean oil fed to growing pigs using indirect calorimetry.

    Science.gov (United States)

    Li, Enkai; Lv, Zhiqian; Liu, Hu; Liu, Ling; Li, Yakui; Li, Zhongchao; Wang, Fenglai; Li, Defa; Zhang, Shuai

    2018-01-01

    The objectives of this experiment were: (i) to determine the net energy (NE) of soybean oil (SBO) fed to growing pigs using indirect calorimetry (IC); and (ii) to evaluate the effects of inclusion rate of SBO on heat production, oxidative status and nutrient digestibility in growing pigs. Eighteen growing barrows were allotted to three diets based on completely randomized design with six replicate pigs (period) per diet. Diets included a corn-soybean meal basal diet and two test diets containing 5% or 10% SBO at the expense of corn and soybean meal. During each period, pigs were individually housed in metabolism crates for 14 days, including 7 days to adapt to feed, metabolism crate and environmental conditions. On day 8, pigs were transferred to the open-circuit respiration chambers for measurement of daily O 2 consumption and CO 2 and CH 4 production. During this time, pigs were fed one of the three diets at 2.4 MJ metabolizable energy/kg body weight (BW) 0.6 /day. Total feces and urine were collected and daily total heat production (THP) was measured from days 9 to 13 and fasted on day 14 to evaluate their fasting heat production (FHP). The results show that trends of decreased apparent total tract digestibility of neutral detergent fiber (linear, P = 0.09) and acid detergent fiber (linear, P = 0.07) were observed as the content of dietary lipids increased. The average THP for the three diets were 1326, 1208 and 1193 kJ/kg BW 0.6 /day, respectively. The FHP of pigs averaged 843 kJ/kg BW 0.6 /day and was not affected by diet characteristics. A reduction of the respiratory quotients in the fed state as the inclusion level of SBO increased was observed. In conclusion, the NE values of SBO we determined by indirect calorimetry were 33.45 and 34.05 MJ/kg dry matter under two inclusion levels. THP could be largely reduced when SBO is added in the feed, but the THP of SBO included at 5% in a corn-soybean meal diet is not different from the THP of SBO included

  16. A digital image-based method for determining of total acidity in red wines using acid-base titration without indicator.

    Science.gov (United States)

    Tôrres, Adamastor Rodrigues; Lyra, Wellington da Silva; de Andrade, Stéfani Iury Evangelista; Andrade, Renato Allan Navarro; da Silva, Edvan Cirino; Araújo, Mário César Ugulino; Gaião, Edvaldo da Nóbrega

    2011-05-15

    This work proposes the use of digital image-based method for determination of total acidity in red wines by means of acid-base titration without using an external indicator or any pre-treatment of the sample. Digital images present the colour of the emergent radiation which is complementary to the radiation absorbed by anthocyanines present in wines. Anthocyanines change colour depending on the pH of the medium, and from the variation of colour in the images obtained during titration, the end point can be localized with accuracy and precision. RGB-based values were employed to build titration curves, and end points were localized by second derivative curves. The official method recommends potentiometric titration with a NaOH standard solution, and sample dilution until the pH reaches 8.2-8.4. In order to illustrate the feasibility of the proposed method, titrations of ten red wines were carried out. Results were compared with the reference method, and no statistically significant difference was observed between the results by applying the paired t-test at the 95% confidence level. The proposed method yielded more precise results than the official method. This is due to the trivariate nature of the measurements (RGB), associated with digital images. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. Simultaneous Absorptance and Thermal-Diffusivity Determination of Optical Components with Laser Calorimetry Technique

    Science.gov (United States)

    Wang, Yanru; Li, Bincheng

    2012-11-01

    The laser calorimetry (LCA) technique is used to determine simultaneously the absorptances and thermal diffusivities of optical components. An accurate temperature model, in which both the finite thermal conductivity and the finite sample size are taken into account, is employed to fit the experimental temperature data measured with an LCA apparatus for a precise determination of the absorptance and thermal diffusivity via a multiparameter fitting procedure. The uniqueness issue of the multiparameter fitting is discussed in detail. Experimentally, highly reflective (HR) samples prepared with electron-beam evaporation on different substrates (BK7, fused silica, and Ge) are measured with LCA. For the HR-coated sample on a fused silica substrate, the absorptance is determined to be 15.4 ppm, which is close to the value of 17.6 ppm, determined with a simplified temperature model recommended in the international standard ISO11551. The thermal diffusivity is simultaneously determined via multiparameter fitting to be approximately 6.63 × 10-7 m2 · s-1 with a corresponding square variance of 4.8 × 10-4. The fitted thermal diffusivity is in reasonably good agreement with the literature value (7.5 × 10-7 m2 · s -1). Good agreement is also obtained for samples with BK7 and Ge substrates.

  18. Determination of calorific values of forest waste biomass by static bomb calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Nunez-Regueira, L.; Rodriguez-Anon, J.A.; Proupin-Castineiras, J.; Vilanova-Diz, A.; Montero-Santovena, N. [Department of Applied Physics, Research Group TERBIPROMAT, University of Santiago, 15706 Santiago (Spain)

    2001-04-26

    Calorific values of forest waste originating from forestry works such as woodland cleaning, reaforestation and, all other silviculture tasks, were measured by static bomb calorimetry. These waste materials, heretofore considered as useless refuse, are beginning to be used as alternative fuels in wide social sectors all over the world. Two of the main forest species, eucalyptus (E. globulus Labill) and pine (P. pinaster Aiton) existing in Galicia (NW Spain), are included in this study. The experimental procedure was based on that proposed by Hubbard et al. [Experimental Thermochemistry, Interscience, New York, 1956, p. 5]. Simultaneously, some other parameters such as elementary chemical composition and heavy metal contents, moisture, density, and ash percentage after combustion in the bomb, were also determined. The experimental results, with calorific values exceeding 20000kJkg{sup -1}, make it advisable to use these materials as alternative fuels. The different parameters were measured using, as main equipment, a bomb calorimeter with an oxygen atmosphere, an elementary analysis equipment, and an atomic absorption spectrophotometer.

  19. Building a Graphite Calorimetry System for the Dosimetry of Therapeutic X-ray Beams

    Directory of Open Access Journals (Sweden)

    In Jung Kim

    2017-06-01

    Full Text Available A graphite calorimetry system was built and tested under irradiation. The noise level of the temperature measurement system was approximately 0.08 mK (peak to peak. The temperature of the core part rose by approximately 8.6 mK at 800 MU (monitor unit for 6-MV X-ray beams, and it increased as X-ray energy increased. The temperature rise showed less spread when it was normalized to the accumulated charge, as measured by an external monitoring chamber. The radiation energy absorbed by the core part was determined to have values of 0.798 J/μC, 0.389 J/μC, and 0.352 J/μC at 6 MV, 10 MV, and 18 MV, respectively. These values were so consistent among repeated runs that their coefficient of variance was less than 0.15%.

