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...

pytc: Open-Source Python Software for Global Analyses of Isothermal Titration Calorimetry Data.

Science.gov (United States)

Duvvuri, Hiranmayi; Wheeler, Lucas C; Harms, Michael J

2018-05-08

Here we describe pytc, an open-source Python package for global fits of thermodynamic models to multiple isothermal titration calorimetry experiments. Key features include simplicity, the ability to implement new thermodynamic models, a robust maximum likelihood fitter, a fast Bayesian Markov-Chain Monte Carlo sampler, rigorous implementation, extensive documentation, and full cross-platform compatibility. pytc fitting can be done using an application program interface or via a graphical user interface. It is available for download at https://github.com/harmslab/pytc .

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

Comparison of calorimetry and destructive analytical measurement techniques for excess plutonium powders

International Nuclear Information System (INIS)

Welsh, T.L.

1996-01-01

In Dec. 1994, IAEA safeguards were initiated on inventory of Pu- bearing materials, originating from the US nuclear weapons complex, at vault 3 of DOE's Plutonium Finishing Plant at Hanford. Because of the diversity and heterogeneity of the Pu, plant operators have increasingly used calorimetry for accountability measurements. During the recent commencement of IAEA safeguards at vault 3, destructive (electrochemical titration) methods were used to determine Pu concentrations in subsamples of inventory items with widely ranging chemical purities. The Pu concentrations in the subsamples were determined and contribution of heterogeneity to total variability was identified. Measurement results, gathered by PFP and IAEA laboratories, showed total measurement variability for calorimetry to be comparable with or lower than those of sampling and chemical analyses

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.

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.

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.

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

International Nuclear Information System (INIS)

Taube, F.; Drobot, B.; Acker, M.; Taut, S.; Stumpf, Thorsten

2017-01-01

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.

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.

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...

Biomolecule-nanoparticle interactions: Elucidation of the thermodynamics by isothermal titration calorimetry.

Science.gov (United States)

Huang, Rixiang; Lau, Boris L T

2016-05-01

Nanomaterials (NMs) are often exposed to a broad range of biomolecules of different abundances. Biomolecule sorption driven by various interfacial forces determines the surface structure and composition of NMs, subsequently governs their functionality and the reactivity of the adsorbed biomolecules. Isothermal titration calorimetry (ITC) is a nondestructive technique that quantifies thermodynamic parameters through in-situ measurement of the heat absorption or release associated with an interaction. This review highlights the recent applications of ITC in understanding the thermodynamics of interactions between various nanoparticles (NPs) and biomolecules. Different aspects of a typical ITC experiment that are crucial for obtaining accurate and meaningful data, as well as the strengths, weaknesses, and challenges of ITC applications to NP research were discussed. ITC reveals the driving forces behind biomolecule-NP interactions and the effects of the physicochemical properties of both NPs and biomolecules by quantifying the crucial thermodynamics parameters (e.g., binding stoichiometry, ΔH, ΔS, and ΔG). Complimentary techniques would strengthen the interpretation of ITC results for a more holistic understanding of biomolecule-NP interactions. The thermodynamic information revealed by ITC and its complimentary characterizations is important for understanding biomolecule-NP interactions that are fundamental to the biomedical and environmental applications of NMs and their toxicological effects. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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+.

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.

Titration calorimetry of anesthetic-protein interaction: negative enthalpy of binding and anesthetic potency.

Science.gov (United States)

Ueda, I; Yamanaka, M

1997-04-01

Anesthetic potency increases at lower temperatures. In contrast, the transfer enthalpy of volatile anesthetics from water to macromolecules is usually positive. The transfer decreases at lower temperature. It was proposed that a few selective proteins bind volatile anesthetics with negative delta H, and these proteins are involved in signal transduction. There has been no report on direct estimation of binding delta H of anesthetics to proteins. This study used isothermal titration calorimetry to analyze chloroform binding to bovine serum albumin. The calorimetrically measured delta H cal was -10.37 kJ.mol-1. Thus the negative delta H of anesthetic binding is not limited to signal transduction proteins. The binding was saturable following Fermi-Dirac statistics and is characterized by the Langmuir adsorption isotherms, which is interfacial. The high-affinity association constant, K, was 2150 +/- 132 M-1 (KD = 0.47 mM) with the maximum binding number, Bmax = 3.7 +/- 0.2. The low-affinity K was 189 +/- 3.8 M-1 (KD = 5.29 mM), with a Bmax of 13.2 +/- 0.3. Anesthetic potency is a function of the activity of anesthetic molecules, not the concentration. Because the sign of delta H determines the temperature dependence of distribution of anesthetic molecules, it is irrelevant to the temperature dependence of anesthetic potency.

Understanding binding affinity : A combined isothermal titration calorimetry/molecular dynamics study of the binding of a series of hydrophobically modified benzamidinium chloride inhibitors to trypsin

NARCIS (Netherlands)

Talhout, Reinskje; Villa, Alessandra; Mark, AE; Engberts, JBFN

2003-01-01

The binding of a series of p-alkylbenzamidinium chloride inhibitors to the serine proteinase trypsin over a range of temperatures has been studied using isothermal titration (micro)calorimetry and molecular dynamics simulation techniques. The inhibitors have small structural variations at the para

Application of a new method for data analysis of isothermal titration calorimetry in the interaction between human serum albumin and Ni{sup 2+}[Serum albumin; Nickel; Isothermal titration calorimetry; Calorimetric method

Energy Technology Data Exchange (ETDEWEB)

Saboury, Ali Akbar. E-mail: saboury@chamran.ut.ac.ir

2003-12-01

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 ({delta}H=-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 {mu}M{sup -1})

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

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.

Van ‘t Hoff global analyses of variable temperature isothermal titration calorimetry data

International Nuclear Information System (INIS)

Freiburger, Lee A.; Auclair, Karine; Mittermaier, Anthony K.

2012-01-01

Highlights: ▶ We developed a global fitting strategy for ITC data collected at multiple temperatures. ▶ This method does not require prior knowledge of the binding mechanism. ▶ Monte Carlo simulations show that the approach improves the accuracy of extracted thermodynamic parameters. ▶ The method is used to study coupled folding/binding in aminoglycoside 6′-N-acetyltransferase-Ii. - Abstract: Isothermal titration calorimetry (ITC) can provide detailed information on the thermodynamics of biomolecular interactions in the form of equilibrium constants, K A , and enthalpy changes, ΔH A . A powerful application of this technique involves analyzing the temperature dependences of ITC-derived K A and ΔH A values to gain insight into thermodynamic linkage between binding and additional equilibria, such as protein folding. We recently developed a general method for global analysis of variable temperature ITC data that significantly improves the accuracy of extracted thermodynamic parameters and requires no prior knowledge of the coupled equilibria. Here we report detailed validation of this method using Monte Carlo simulations and an application to study coupled folding and binding in an aminoglycoside acetyltransferase enzyme.

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.

Evaluation of Staphylococcus aureus DNA aptamer by enzyme-linked aptamer assay and isothermal titration calorimetry.

Science.gov (United States)

Bayraç, Ceren; Öktem, Hüseyin Avni

2017-02-01

To monitor the specificity of Staphylococcus aureus aptamer (SA-31) against its target cell, we used enzyme-linked aptamer assay. In the presence of target cell, horseradish peroxidase-conjugated streptavidin bound to biotin-labeled SA-31 showed specific binding to S  aureus among 3 different bacteria with limit of detection of 10 3 colony-forming unit per milliliter. The apparent K a was 1.39 μM -1  ± 0.3 μM -1 . The binding of SA-31 to membrane proteins extracted from cell surface was characterized using isothermal titration calorimetry, and the effect of changes in binding temperature and salt concentrations of binding buffer was evaluated based on thermodynamic parameters (K a , ΔH, and ΔG). Since binding of aptamer to its targets solely depends on its 3-dimensional structure under experimental conditions used in selection process, the change in temperature and ion concentration changed the affinity of SA-31 to its target on surface of bacteria. At 4°C, SA-31 did not show an affinity to its target with poor heat change upon injection of membrane fraction to aptamer solution. However, the apparent association constants of SA-31 slightly varied from K a  = 1.56 μM -1  ± 0.69 μM -1 at 25°C to K a  = 1.03 μM -1  ± 0.9 μM -1 at 37°C. At spontaneously occurring exothermic binding reactions, affinities of S aureus aptamer to its target were also 9.44 μM -1  ± 0.38 μM -1 at 50mM, 1.60 μM -1  ± 0.11 μM -1 at 137mM, and 3.28 μM -1  ± 0.46 μM -1 at 200 mM of salt concentration. In this study, it was demonstrated that enzyme-linked aptamer assay and isothermal titration calorimetry were useful tools for studying the fundamental binding mechanism between a DNA aptamer and its target on the outer surface of S aureus. Copyright © 2016 John Wiley & Sons, Ltd.