  20. Determination of kinetics and heat of hydrolysis for non-homogenous substrate by isothermal calorimetry.

    Science.gov (United States)

    Tafoukt, D; Soric, A; Sigoillot, J-C; Ferrasse, J-H

    2017-04-01

    The competitiveness of the second-generation bioethanol by biotechnological process requires an effective and quantitative control of biochemical reactions. In this study, the potential of isothermal calorimetry technique to measure heat and kinetics of a non-homogeneous substrate enzymatic hydrolysis is intended. Using this technique, optimum temperature of the enzymes used for lignocellulosic molecules hydrolysis was determined. Thus, the amount of substrate-to-enzyme ratio was highlighted as an important parameter of the hydrolysis yield. Furthermore, a new enzymes' cocktail efficiency consisting of a mix of cellulases and cellobiose dehydrogenase (CDH) was qualified by this technique. The results showed that this cocktail allowed the production of a high amount of gluconic acid that could improve the attractiveness of these second-generation biofuels. From the set of experiments, the hydrolysis heat of wheat straw was derived and a meaningful value of -32.2 ± 3.2 J g -1 (gram reducing sugars product) is calculated. Then, isothermal measurements were used to determine kinetic constants of the cellulases and CDH mix on wheat straw. Results showed that this enzyme cocktail has an optimal rate at 45 °C in the range of temperatures tested (40-55 °C).

  1. Thermal hazard assessment of oxidizer solutions and emulsion explosives utilizing accelerating rate and Dewar calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Jones, D.E.G.; Lightfoot, P.D.; Fouchard, R.C. [Natural Resources Canada, CANMET, Canadian Explosives Research Laboratory, Ottawa, ON (Canada)

    2002-07-01

    Accelerating rate calorimetry (ARC) and adiabatic Dewar calorimetric experiments were carried out on oxidizers used in the manufacture of emulsion explosives, their aqueous solutions, a bulk explosive matrix and a detonator-sensitive packaged explosive. The experiments were carried out in both closed and vented experimental configurations. The effects of water levels on the oxidizer solutions were investigated and the results obtained by using the two different techniques were compared. The Dewar experiments were found to yield a better direct estimation of bulk onset temperatures due to their greater sensitivity and lower 'phi factor'. Onset temperatures of oxidizer solutions measured using the Dewar calorimeter were found to be about 15 degrees C lower than those measured by ARC. Onset temperatures for the same oxidizer solution are lower for open systems than for closed systems. Results for emulsion explosives appeared complex, but indications are that oxidation of the oil phase in air is the first exothermic step in the runaway reaction. Whether this oxidation reaction can generate enough heat to drive the reaction to runaway, is not clear. Further elucidation of the complex exothermic reactions of emulsion explosives and their constituents, using both ARC and Dewar calorimetric techniques is recommended. 8 refs., 1 tab., 9 figs.

  2. Appropriateness of the definition of 'sedentary' in young children: Whole-room calorimetry study.

    Science.gov (United States)

    Reilly, John J; Janssen, Xanne; Cliff, Dylan P; Okely, Anthony D

    2015-09-01

    The present study aimed to measure the energy cost of three common sedentary activities in young children to test whether energy expended was consistent with the recent consensus definition of 'sedentary' as 'any behaviour conducted in a sitting or reclining posture and with an energy cost ≤ 1.5 metabolic equivalents (METs)' (Sedentary Behaviour Research Network, 2012). Observational study. Whole-room calorimetry measures of television viewing, sitting at a table drawing and reading, and sitting on the floor playing with toys were made in 40 young children (mean age 5.3 years, SD 1.0). The energy cost of each sedentary activity was consistent with the recent consensus definition of sedentary: 1.17 METs (95% CI 1.07-1.27) for TV viewing; 1.38 METs (95% CI 1.30-1.46) for sitting at a table; and 1.35 METs (95% CI 1.28-1.43) for floor-based play. Common sedentary activities in young children have energy costs which are consistent with the recent consensus definition of 'sedentary', and the present study is supportive of this definition. Copyright © 2014 Sports Medicine Australia. Published by Elsevier Ltd. All rights reserved.

  3. Thermodynamic study of complexation of thorium with pyridine monocarboxylates by calorimetry and DFT calculations

    International Nuclear Information System (INIS)

    Rama Mohana Rao, D.; Rawat, Neetika; Sawant, R.M.; Tomar, B.S.; Manna, D.; Ghanty, T.K.

    2013-01-01

    Stability constants of Th(IV) complexes with pyridine mono-carboxylates, namely, picolinate, nicotinate and isonicotinate have been determined following potentiometric titration of the metal ion and ligand mixtures with NaOH solution of known concentration. These data were used during the analysis of the calorimetric titration data to obtain the enthalpy of complexation reactions. The experimental data have been compared with that obtained from the DFT based theoretical calculations. (author)

  4. Approximate time to steady state resting energy expenditure using indirect calorimetry in young, healthy adults

    Directory of Open Access Journals (Sweden)

    Collin Popp

    2016-11-01

    Full Text Available Indirect calorimetry (IC measurements to estimate resting energy expenditure (REE necessitate a stable measurement period, or steady state (SS. There is limited evidence when assessing the time to reach SS in young, healthy adults. The aims of this prospective study are to determine the approximate time to necessary reach SS using open-circuit IC and to establish the appropriate duration of SS needed to estimate REE. One hundred young, healthy participants (54 males and 46 females; age = 20.6 ± 2.1 years; body weight = 73.6 ± 16.3 kg; height 172.5 ± 9.3 cm; BMI = 24.5 ± 3.8 kg/m2 completed IC measurement for approximately 30-minutes while the volume of oxygen (VO2 and volume of carbon dioxide (VCO2 were collected. SS was defined by variations in the VO2 and VCO2 of ≤10% coefficient of variation (%CV over a period of 5- consecutive minutes. The 30-minute IC measurement was divided into six 5-minute segments, S1, S2, S3, S4, S5 and S6. The results show that SS was achieved during S2 (%CV = 6.81 ± 3.2%, and the %CV continued to met the SS criteria for the duration of the IC measurement (S3= 8.07 ± 4.4%; S4 = 7.93 ± 3.7%; S5 = 7.75 ± 4.1%; S6 = 8.60 ± 4.6%. The current study found that in a population of young, healthy adults the duration of the IC measurement period could be a minimum of 10 minutes. The first 5-minute segment was discarded, while SS occurred by the second 5-minute segment.

  5. Determination of surface charge density of α-alumina by acid-base titration

    Directory of Open Access Journals (Sweden)

    Justin W. Ntalikwa

    2007-04-01

    Full Text Available The surface charge density (σo of colloidal alpha alumina suspended in various 1:1 electrolytes was measured using acid-base titration. An autotitrator capable of dispensing accurately 25 plus or minus 0.1 μL of titrant was used. The pH and temperature in the titration cell were monitored using single junction electrodes and platinum resistance thermometers, respectively. A constant supply of nitrogen gas in the cell was used to maintain inert conditions. The whole set up was interfaced with a computer for easy data acquisition. It was observed that the material exhibits a point of zero charge (PZC, this occurred at pH of 7.8 plus or minus 0.1, 7.6 plus or minus 0.2, 8.5 plus or minus 0.1, 8.3 plus or minus 0.1 for NaCl, NaNO3, CsCl and CsNO3 systems, respectively. It was also observed that below PZC, σo increases with increase in electrolyte concentration (Co whereas above PZC, σo decreases with increase in Co. It was concluded that σo of this material is a function of pH and Co and that its polarity can be varied through zero by varying these parameters.