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

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.

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

2016-01-15

Steady-state and time-resolved fluorescence quenching measurements supported by Isothermal Titration Calorimetry (ITC) were used to study the interactions of Cu(2+) 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 298.15K in 20mM 2-(N-morpholino)ethanesulfonic acid (MES) buffer solution with a pH of 6. The fluorescence of all peptides was quenched by Cu(2+) ions. The stoichiometry, conditional stability constants and thermodynamic parameters for the interactions of the Cu(2+) 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 Cu(2+) ions are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

The use of isothermal titration calorimetry to determine the thermodynamics of metal ion binding to low-cost sorbents

International Nuclear Information System (INIS)

Karlsen, Vigdis; Heggset, Ellinor Baevre; Sorlie, Morten

2010-01-01

The thermodynamics of Al 3+ , Cr 3+ , and Pb 2+ binding to the abundant biopolymer chitin have been determined using isothermal titration calorimetry (ITC) and compared to what is observed for binding to activated carbon. The use of ITC enables the detection of two distinct binding sites on chitin for all three metal ions. For the relative strong binding sites, free energy changes ranges from -37.6 kJ/mol to -41.8 kJ/mol while the same values are from -30.1 kJ/mol to -31.8 kJ/mol for the relative weak binding sites. All binding reactions to chitin are entropically driven. Interactions of the metal ions to activated carbon are best fitted as a single-site binding with relative weak binding with free energy changes from -26.3 kJ/mol to -26.8 kJ/mol.

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.

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.

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...... of experiments showed that weak forces determine precipitation. Indeed, isothermal titration calorimetry could not detect any clear signal although this technique can detect low-energy transitions such as liquid-liquid equilibrium and rnicellization. The second series of tests proved that precipitation caused...... by T and P variations is exothermic for this system. Furthermore, the temperature-induced precipitation is accompanied by an increase in the apparent thermal expansivity. Therefore, it seems that these two phase transitions exhibit different calorimetric behaviours and they may not be as similar...

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...

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

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.

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.

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. 7 refs., 4 figs., 1 tab

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...

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

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 )

Antihypertensive Effects, Molecular Docking Study, and Isothermal Titration Calorimetry Assay of Angiotensin I-Converting Enzyme Inhibitory Peptides from Chlorella vulgaris.

Science.gov (United States)

Xie, Jingli; Chen, Xujun; Wu, Junjie; Zhang, Yanyan; Zhou, Yan; Zhang, Lujia; Tang, Ya-Jie; Wei, Dongzhi

2018-02-14

The aim of this work is to explore angiotensin I-converting enzyme (ACE) inhibitory peptides from Chlorella vulgaris (C. vulgaris) and discover the inhibitory mechanism of the peptides. After C. vulgaris proteins were gastrointestinal digested in silico, several ACE inhibitory peptides with C-terminal tryptophan were screened. Among them, two novel noncompetitive ACE inhibitors, Thr-Thr-Trp (TTW) and Val-His-Trp (VHW), exhibited the highest inhibitory activity indicated by IC 50 values 0.61 ± 0.12 and 0.91 ± 0.31 μM, respectively. Both the peptides were demonstrated stable against gastrointestinal digestion and ACE hydrolysis. The peptides were administrated to spontaneously hypertensive rats (SHRs) in the dose 5 mg/kg body weight, and VHW could decrease 50 mmHg systolic blood pressure of SHRs (p < 0.05). Molecular docking displayed that both TTW and VHW formed six hydrogen bonds with active site pockets of ACE. Besides, isothermal titration calorimetry assay discovered that VHW could form more stable complex with ACE than TTW. Therefore, VHW was an excellent ACE inhibitor.

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.

Tritium inventory measurements by 'in-bed' gas flowing calorimetry

International Nuclear Information System (INIS)

Hayashi, T.; Suzuki, T.; Yamada, M.; Okuno, K.

1996-01-01

In order to establish the 'in-bed' tritium accounting technology for the ITER scale tritium storage system, a gas flowing calorimetry has been studied using a scaled ZrCo bed (25 g tritium capacity). The basic calorimetric characteristics, steady state temperature raise of He gas stream flowing through a secondary coil line fixed in the ZrCo tritide, was measured and correlated with the stored tritium inventory. The results shows that about 4 degrees raise of He stream temperature can be detected for each gram of tritium storage. The sensitivity of this calorimetry is about 0.05 g of tritium, calculated by 0.2 degrees of temperature sensor error. The accuracy is better than 0.25 g of tritium on 25 g storage, evaluated by 2 times of standard deviation from the repeat measurements. This accuracy of < 1% on full storage capacity is satisfied the target accountability to measure ± 1 gram of tritium on 100 g storage for ITER. 13 refs., 7 figs

Tritium inventory measurements using calorimetry

International Nuclear Information System (INIS)

Kapulla, H.; Kraemer, R.; Heine, R.

1992-01-01

In the past calorimetry has been developed as a powerful tool in radiometrology. Calorimetric methods have been applied for the determination of activities, half lives and mean energies released during the disintegration of radioactive isotopes. The fundamental factors and relations which determine the power output of radioactive samples are presented and some basic calorimeter principles are discussed in this paper. At the Kernforschungszentrum Karlsruhe (KfK) a family of 3 calorimeters has been developed to measure the energy release from radiative waste products arising from reprocessing operations. With these calorimeters, radiative samples with sizes from a few cm 3 to 2 ·10 5 cm 3 and heat ratings ranging from a few nW to kW can be measured. After modifications of tits inner part the most sensitive calorimeter among the three calorimeters mentioned above would be best suited for measuring the tritium inventory in T-getters of the Amersham-type

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...

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

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.

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.

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

Microcalorimetric and potentiometric titration studies on the adsorption of copper by extracellular polymeric substances (EPS), minerals and their composites.

Science.gov (United States)

Fang, Linchuan; Huang, Qiaoyun; Wei, Xing; Liang, Wei; Rong, Xinming; Chen, Wenli; Cai, Peng

2010-08-01

Equilibrium adsorption experiments, isothermal titration calorimetry and potentiometric titration techniques were employed to investigate the adsorption of Cu(II) by extracellular polymeric substances (EPS) extracted from Pseudomonas putida X4, minerals (montmorillonite and goethite) and their composites. Compared with predicted values of Cu(II) adsorption on composites, the measured values of Cu(II) on EPS-montmorillonite composite increased, however, those on EPS-goethite composite decreased. Potentiometric titration results also showed that more surface sites were observed on EPS-montmorillonite composite and less reactive sites were found on EPS-goethite composite. The adsorption of Cu(II) on EPS molecules and their composites with minerals was an endothermic reaction, while that on minerals was exothermic. The positive values of enthalpy change (Delta H) and entropy change (DeltaS) for Cu(II) adsorption on EPS and mineral-EPS composites indicated that Cu(II) mainly interacts with carboxyl and phosphoryl groups as inner-sphere complexes on EPS molecules and their composites with minerals. (c) 2010 Elsevier Ltd. All rights reserved.

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...

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.

Strategies for assessing proton linkage to bimolecular interactions by global analysis of isothermal titration calorimetry data

International Nuclear Information System (INIS)

Coussens, Nathan P.; Schuck, Peter; Zhao, Huaying

2012-01-01

Highlights: ► We demonstrate the usefulness of global analysis of ITC data for proton-linked binding study. ► Various experimental strategies are evaluated for their information content. ► Data at multiple temperatures might improve the precision of binding parameters. ► Methods for detailed error analysis of parameter uncertainties are discussed. ► By global modeling, an uncertainty in molecular concentrations can be accounted for. - Abstract: Isothermal titration calorimetry (ITC) is a traditional and powerful method for studying the linkage of ligand binding to proton uptake or release. The theoretical framework has been developed for more than two decades and numerous applications have appeared. In the current work, we explored strategic aspects of experimental design. To this end, we simulated families of ITC data sets that embed different strategies with regard to the number of experiments, range of experimental pH, buffer ionization enthalpy, and temperature. We then re-analyzed the families of data sets in the context of global analysis, employing a proton linkage binding model implemented in the global data analysis platform SEDPHAT, and examined the information content of all data sets by a detailed statistical error analysis of the parameter estimates. In particular, we studied the impact of different assumptions about the knowledge of the exact concentrations of the components, which in practice presents an experimental limitation for many systems. For example, the uncertainty in concentration may reflect imperfectly known extinction coefficients and stock concentrations or may account for different extents of partial inactivation when working with proteins at different pH values. Our results show that the global analysis can yield reliable estimates of the thermodynamic parameters for intrinsic binding and protonation, and that in the context of the global analysis the exact molecular component concentrations may not be required. Additionally