  6. Determination of water in forages and animal feeds by Karl Fischer titration.

    Science.gov (United States)

    Van Erem, T; Thiex, N; Pohmer, J; Poffenbarger, W M; Smith, V; Patel, E

    1998-01-01

    Oven methods for determining moisture (volatiles) in forages and other animal feeds are empirical. The moisture concentration obtained depends upon the time and temperature the sample was dried and is influenced by the presence of other volatiles than water. A validated reference method to measure water in forages and animal feeds could be used to evaluate the appropriateness of oven methods for various types of animal feeds and forages. Karl Fischer titration is a well-established method for determining water. However, thorough extraction of water from forages and feeds is a challenge because they often contain cellular structures that release water slowly. Water was successfully extracted into methanol-formamide (50 + 50) by high-speed homogenization and then titrated directly at 50 degrees C with a one-component Karl Fischer reagent based on imidazole. The method is described in detail, results of day-to-day repeatability and laboratory-to-laboratory reproducibility are reported, and preliminary comparison data between oven methods are provided.

  7. A new method for determining the acid number of biodiesel based on coulometric titration.

    Science.gov (United States)

    Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

    2012-08-15

    A new method is proposed for determining the acid number (AN) of biodiesel using coulometric titration with potentiometric detection, basically employing a potentiostat/galvanostat and an electrochemical cell containing a platinum electrode, a silver electrode, and a combination pH electrode. The method involves a sequential application of a constant current between the platinum (cathode) and silver (anode) electrodes, followed by measuring the potential of the combination pH electrode, using an isopropanol/water mixture as solvent and LiCl as the supporting electrolyte. A preliminary evaluation of the new method, using acetic acid for doping a biodiesel sample, showed an average recovery of 100.1%. Compared to a volumetric titration-based method for determining the AN of several biodiesel samples (ranging from about 0.18 to 0.95 mg g(-1)), the new method produced statistically similar results with better repeatability. Compared to other works reported in the literature, the new method presented an average repeatability up to 3.2 times better and employed a sample size up to 20 times smaller. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. A novel method for the determination of the degree of deacetylation of chitosan by coulometric titration.

    Science.gov (United States)

    Wang, Chao; Yuan, Fang; Pan, Jiabao; Jiao, Shining; Jin, Ling; Cai, Hongwei

    2014-09-01

    A novel method to determine the degree of deacetylation of chitosan is described. In this method, the coulometric titrant OH- is generated by the electrolysis of water. The OH- reacted with the residual hydrochloric acid in chitosan solution and the degree of deacetylation was obtained by Faraday's law. The optimized experimental parameters in this study were 1.0 mol/L KCl as supporting electrolyte, 15.00 mA as the intensity of constant current, composite glass electrode as indicating electrode couples, double platinum generated electrode-platinum wire auxiliary electrode as working electrode pairs, pH 3.80 as the titration end-point. The degree of deacetylation in the four samples, which varied from 70 to 95% were measured. The results were similar to those from 1H NMR and the standard deviations were lower than 0.5%. With merit of simplicity, convenience, quickness, high accuracy and precision, automatic detection of titration end-point and low-cost, the proposed method will be very useful in the industrial production. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Clinical usefulness of the bispectral index for titrating propofol target effect-site concentration.

    Science.gov (United States)

    Struys, M; Versichelen, L; Byttebier, G; Mortier, E; Moerman, A; Rolly, G

    1998-01-01

    The bispectral index, a new processed electroencephalographic parameter which may give information on depth of anaesthesia, was used in 58 patients undergoing outpatient gynaecological surgery in order to study if the addition of bispectral index monitoring to standard clinical monitoring could improve the titration of target propofol concentration when using effect-site target-controlled propofol infusion for sedation. In Group 1 (n = 30), the bispectral index was recorded but the anaesthetist was unaware of the readings and therefore only classical signs of depth of anaesthesia were used to guide the anaesthetist in controlling the effect-site concentration. In Group 2 (n = 28), bispectral index readings were available to the anaesthetist and effect-site concentration was adjusted to ensure that bispectral index was maintained between 40 and 60. Similar propofol induction and maintenance doses, blood and effect-site concentrations and mean bispectral index were found in the two groups. A greater percentage of bispectral index readings lying outside the target range (i.e. 60) and more movement at incision and during maintenance were found in Group 1. There was a trend towards more implicit awareness in patients in Group 1. Bispectral index was found to be useful for measuring depth of sedation when using propofol target-controlled infusion. Propofol dosage could not be decreased but a more consistent level of sedation could be maintained due to a more satisfactory titration of target effect-site concentration.

  10. Characterization of Sea Lettuce Surface Functional Groups by Potentiometric Titrations

    Science.gov (United States)

    Ebling, A. M.; Schijf, J.

    2008-12-01

    In pursuit of our ultimate goal to better understand the prodigious capacity of the marine macroalga Ulva lactuca (sea lettuce) for adsorbing a broad range of dissolved trace metals from seawater, we performed an initial characterization of its surface functional groups. Specifically, the number of distinct functional groups as well as their individual bulk concentrations and acid dissociation constants (pKas) were determined by potentiometric titrations in NaCl solutions of various ionic strengths (I = 0.01-5.0 M), under inert nitrogen atmosphere at 25°C. Depending on the ionic strength, Ulva samples were manually titrated down to pH 2 or 3 with 1 N HCl and then up to pH 10 with 1 N NaOH in steps of 0.1-0.2 units, continuously monitoring pH with a glass combination electrode. Titrations of a dehydrated Ulva standard reference material (BCR-279) were compared with fresh Ulva tissue cultured in our laboratory. A titration in filtered natural seawater was also compared with one in an NaCl solution of equal ionic strength. Equilibrium constants for the ionization of water in NaCl solutions as a function of ionic strength were obtained from the literature. Fits to the titration data ([H]T vs. pH) were performed with the FITEQL4.0 computer code using non-electrostatic 3-, 4-, and 5-site models, either by fixing ionic strength at its experimental value or by allowing it to be extrapolated to zero, while considering all functional group pKas and bulk concentrations as adjustable parameters. Since pKas and bulk concentrations were found to be strongly correlated, the latter were also fixed in some cases to further constrain the pKas. Whereas these calculations are currently ongoing, preliminary results point to three, possibly four, functional groups with pKas of about 4.1, 6.3, and 9.5 at I = 0. Bulk concentrations of the three groups are very similar, about 5-6×10-4 mol/g based on dry weight, which suggests that all are homogeneously distributed over the surface and

  11. Titratable acidity of beverages influences salivary pH recovery

    Directory of Open Access Journals (Sweden)

    Livia Maria Andaló TENUTA

    2015-01-01

    Full Text Available A low pH and a high titratable acidity of juices and cola-based beverages are relevant factors that contribute to dental erosion, but the relative importance of these properties to maintain salivary pH at demineralizing levels for long periods of time after drinking is unknown. In this crossover study conducted in vivo, orange juice, a cola-based soft drink, and a 10% sucrose solution (negative control were tested. These drinks differ in terms of their pH (3.5 ± 0.04, 2.5 ± 0.05, and 5.9 ± 0.1, respectively and titratable acidity (3.17 ± 0.06, 0.57 ± 0.04 and < 0.005 mmols OH- to reach pH 5.5, respectively. Eight volunteers with a normal salivary flow rate and buffering capacity kept 15 mL of each beverage in their mouth for 10 s, expectorated it, and their saliva was collected after 15, 30, 45, 60, 90, and 120 s. The salivary pH, determined using a mini pH electrode, returned to the baseline value at 30 s after expectoration of the cola-based soft drink, but only at 90 s after expectoration of the orange juice. The salivary pH increased to greater than 5.5 at 15 s after expectoration of the cola drink and at 30 s after expectoration of the orange juice. These findings suggest that the titratable acidity of a beverage influences salivary pH values after drinking acidic beverages more than the beverage pH.