Affinity between TBC1D4 (AS160 phosphotyrosine-binding domain and insulin-regulated aminopeptidase cytoplasmic domain measured by isothermal titration calorimetry

Directory of Open Access Journals (Sweden)

SangYoun Park*, Keon Young Kim, Sunmin Kim & Young Seok Yu

2012-06-01

Full Text Available Uptake of circulating glucose into the cells happens via the insulin-mediated signalling pathway, which translocates the glucosetransporter 4 (GLUT4 vesicles from the intracellular compartmentto the plasma membrane. RabㆍGTPases are involvedin this vesicle trafficking, where RabㆍGTPase-activatingproteins (RabGAP enhance the GTP to GDP hydrolysis.TBC1D4 (AS160 and TBC1D1 are functional RabGAPs in theadipocytes and the skeletonal myocytes, respectively. Theseproteins contain two phosphotyrosine-binding domains (PTBsat the amino-terminus of the catalytic RabGAP domain. Thesecond PTB has been shown to interact with the cytoplasmicregion of the insulin-regulated aminopeptidase (IRAP of theGLUT4 vesicle. In this study, we quantitatively measured the∼μM affinity (KD between TBC1D4 PTB and IRAP using isothermaltitration calorimetry, and further showed that IRAP residues1-49 are the major region mediating this interaction. Wealso demonstrated that the IRAP residues 1-15 are necessarybut not sufficient for the PTB interaction.

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

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

Calorimetry

International Nuclear Information System (INIS)

McDonald, J.C.

1978-01-01

The techniques and equipment currently employed for calorimetric dosimetry have been briefly surveyed and the status of some recent measurements presented. The problems which remain to be investigated are: the thermal defect, the suitability of A-150 plastic as a material for heavy charged particle calorimetry and calorimeter designs that are appropriate for specific radiation situations, including cryogenic calorimeters

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…

Study of interactions between hyaluronan and cationic surfactants by means of calorimetry, turbidimetry, potentiometry and conductometry.

Science.gov (United States)

Krouská, J; Pekař, M; Klučáková, M; Šarac, B; Bešter-Rogač, M

2017-02-10

The thermodynamics of the micelle formation of the cationic surfactants tetradecyltrimethylammonium bromide (TTAB) and cetyltrimethylammonium bromide (CTAB) with and without the addition of hyaluronan of two molecular weights was studied in aqueous solution by titration calorimetry. Macroscopic phase separation, which was detected by calorimetry and also by conductometry, occurs when charges on the surfactant and hyaluronan are balanced. In contrast, turbidimetry and potentiometry showed hyaluronan-surfactant interactions at very low surfactant concentrations. The observed differences between systems prepared with CTAB and TTAB indicate that besides the electrostatic interactions, which probably predominate, hydrophobic effects also play a significant role in hyaluronan interactions with cationic surfactants. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

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

Probing the binding of Cu(2+) ions to a fragment of the Aβ(1-42) polypeptide using fluorescence spectroscopy, isothermal titration calorimetry and molecular dynamics simulations.

Science.gov (United States)