  12. Modelling of acid-base titration curves of mineral assemblages

    Directory of Open Access Journals (Sweden)

    Stamberg Karel

    2016-01-01

    Full Text Available The modelling of acid-base titration curves of mineral assemblages was studied with respect to basic parameters of their surface sites to be obtained. The known modelling approaches, component additivity (CA and generalized composite (GC, and three types of different assemblages (fucoidic sandstones, sedimentary rock-clay and bentonite-magnetite samples were used. In contrary to GC-approach, application of which was without difficulties, the problem of CA-one consisted in the credibility and accessibility of the parameters characterizing the individual mineralogical components.

  13. Determination of concentration and molar absorptivity of hypochlorous acid and hypobromous acid species by hydrogen peroxide titration

    Science.gov (United States)

    Uehara, H.; Arakaki, T.

    2017-12-01

    Hypochlorous acid and hypobromous acid (abbreviated as "HypoX acids") are the main ingredients of bleaching and bactericides. The HypoX acids change their chemical forms depending on environmental factors such as pH and various chemical reactions. For example, it has been reported that hypobromite ion in water changes to carcinogenic bromate by photochemical reaction with ultraviolet light. In this study, concentrations of HypoX acids were determined by UV-VIS absorbance measurement utilizing the fact that HypoX acids react with hydrogen peroxide and do not co-exist in the solution. The method for determining the concentration by titration with hydrogen peroxide can be carried out simpler and more efficiently than the DPD method or the current titration method generally used for chlorine concentration measurement. Molar absorptivity between 250 - 500 nm of HypoX acids, including their conjugate base species, was determined by solving theoretical acid-base formula including molar fraction of each chemical species at various pHs. Molar absorptivity of OCl- and OBr- between 250 - 500 nm was determined based on the concentrations obtained from titration with hydrogen peroxide and absorbance at pH > 10, where OCl- and OBr- dominate. Furthermore, the HypoX acids solutions were irradiated with a solar simulator, and the photolysis rate constants were obtained. Based on those values, the half-lives were calculated and the behavior of HypoX acids in the environment was elucidated.

  14. Evaluation of inductive heating energy of ITER toroidal field conductor by calorimetry

    Science.gov (United States)

    Ozeki, H.; Suwa, T.; Saito, T.; Matsui, K.; Isono, T.; Kawano, K.; Takahashi, Y.

    2017-05-01

    The influence of a fast electromagnetic perturbation, such as plasma disruption, on the ITER toroidal field (TF) coil conductor was studied. When a fast magnetic field change is superimposed, the TF conductor is inductively heated by internally generated eddy currents. To measure the inductive heating (IH) energy amount by calorimetry, an IH experiment using short TF conductor samples with length of 20 cm was performed in a liquid He bath. The sample components used were a TF conductor, TF jacket and a TF conductor cable. A 60-turn, single layer solenoid coil was installed around each sample as an IH coil. Also, the Joule heat of the IH coil was solely measured to subtract its thermal contribution from the other samples. A 1 kHz sinusoidal AC current was applied to each IH coil, changing the current amplitude. The heat generated in the samples, including the IH coil, was eventually absorbed into the liquid He, and the liquid He was then vaporized. Thus, the heat amount was measured by a He level sensor inside a gas collection cylinder attached above the sample. The validity of the experimental results was confirmed by comparing them with computation results of the IH energy of the samples with a computation model. Also, the consumed energy was calculated from the measured waveforms of the applied AC voltage and current to the samples. As the result, the measured and calculated IH energy were found to be in good agreement. Finally, based on the results of the experiment, the minimum magnetic field strength, which triggers quench of the TF conductor by fast dumping like plasma disruption, was evaluated using estimated TF conductor minimum quench energy.

  15. The relationship between turgor pressure and titratable acidity in mesophyll cells of intact leaves of a Crassulacean-acid-metabolism plant, Kalanchoe daigremontiana Hamet et Perr.

    Science.gov (United States)

    Rygol, J; Winter, K; Zimmermann, U

    1987-12-01

    Day/night changes in turgor pressure (P) and titratable acidity content were investigated in the (Crassulacean-acid-metabolism (CAM) plant Kalanchoe daigremontiana. Measurements of P were made on individual mesophyll cells of intact attached leaves using the pressure-probe technique. Under conditions of high relative humidity, when transpiration rates were minimal, changes in P correlated well with changes in the level of titratable acidity. During the standard 12 h light/12 h dark cycle, maximum turgor pressure (0.15 MPa) occurred at the end of the dark period when the level of titratable acidity was highest (about 300 μeq H(+)·g(-1) fresh weight). A close relationship between P and titratable acidity was also seen in leaves exposed to perturbations of the standard light/dark cycle. (The dark period was either prolonged, or else only CO2-free air was supplied in this period). In plants deprived of irrigation for five weeks, diurnal changes in titratable acidity of the leaves were reduced (ΔH=160 μeq H(+)·g(-1) fresh weight) and P increased from essentially zero at the end of the light period to 0.02 MPa at the end of the dark period. Following more severe water stress (experiments were made on leaves which had been detached for five weeks), P was zero throughout day and night, yet small diurnal changes in titratable acidity were still measured. These findings are discussed in relation to a hypothesis by Lüttge et al. 1975 (Plant Physiol. 56,613-616) for the role of P in the regulation of acidification/de-acidification cycles of plants exhibiting CAM.

  16. Isothermal calorimetry study of calcium caseinate and whey protein isolate edible films cross-linked by heating and gamma-irradiation.

    Science.gov (United States)

    Letendre, M; D'Aprano, G; Delmas-Patterson, G; Lacroix, M

    2002-10-09

    The contribution of thermal and radiative treatments as well as the presence of some excipients, namely glycerol, carboxymethylcellulose (CMC), pectin, and agar, on the formation of protein-protein interactions as well as the formation and loss of protein-water interactions was investigated by means of differential scanning calorimetry in an isothermal mode. Protein-water interactions were assessed through measurement of the heat of the wetting parameter. Isothermal calorimetry measurements pointed out that gamma-irradiation does not favor protein-water interactions, as reflected by its endothermic contribution (P biofilm formulations, glycerol generated the most important losses of protein-water interactions, as inferred by its significant (P < or = 0.05) endothermic impact on the heat of wetting values.

  17. Free Software Development. 3. Numerical Description of Soft Acid with Soft Base Titration

    Directory of Open Access Journals (Sweden)

    Lorentz JÄNTSCHI

    2002-12-01

    Full Text Available The analytical methods of qualitative and quantitative determination of ions in solutions are very flexible to automation. The present work is focus on modeling the process of titration and presents a numerical simulation of acid-base titration. A PHP program to compute all iterations in titration process that solves a 3th rank equation to find value of pH for was built and is available through http internet protocol at the address: http://vl.academicdirect.org/molecular_dynamics/ab_titrations/v1.1/ The method allows expressing the value of pH in any point of titration process and permits to observe the equivalence point of titration.

  18. [A double antibody sandwich ELISA based assay for titration of severe fever with thrombocytopenia syndrome virus].

    Science.gov (United States)

    Liu, Lin; Zhang, Quan-Fu; Li, Chuan; Li, Jian-Dong; Jiang, Xiao-Lin; Zhang, Fu-Shun; Wu, Wei; Liang, Mi-Fang; Li, De-Xin

    2013-06-01

    To develop an assay for titration of severe fever with thrombocytopenia syndrome virus (SFTSV) based on double antibody sandwich ELISA. A double antibody sandwich ELISA was developed for detection of SFTSV based on SFTSV nucleocapsid (N) protein specific poly- and monoclonal antibodies, procedures were optimized and evaluated. This ELISA based titration assay was compared with fluorescence assasy and plaque assay based titration method. The results suggested that the titers obtained by ELISA based method are consistent with those obtained by IFA based method (R = 0.999) and the plaque assay titration method (R = 0.949). The novel ELISA based titration method with high sensitivity and specificity is easy to manage and perform, and can overcome the subjectivity associated with result determination of the fluorescence assay and plaque assay based methods. The novel ELISA based titration method can also be applied to high throughput detection.

  19. Ring-shaped Calorimetry Information for a Neural eGamma Identification with ATLAS Detector

    CERN Document Server

    Da Fonseca Pinto, Joao Victor; The ATLAS collaboration; Oliveira Damazio, Denis; Seixas, Jose

    2016-01-01

    \\title{Ring-shaped Calorimetry Information for a Neural e/$\\gamma$ Identification with ATLAS Detector} After the successful operation of the Large Hadron Collider resulting with the discovery of the Higgs boson, a new data-taking period (Run 2) has started. For the first time, collisions are produced with energies of 13 TeV in the centre of mass. It is foreseen the luminosity increase, reaching values as high as $10^{34}cm^{-2}s^{-1}$ yet in 2015. These changes in experimental conditions bring a proper environment for possible new physics key-findings. ATLAS is the largest LHC detector and was designed for general-purpose physics studies. Many potential physics channels have electrons or photons in their final states. For efficient studies on these channels precise measurement and identification of such particles is necessary. The identification task consists of disentangling those particles (signal) from collimated hadronic jets (background). Reported work concerns the identification process based on the cal...

  20. Morphological Investigation into Starch Bio-Nanocomposites via Synchrotron Radiation and Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    Huihua Liu

    2011-01-01

    Full Text Available We studied a hydrophilic, plasticized bionanocomposite system involving sorbitol plasticizer, amylose biopolymer, and montmorillonite (MMT for the presence of competitive interactions among them at different moisture content. Synchrotron analysis via small angle X-ray scattering (SAXS and thermal analysis using differential scanning calorimetry (DSC were performed to understand crystalline growth and the distribution of crystalline domains within the samples. The SAXS diffraction patterns showed reduced interhelix spacing in the amylose network indicating strong amylose-sorbitol interactions. Depending on the sorbitol and MMT concentration, these interactions also affected the free moisture content and crystalline domains. Domains of around 95 Å and 312 Å were found in the low-moisture-content samples as compared to a single domain of 95 Å in the high-moisture-content samples. DSC measurements confirmed that the MMT increased the onset and the melting temperature of nanocomposites. Moreover, the results showed that the ternary interactions among sorbitol-amylose-MMT supported the crystalline heterogeneity through secondary nucleation.

  1. Magnetocaloric effect in Mn2-pyrazole-[Nb(CN)8] molecular magnet by relaxation calorimetry

    Science.gov (United States)

    Pełka, R.; Gajewski, M.; Miyazaki, Y.; Yamashita, S.; Nakazawa, Y.; Fitta, M.; Pinkowicz, D.; Sieklucka, B.

    2016-12-01

    Magnetocaloric effect in {[Mn(pyrazole)4]2[Nb(CN)8]·4 H2O}n molecular magnet is reported. It crystallizes in tetragonal I41/a space group. The compound exhibits a phase transition to a long range magnetically ordered state at TN ≈ 22.8 K. Temperature dependences of the magnetic entropy change ΔSM as well as the adiabatic temperature change ΔTad due to applied field change μ0 ΔH in the range of 0.1-9 T have been inferred from the relaxation calorimetry measurements. A systematic approximate approach has been used to determine the lattice contribution to the heat capacity. The maximum value of ΔSM for μ0 ΔH = 5 T is 6.83 J mol-1 K-1 (6.65 J kg-1 K-1) at 24.3 K. The corresponding maximum value of ΔTad is 1.4 K at 23.8 K. The temperature dependence of the exponent n characterizing the field dependence of ΔSM has been estimated. It attains the value of 0.64 at the transition temperature, which is consistent with the 3D Heisenberg universality class. A hitherto unobserved two-peak structure has been revealed in the temperature dependence of ΔTad.

  2. Accurate temperature model for absorptance determination of optical components with laser calorimetry.

    Science.gov (United States)

    Wang, Yanru; Li, Bincheng

    2011-03-20

    In the international standard (International Organization for Standardization 11551) for measuring the absorptance of optical components (i.e., laser calorimetry), the absorptance is obtained by fitting the temporal behavior of laser irradiation-induced temperature rise to a homogeneous temperature model in which the infinite thermal conductivity of the sample is assumed. In this paper, an accurate temperature model, in which both the finite thermal conductivity and size of the sample are taken into account, is developed to fit the experimental temperature data for a more precise determination of the absorptance. The difference and repeatability of the results fitted with the two theoretical models for the same experimental data are compared. The optimum detection position when the homogeneous model is employed in the data-fitting procedure is also analyzed with the accurate temperature model. The results show that the optimum detection location optimized for a wide thermal conductivity range of 0.2-50W/m·K moves toward the center of the sample as the sample thickness increases and deviates from the center as the radius and irradiation time increase. However, if the detection position is optimized for an individual sample with known sample size and thermal conductivity by applying the accurate temperature model, the influence of the finite thermal conductivity and sample size on the absorptance determination can be fully compensated for by fitting the temperature data recorded at the optimum detection position to the homogeneous temperature model.

  3. SPECIAL CONSIDERATIONS REGARDING WARFARIN DOSE TITRATION IN PATIENTS WITH ATRIAL FIBRILLATION DEPENDING ON CLINICAL FACTORS

    OpenAIRE

    E. L. Artanova; E. V. Saleeva; I. M. Sokolov; Y. G. Shvarts

    2011-01-01

    Aim. To study the relations of clinical characteristics and individual warfarin dose titration in patients with atrial fibrillation. Material and methods. Period of warfarin dose titration was analyzed in 68 patients with atrial fibrillation due to ischemic heart disease. Adjusted warfarin dose in milligram, duration of dose titration in days and maximal international normalized ratio (INR) were taken into account. Sex, age, history of myocardial infarction and stroke, concomitant diseases, a...

  4. Potentiometric titration of molybdenum (6) with a cathode-polarized solid electrode

    International Nuclear Information System (INIS)

    Boeva, L.V.; Kimstach, V.A.; Bagdasarov, K.N.