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

2016-09-01

Steady-state and time-resolved fluorescence quenching measurements supported by isothermal titration calorimetry (ITC) and molecular dynamics simulations (MD), with the NMR-derived restraints, were used to investigate the interactions of Cu(2+) ions with a fragment of the Aβ(1-42) polypeptide, Aβ(5-16) with the following sequence: Ac-Arg-His-Asp-Ser-Gly-Tyr-Glu-Val-His-His-Gln-Lys-NH2, denoted as HZ1. The studies presented in this paper, when compared with our previous results (Makowska et al., Spectrochim. Acta A 153: 451-456), show that the affinity of the peptide to metal ions is conformation-dependent. All the measurements were carried out in 20mM 2-(N-morpholino)ethanesulfonic acid (MES) buffer solution, pH6.0. The Stern-Volmer equations, along with spectroscopic observations, were used to determine the quenching and binding parameters. The obtained results unequivocally suggest that Cu(2+) ions quench the fluorescence of HZ1 only through a static quenching mechanism, in contrast to the fragment from the N-terminal part of the FPB28 protein, with sequence Ac-Tyr-Lys-Thr-Ala-Asp-Gly-Lys-Thr-Tyr- NH2 (D9) and its derivative with a single point mutation: Ac-Tyr-Lys-Thr-Ala-Asn-Gly-Lys-Thr-Tyr- NH2 (D9_M), where dynamic quenching occurred. The thermodynamic parameters (ΔITCH, ΔITCS) for the interactions between Cu(2+) ions and the HZ1 peptide were determined from the calorimetric data. The conditional thermodynamic parameters suggest that, under the experimental conditions, the formation of the Cu(2+)-HZ1 complex is both an enthalpy and entropy driven process. Copyright © 2016 Elsevier B.V. All rights reserved.

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...

Analyzing Protein Denaturation using Fast Differential Scanning Calorimetry

NARCIS (Netherlands)

Splinter, R.; Van Herwaarden, A.W.; Iervolino, E.; Vanden Poel, G.; Istrate, D.; Sarro, P.M.

2012-01-01

This paper investigates the possibility to measure protein denaturation with Fast Differential Scanning Calorimetry (FDSC). Cancer can be diagnosed by measuring protein denaturation in blood plasma using Differential Scanning Calorimetry (DSC). FDSC can reduce diagnosis time from hours to minutes,

Isothermal titration calorimetry in nanoliter droplets with subsecond time constants.

Science.gov (United States)

Lubbers, Brad; Baudenbacher, Franz

2011-10-15

We reduced the reaction volume in microfabricated suspended-membrane titration calorimeters to nanoliter droplets and improved the sensitivities to below a nanowatt with time constants of around 100 ms. The device performance was characterized using exothermic acid-base neutralizations and a detailed numerical model. The finite element based numerical model allowed us to determine the sensitivities within 1% and the temporal dynamics of the temperature rise in neutralization reactions as a function of droplet size. The model was used to determine the optimum calorimeter design (membrane size and thickness, junction area, and thermopile thickness) and sensitivities for sample volumes of 1 nL for silicon nitride and polymer membranes. We obtained a maximum sensitivity of 153 pW/(Hz)(1/2) for a 1 μm SiN membrane and 79 pW/(Hz)(1/2) for a 1 μm polymer membrane. The time constant of the calorimeter system was determined experimentally using a pulsed laser to increase the temperature of nanoliter sample volumes. For a 2.5 nanoliter sample volume, we experimentally determined a noise equivalent power of 500 pW/(Hz)(1/2) and a 1/e time constant of 110 ms for a modified commercially available infrared sensor with a thin-film thermopile. Furthermore, we demonstrated detection of 1.4 nJ reaction energies from injection of 25 pL of 1 mM HCl into a 2.5 nL droplet of 1 mM NaOH. © 2011 American Chemical Society

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)

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

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...

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.

Measurement of the thermophysical properties of industrial liquid metallic alloys by non-contact calorimetry under reduced gravity

International Nuclear Information System (INIS)

Wunderlich, R.K.; Fecht, H.-J.

2001-01-01

Full Text: The numerical modeling of casting and solidification is becoming of increased importance in industrial process design. While the numerical algorithms have made large progress towards real process design and optimization, there is a pronounced lack of precise thermophysical input data. This lack is caused by the high chemical reactivity of many metallic alloys in the liquid phase making conventional measurement techniques such as differential thermal analysis difficult if at all possible to apply. In this contribution we report about a project planning to use containerless electromagnetic processing under reduced gravity conditions for thermophysical property measurement of industrially relevant alloys. Alloys of interest are, among others, Ti-alloys, Ni-base superalloys, and steels. In preparation of this project, a survey among leading European industries was conducted revealing properties such as melting range, fraction solid/liquid, specific heat capacity, enthalpy, as well as density, viscosity and surface tension as properties most in need. Non-contact calorimetry of electromagnetically levitated specimens was developed for an investigation of the thermophysical properties of Zr-alloys in the liquid phase. These methods have been applied successfully under reduced gravity conditions on board spacelab to the measurement of the specific heat capacity by modulation calorimetry, the enthalpy of fusion, the total hemispherical emissivity and for an effective thermal conductivity. Specific examples from these experiments demonstrating the applicability of these methods for quantitative calorimetry as well as application at higher Biot numbers will be discussed. New developments include modulation calorimetry in the two phase region for the measurement of the fraction solid. (author)

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''

The heat capacity of polyethylene fibers measured by multi-frequency temperature-modulated calorimetry

International Nuclear Information System (INIS)

Pyda, M.; Nowak-Pyda, E.; Wunderlich, B.