    1980-01-01

    The possibility has been studied of using solid electrodes for potentiometric precipitation titration of molybdenum (6). A cathode-polarized electrode, electrochemically covered with a molybdenum blue layer, can be used as indicator electrode. The best results were obtained during deposition of molybdenum blue on a tungsten electrode. The mechanism of electrode work during titration has been investigated. A procedure has been developed of titration of molybdenum (6) in acid solutions using hydroxylamine N-aryl derivatives as titrants

  5. Thermometric Titration for Rapid Determination of Trace Water in Jet Fuel

    OpenAIRE

    Jian-Qiang Hu; Jian-Jian Zhang; Shi-Zhao Yang; Yong-Liang Xin; Li Guo; Ting Yao

    2017-01-01

    Water content in jet fuels is detected by thermometric titration (TMT), and the optimal detected system is 2,2-dimethoxypropane as titrant, cyclohexane and isopropanol as titration solvents, and methanesulfonic acid as catalyst in this method. The amounts of oil, concentration and delivery rate of titrant, volumes, and the reliability and accuracy of thermometric titration were emphasized. The results show that the accuracy, validity, and reliability of TMT are excellent by different indicate...

  6. Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

    OpenAIRE

    Eva Tavčar; Erika Turk; Samo Kreft

    2012-01-01

    The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes p...

  7. New developments in calorimetry and thermal analysis above 2000 °C

    Science.gov (United States)

    Navrotsky, A.; Ushakov, S.; Kapush, D.; Pavlik, A.; Fyhrie, M.

    2016-12-01

    Thermochemical and structural data above 2000 °C for many refractory oxides, including those of the rare earths, are largely absent. Fusion enthalpies are essential for modeling igneous processes, as are volume changes and enthalpies of high temperature phase transitions . The following set of new experimental techniques has been developed for high temperature studies: i) A commercial ultra-high-temperature differential thermal analyzer (DTA)was modified for use to 2500 °C with sealed crucibles and enthalpies of fusion for La2O3 X-phase (78 kJ/mol at 2300 °C), LaAlO3 perovskite (124 kJ/mol at 2134 °C), MgAl2O4 spinel (180 kJ/mol at 2113 °C) were successfully measured. ii) X-ray and neutron diffraction on crystalline laser heated levitated samples has been used to obtain thermal expansion, refine high temperature crystal structure and for in situ study of phase transitions and melting in variable atmospheres using levitators at the Advanced Photon Source and the Spallation Neutron Source. Pre-melting phase transitions in Y2O3, Ho2O3 and Er2O3 from cubic bixbyite-type structures to disordered hexagonal phases are accompanied by 3-4 % decrease in volume. iii) Drop-and-catch (DnC) calorimetry on laser heated aerodynamically levitated samples was developed to allow direct measurement of fusion enthalpies in various atmospheres. The DnC technique was validated by measurement of fusion enthalpy of Al2O3 corundum (120 kJ/mol at 2054 °C) and used to measure fusion enthalpy of cubic bixbyite type Y2O3 (119 kJ/mol at 2430 °C) and Yb2O3 (97 kJ/mol at 2435 °C). Further methodologiccal improvements and applications to earth and planetary materials are discussed.

  8. Use of Indirect Calorimetry to Detect Overfeeding in Critically Ill Children: Finding the Appropriate Definition.

    Science.gov (United States)

    Kerklaan, Dorian; Hulst, Jessie M; Verhoeven, Jennifer J; Verbruggen, Sascha C A T; Joosten, Koen F M

    2016-10-01

    Overfeeding during critical illness is associated with adverse effects such as metabolic disturbances and increased risk of infection. Because of the lack of sound studies with clinical endpoints, overfeeding is arbitrarily defined as the ratio caloric intake/measured resting energy expenditure (mREE) or alternatively as a comparison of measured respiratory quotient (RQ) to the predicted RQ based on the macronutrient intake (RQmacr). We aimed to compare definitions of overfeeding in critically ill mechanically ventilated children based on mREE, RQ, and caloric intake to find an appropriate definition. Indirect calorimetry measurements were performed in 78 mechanically ventilated children, median age 6.3 months. Enteral and/or parenteral nutrition was provided according to the local guidelines. Definitions used to indicate overfeeding were the ratio caloric intake/mREE of >110% and >120% and by the measured RQ > RQmacr + 0.05. The proportion of patients identified as overfed varied widely depending on the definition used, ranging from 22% (RQ > RQmacr + 0.05), to 40% and 50% (caloric intake/mREE of >120% and >110%, respectively). Linear regression analysis showed that all patients would be identified as overfed with the definition RQ > RQmacr + 0.05 when the ratio caloric intake/mREE exceeded 165%. Caloric intake was higher in children with a standard deviation-score weight for age definition applied. These currently used definitions fail to take into account several relevant factors affecting metabolism during critical illness and are therefore not generally applicable to the pediatric intensive care unit population.

  9. Fast Proton Titration Scheme for Multiscale Modeling of Protein Solutions.

    Science.gov (United States)

    Teixeira, Andre Azevedo Reis; Lund, Mikael; da Silva, Fernando Luís Barroso

    2010-10-12

    Proton exchange between titratable amino acid residues and the surrounding solution gives rise to exciting electric processes in proteins. We present a proton titration scheme for studying acid-base equilibria in Metropolis Monte Carlo simulations where salt is treated at the Debye-Hückel level. The method, rooted in the Kirkwood model of impenetrable spheres, is applied on the three milk proteins α-lactalbumin, β-lactoglobulin, and lactoferrin, for which we investigate the net-charge, molecular dipole moment, and charge capacitance. Over a wide range of pH and salt conditions, excellent agreement is found with more elaborate simulations where salt is explicitly included. The implicit salt scheme is orders of magnitude faster than the explicit analog and allows for transparent interpretation of physical mechanisms. It is shown how the method can be expanded to multiscale modeling of aqueous salt solutions of many biomolecules with nonstatic charge distributions. Important examples are protein-protein aggregation, protein-polyelectrolyte complexation, and protein-membrane association.

  10. Semi-automated potentiometric titration method for uranium characterization

    Energy Technology Data Exchange (ETDEWEB)

    Cristiano, B.F.G., E-mail: barbara@ird.gov.br [Comissao Nacional de Energia Nuclear (CNEN), Instituto de Radioprotecao e Dosimetria (IRD), Avenida Salvador Allende s/n Recreio dos Bandeirantes, PO Box 37750, Rio de Janeiro, 22780-160 RJ (Brazil); Delgado, J.U.; Silva, J.W.S. da; Barros, P.D. de; Araujo, R.M.S. de [Comissao Nacional de Energia Nuclear (CNEN), Instituto de Radioprotecao e Dosimetria (IRD), Avenida Salvador Allende s/n Recreio dos Bandeirantes, PO Box 37750, Rio de Janeiro, 22780-160 RJ (Brazil); Lopes, R.T. [Programa de Engenharia Nuclear (PEN/COPPE), Universidade Federal do Rio de Janeiro (UFRJ), Ilha do Fundao, PO Box 68509, Rio de Janeiro, 21945-970 RJ (Brazil)

    2012-07-15

    The manual version of the potentiometric titration method has been used for certification and characterization of uranium compounds. In order to reduce the analysis time and the influence of the analyst, a semi-automatic version of the method was developed in the Brazilian Nuclear Energy Commission. The method was applied with traceability assured by using a potassium dichromate primary standard. The combined standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization. - Highlights: Black-Right-Pointing-Pointer We developed a semi-automatic version of potentiometric titration method. Black-Right-Pointing-Pointer The method is used for certification and characterization of uranium compounds. Black-Right-Pointing-Pointer The traceability of the method was assured by a K{sub 2}Cr{sub 2}O{sub 7} primary standard. Black-Right-Pointing-Pointer The results of U{sub 3}O{sub 8} reference material analyzed was consistent with certified value. Black-Right-Pointing-Pointer The uncertainty obtained, near 0.01%, is useful for characterization purposes.