2006-01-01

The apparent heat capacity of polyethylene fibers in the melting region was measured by quasi-isothermal, temperature-modulated differential scanning calorimetry (TMDSC) and compared with results from standard differential scanning calorimetry (DSC) and the solid and liquid thermodynamic heat capacity as references from the ATHAS Data Bank. Using a multi-frequency, complex sawtooth modulation in the quasi-isothermal mode disclosed for the first time that the uncorrected apparent heat capacity C p =A Φ /(A T s ω) of the liquid polyethylene fiber increases with increasing frequency (A Φ is the differential heat-flow rate and A T s is the sample temperature). The frequency-dependent heat capacity cannot be represented by the expression: C p =A Φ /(A T s νω)[1+(τνω) 2 ] 0.5 because of a negative τ 2 . The results were later confirmed by independent measurements on single sinusoidal quasi-isothermal TMDSC on the same material. The error is caused by shrinking of the fiber, which deforms the sample pan

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...

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.

Calorimetry

International Nuclear Information System (INIS)

Pope, B.

1983-01-01

An overall review of properties of various types of calorimeters is given, with special attention given to the challenges of high luminosity and high energy. The calorimeters described include continuous calorimeters, scintillation sampling calorimetry, gas sampling calorimetry, and liquid ionization calorimeters. Next explored are some limiting factors involved in experiments at high luminosities (or at high energies), and some examples are offered of detectors capable of operating at the highest luminosities (energies). Specific areas where substantial research and development work is needed are itemized

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

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

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...

Forward calorimetry in the upgraded UA1 experiment

International Nuclear Information System (INIS)

Alvarez-Taviel, F.J.; Diez-Hedo, F.; Doncel, P.; Marquina, M.A.; Rodrigo, T.; Bacci, C.; Petrolo, E.; Tusi, A.; Ferrando, A.; Givernaud, A.; Rubbia, C.; Vuillemin, V.

1989-01-01

The major improvement in the upgraded UA1 calorimetry at the Santi ppS is the general use of ionization chambers filled with tetramethylpentane (TMP) as a detection medium interspersed with uranium plates as absorber. To achieve overall uniformity of detection down to very small angles, an identical solution is proposed for the forward calorimetry. Forward calorimetry is essential for good total and missing energy measurement at high luminosity in view of the increasing rate of multiple collisions. Both designs for forward and very forward calorimeters are presented along with expected resolutions. (orig.)

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.

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)

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

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

Thermometric titration of sulphate.

Science.gov (United States)

Williams, M B; Janata, J

1970-06-01

Direct thermometric titration of sulphate with a solution of barium perchlorate is proposed. The stoichiometry of the titration is shown to be critically dependent on the concentration of ethanol in the titration medium. The titration is rapid and suffers from only a few interferences.

Potentiometric titration of metal ions in ethanol.

Science.gov (United States)

Gibson, Graham T T; Mohamed, Mark F; Neverov, Alexei A; Brown, R S

2006-09-18

The potentiometric titrations of Zn2+, Cu2+ and 12 Ln3+ metal ions were obtained in ethanol to determine the titration constants (defined as the at which the [-OEt]/[Mx+]t ratios are 0.5, 1.5, and 2.5) and in two cases (La3+ and Zn2+) a complete speciation diagram. Several simple monobasic acids and aminium ions were also titrated to test the validity of experimental titration measurements and to establish new constants in this medium that will be useful for the preparation of buffers and standard solutions. The dependence of the titration constants on the concentration and type of metal ion and specific counterion effects is discussed. In selected cases, the titration profiles were analyzed using a commercially available fitting program to obtain information about the species present in solution, including La3+ for which a dimer model is proposed. The fitting provides the microscopic values for deprotonation of one to four metal-bound ethanol molecules. Kinetics for the La3+-catalyzed ethanolysis of paraoxon as a function of are presented and analyzed in terms of La3+ speciation as determined by the analysis of potentiometric titration curves. The stability constants for the formation of Zn2+ and Cu2+ complexes with 1,5,9-triazacyclododecane as determined by potentiometric titration are presented.