  11. Common Standards of Basal Insulin Titration in T2DM

    Science.gov (United States)

    Arnolds, Sabine; Heise, Tim; Flacke, Frank; Sieber, Jochen

    2013-01-01

    Type 2 diabetes mellitus has become a worldwide major health problem, and the number of people affected is steadily increasing. Thus, not all patients suffering from the disease can be treated by specialized diabetes centers or outpatient clinics, but by primary care physicians. The latter, however, might have time constraints and have to deal with many kinds of diseases or with multimorbid patients, so their focus is not so much on lowering high blood glucose values. Thus, the physicians, as well as the patients themselves, are often reluctant to initiate and adjust insulin therapy, although basal insulin therapy is considered the appropriate strategy after oral antidiabetic drug failure, according to the latest international guidelines. A substantial number of clinical studies have shown that insulin initiation and optimization can be managed successfully by using titration algorithms—even in cases where patients themselves are the drivers of insulin titration. Nevertheless, tools and strategies are needed to facilitate this process in the daily life of both primary health care professionals and patients with diabetes. PMID:23759411

  12. Subject-driven titration of biphasic insulin aspart 30 twice daily is non-inferior to investigator-driven titration in Chinese patients with type 2 diabetes inadequately controlled with premixed human insulin: A randomized, open-label, parallel-group, multicenter trial.

    Science.gov (United States)

    Yang, Wenying; Zhu, Lvyun; Meng, Bangzhu; Liu, Yu; Wang, Wenhui; Ye, Shandong; Sun, Li; Miao, Heng; Guo, Lian; Wang, Zhanjian; Lv, Xiaofeng; Li, Quanmin; Ji, Qiuhe; Zhao, Weigang; Yang, Gangyi

    2016-01-01

    The present study was to compare the efficacy and safety of subject-driven and investigator-driven titration of biphasic insulin aspart 30 (BIAsp 30) twice daily (BID). In this 20-week, randomized, open-label, two-group parallel, multicenter trial, Chinese patients with type 2 diabetes inadequately controlled by premixed/self-mixed human insulin were randomized 1:1 to subject-driven or investigator-driven titration of BIAsp 30 BID, in combination with metformin and/or α-glucosidase inhibitors. Dose adjustment was decided by patients in the subject-driven group after training, and by investigators in the investigator-driven group. Eligible adults (n = 344) were randomized in the study. The estimated glycated hemoglobin (HbA1c) reduction was 14.5 mmol/mol (1.33%) in the subject-driven group and 14.3 mmol/mol (1.31%) in the investigator-driven group. Non-inferiority of subject-titration vs investigator-titration in reducing HbA1c was confirmed, with estimated treatment difference -0.26 mmol/mol (95% confidence interval -2.05, 1.53) (-0.02%, 95% confidence interval -0.19, 0.14). Fasting plasma glucose, postprandial glucose increment and self-measured plasma glucose were improved in both groups without statistically significant differences. One severe hypoglycemic event was experienced by one subject in each group. A similar rate of nocturnal hypoglycemia (events/patient-year) was reported in the subject-driven (1.10) and investigator-driven (1.32) groups. There were 64.5 and 58.1% patients achieving HbA1c titration of BIAsp 30 BID was as efficacious and well-tolerated as investigator-titration. The present study supported patients to self-titrate BIAsp 30 BID under physicians' supervision.

  13. Ruthenium determination in new composite materials by coulometric titration with generated iron(2)

    International Nuclear Information System (INIS)

    Butakova, N.A.; Oganesyan, L.B.

    1983-01-01

    A coulometric technique is developed for ruthenium (4) titration with generated iron (2) in a mixture of hydrochloric-, sulfuric- and phosphoric acids with potentiometric and biammetric indication of the final titration point. Bi (3), Pd (2), Nb (5), Pt (4) Pb (2), Rh (3) do not interfere with the titration. Together with Ru (4) titrated are Ir (4), V (5), Au (3). The method is applied to analyze commercial samples of ruthenium dioxides, lead- and bismuth ruthenites, ruthenium pentafluorides containing 30-80% of ruthenium. The Ssub(r) values do not exceed 0.002

  14. The role of titration schedule of topiramate for the development of depression in patients with epilepsy.

    Science.gov (United States)

    Mula, Marco; Hesdorffer, Dale C; Trimble, Michael; Sander, Josemir W

    2009-05-01

    To determine whether a fast titration schedule of topiramate (TPM) has different effects on the occurrence of depression, in relation to other risk factors for TPM-induced depression, including history of depression (HxDEP), febrile seizures (FS), and hippocampal sclerosis (HS). Using data from a large case registry of patients prescribed TPM, two models were constructed: Model 1 examined the independent effect of rapid TPM titration after separate adjustment for FS, HxDEP, and HS. Model 2 examined effect of the cooccurrence of rapid titration on the development of depression with each of these risk factors. A total of 423 patients were included (51.8% females), mean age (SD) 35.5 (11.8) years, mean duration of epilepsy of 22.2 (11.5) years. Forty-four patients (10.4%) developed depression during TPM therapy. A rapid TPM titration was associated with 5-fold increased risk of depression that increased to 12.7-fold in the presence of both FS and rapid TPM titration, 23.3-fold in the presence of both HxDEP and rapid TPM titration, and 7.6-fold in the presence of both HS and rapid TPM titration schedule. Our study suggests that a rapid titration schedule is associated with an increased risk of developing depression during TPM therapy. HxDEP and FS are major contraindications to the use of a rapid titration, with a 23.3-fold and 12.7 fold increased risk, respectively.

  15. Method for linearizing the potentiometric curves of precipitation titration in nonaqueous and aqueous-organic solutions

    International Nuclear Information System (INIS)

    Bykova, L.N.; Chesnokova, O.Ya.; Orlova, M.V.

    1995-01-01

    The method for linearizing the potentiometric curves of precipitation titration is studied for its application in the determination of halide ions (Cl - , Br - , I - ) in dimethylacetamide, dimethylformamide, in which titration is complicated by additional equilibrium processes. It is found that the method of linearization permits the determination of the titrant volume at the end point of titration to high accuracy in the case of titration curves without a potential jump in the proximity of the equivalent point (5 x 10 -5 M). 3 refs., 2 figs., 3 tabs

  16. [Comparison of different continuous positive airway pressure titration methods for obstructive sleep apnea hypopnea syndrome].

    Science.gov (United States)

    Li, Jingjing; Ye, Jingying; Zhang, Peng; Kang, Dan; Cao, Xin; Zhang, Yuhuan; Ding, Xiu; Zheng, Li; Li, Hongguang; Bian, Qiuli

    2014-10-01

    To explore whether there were differences between the results of automatic titration and the results of manual titration for positive airway pressure treatment in patients with obstructive sleep apnea hypopnea syndrome (OSAHS) and its influencing factors, the results might provide a theoretical basis for the rational use of two pressure titration methods. Sixty one patients with OSAHS were included in this study. All patients underwent a manual titration and an automatic titration within one week. The clinical informations, polysomnography data, and the results of both two titration of all patients were obtained for analysis. The overall apnea/hypopnea index was (63.1 ± 17.7)/h, with a range of 14.9/h to 110.4/h. The treatment pressure of manual titration was (8.4 ± 2.1) cmH(2)O, which was significantly lower than the treatment pressure of automatic titration, (11.5 ± 2.7) cmH(2)O (t = -9.797, P titration and manual titration), it was found that the pressure of automatic titration was significantly higher in patients with a ΔP > 3 cmH(2)O than in patients with a ΔP ≤ 3 cmH(2)O, which was (13.3 ± 2.3) cmH(2)O vs (10.0 ± 2.0) cmH(2)O (t = -6.159, P titration between these two groups, which was (8.6 ± 2.4) cmH(2)O vs (8.3 ± 2.0)cmH(2)O (P > 0.05). There was no significant difference in age, body mass index, neck circumference, abdomen circumference, apnea hypopnea index, and arterial oxygen saturation between these two groups. The treatment pressure of automatic titration is usually higher than that of manual titration. For patients with a high treatment pressure which is derived from automatic titration, a suggestion about manual titration could be given to decrease the potential treatment pressure of continuous positive airway pressure, which may be helpful in improving the comfortableness and the compliance of this treatment.

  17. A nine-point pH titration method to determine low-concentration VFA in municipal wastewater.

    Science.gov (United States)

    Ai, Hainan; Zhang, Daijun; Lu, Peili; He, Qiang

    2011-01-01

    Characterization of volatile fatty acid (VFA) in wastewater is significant for understanding the wastewater nature and the wastewater treatment process optimization based on the usage of Activated Sludge Models (ASMs). In this study, a nine-point pH titration method was developed for the determination of low-concentration VFA in municipal wastewater. The method was evaluated using synthetic wastewater containing VFA with the concentration of 10-50 mg/l and the possible interfering buffer systems of carbonate, phosphate and ammonium similar to those in real municipal wastewater. In addition, the further evaluation was conducted through the assay of real wastewater using chromatography as reference. The results showed that the recovery of VFA in the synthetic wastewater was 92%-102 and the coefficient of variance (CV) of reduplicate measurements 1.68%-4.72%. The changing content of the buffering substances had little effect on the accuracy of the method. Moreover, the titration method was agreed with chromatography in the determination of VFA in real municipal wastewater with R(2)= 0.9987 and CV =1.3-1.7. The nine-point pH titration method is capable of satisfied determination of low-concentration VFA in municipal wastewater.

  18. Evaluation of the amorphous content of lactose by solution calorimetry and Raman spectroscopy.

    Science.gov (United States)

    Katainen, Erja; Niemelä, Pentti; Harjunen, Päivi; Suhonen, Janne; Järvinen, Kristiina

    2005-11-15

    Solution calorimetry can be used to determine the amorphous content of a compound when the solubility and dissolution rate of the compound in the chosen solvent are reasonably high. Sometimes, it can be difficult find a solvent in which a sample is freely soluble. The present study evaluated the use of solution calorimetry for the assessment of the amorphous content of a sample that is poorly soluble in a solvent. Physical mixtures of lactose and spray-dried lactose samples (the amorphous content varied from 0 to 100%) were analyzed by a solution calorimeter and the results were compared with Raman spectroscopy determinations. The heat of solvation of the samples was determined by solution calorimetry in organic solvents MeOH, EtOH, ACN, THF, acetone (400mg sample/100ml solvent). Lactose is virtually insoluble in ACN, THF and acetone and very slightly soluble in EtOH and MeOH. The amorphous content of the samples could not be determined by solution calorimetry in EtOH, ACN, THF or acetone. However, an excellent correlation was observed between the heat of solvation and the amorphous content of the samples in MeOH. Furthermore, the heat of solvation values of the samples in MeOH showed a linear correlation with the Raman quantifications. Therefore, our results demonstrate that solution calorimetry may represent a rapid and simple method for determining the amorphous content also in samples that are not freely soluble in the solvent.

  19. Chemical processes at the surface of various clays on acid-base titration

    International Nuclear Information System (INIS)

    Park, K. K.; Park, Y. S.; Jung, E. C.

    2010-01-01

    The chemical reaction of radionuclides at the interface between groundwater and geological mineral is an important process determining their retardation of transport through groundwater flow in a nuclear waste disposal. Clay minerals are major components of soil and argillaceous rock, and some of them are considered to be important base materials in the design of high-level nuclear waste repository due to their large swelling, low-permeability, large surface area, and strong and large sorption of radionuclides. Clay materials are phyllosilicates containing accessory minerals such as metal oxides, hydroxides, oxyhydroxides. Their structures are condensed 1:1 or 2:1 layers of tetrahedral SiO 3/2 OH and octahedral Al(OH) 6/2 sheets. An accurate knowledge about the properties of clay surface is required as a parameter for a long-term estimation of radionuclide retardation effects. Electric surface charge is a primary property determining ion exchange and surface complexation of radionuclides on its surface. The sources of electric surface charge are a permanent structural negative charge on a basal plane and a dissociable charge at an edge surface. Investigation of proton sorption is a prerequisite to the understanding of radionuclide sorption. The reactions on a permanently charged site and on an edge site are measured by an electrokinetic measurement and by potentiometric titration, respectively. However, side reactions such as complexation, proton/cation exchange, dissolution, hydrolysis, precipitation and re adsorption, and the reaction of secondary minerals hinder an experimental measurement of accurate acid-base properties. This presentation describes the pH change on dispersing various clays in water and adding acid, base or Eu(III) ion to these solutions, and the effect of Eu(III) ion on acid-base titration of clay solutions

  20. Noble Liquid (Xenon or Krypton) Totally Active Calorimetry

    CERN Multimedia

    2002-01-01

    Main Goals\\\\ \\\\ Determine ionization and scintillation yields in liquid Xenon (LXe) or Krypton.\\\\ \\\\ Determine the electron lifetime and photon mean free path in LXe or LKr. \\\\ \\\\ Determine energy resolution of LXe or LKr via ionization or scintillation.\\\\ \\\\ Determine correlation of fluctuations between ionization and scintillation. Summary of Results \\\\ \\\\ -~measured the electron lifetime in LXe, ($\\tau$~$>$~400 $\\mu$s).\\\\ \\\\ -~measured the energy to create an ionization electron in LXe, W=9.8 eV.\\\\ \\\\ -~measured the energy to create a LXe scintillation photon, W$ _{s} $~=~14.2~eV. \\\\ \\\\ -~measured the anticorrelation of scintillation and ionization yields. \\\\ \\\\ -~measured the energy resolution in LXe via ionization, $ sigma _{E} / $E=0.07\\%/$\\sqrt$E(GeV). \\\\ \\\\ -~measured resolution in LXe via scintillation $ sigma _{E} / $E=0.24\\%/$\\sqrt$E(GeV)+0.26\\%. \\\\ \\\\ -~measured electron drift velocity in LXe:~neat (2.5 mm/$\\mu$s), doped (4.4~mm/$\\mu$s). \\\\ \\\\ -~measured the photon mean free path in LXe vs $ lambd...