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.

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.

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.

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.

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…

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

Potentiometric Titrations for Measuring the Capacitance of Colloidal Photodoped ZnO Nanocrystals.

Science.gov (United States)

Brozek, Carl K; Hartstein, Kimberly H; Gamelin, Daniel R

2016-08-24

Colloidal semiconductor nanocrystals offer a unique opportunity to bridge molecular and bulk semiconductor redox phenomena. Here, potentiometric titration is demonstrated as a method for quantifying the Fermi levels and charging potentials of free-standing colloidal n-type ZnO nanocrystals possessing between 0 and 20 conduction-band electrons per nanocrystal, corresponding to carrier densities between 0 and 1.2 × 10(20) cm(-3). Potentiometric titration of colloidal semiconductor nanocrystals has not been described previously, and little precedent exists for analogous potentiometric titration of any soluble reductants involving so many electrons. Linear changes in Fermi level vs charge-carrier density are observed for each ensemble of nanocrystals, with slopes that depend on the nanocrystal size. Analysis indicates that the ensemble nanocrystal capacitance is governed by classical surface electrical double layers, showing no evidence of quantum contributions. Systematic shifts in the Fermi level are also observed with specific changes in the identity of the charge-compensating countercation. As a simple and contactless alternative to more common thin-film-based voltammetric techniques, potentiometric titration offers a powerful new approach for quantifying the redox properties of colloidal semiconductor nanocrystals.

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

LIGHT TITRATIONS

Science.gov (United States)

Field, John; Baas-Becking, Lourens G. M.

1926-01-01

1. The usefulness of the radiomicrometer in titration work has been pointed out. The authors suggest that light titration may also be used where a reaction mixture changes its absorption in the (near) infra-red. 2. The applicability of this method to the starch-iodine reaction has been demonstrated. PMID:19872266

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)

Thermodynamic properties of soddyite from solubility and calorimetry measurements

International Nuclear Information System (INIS)

Gorman-Lewis, Drew; Mazeina, Lena; Fein, Jeremy B.; Szymanowski, Jennifer E.S.; Burns, Peter C.; Navrotsky, Alexandra

2007-01-01

The release of uranium from geologic nuclear waste repositories under oxidizing conditions can only be modeled if the thermodynamic properties of the secondary uranyl minerals that form in the repository setting are known. Toward this end, we synthesized soddyite ((UO 2 ) 2 (SiO 4 )(H 2 O) 2 ), and performed solubility measurements from both undersaturation and supersaturation. The solubility measurements rigorously constrain the value of the solubility product of synthetic soddyite, and consequently its standard-state Gibbs free energy of formation. The log solubility product (lg K sp ) with its error (1σ) is (6.43 + 0.20/-0.37), and the standard-state Gibbs free energy of formation is (-3652.2 ± 4.2 (2σ)) kJ mol -1 . High-temperature drop solution calorimetry was conducted, yielding a calculated standard-state enthalpy of formation of soddyite of (-4045.4 ± 4.9 (2σ)) kJ . mol -1 . The standard-state Gibbs free energy and enthalpy of formation yield a calculated standard-state entropy of formation of soddyite of (-1318.7 ± 21.7 (2σ)) J . mol -1 . K -1 . The measurements and associated thermodynamic calculations not only describe the T = 298 K stability and solubility of soddyite, but they also can be used in predictions of repository performance through extrapolation of these properties to repository temperatures

Recent developments in silicon calorimetry

International Nuclear Information System (INIS)

Brau, J.E.

1990-11-01

We present a survey of some of the recent calorimeter applications of silicon detectors. The numerous attractive features of silicon detectors are summarized, with an emphasis on those aspects important to calorimetry. Several of the uses of this technology are summarized and referenced. We consider applications for electromagnetic calorimetry, hadronic calorimetry, and proposals for the SSC

Differential scanning calorimetry (DSC) of semicrystalline polymers.

Science.gov (United States)

Schick, C

2009-11-01

Differential scanning calorimetry (DSC) is an effective analytical tool to characterize the physical properties of a polymer. DSC enables determination of melting, crystallization, and mesomorphic transition temperatures, and the corresponding enthalpy and entropy changes, and characterization of glass transition and other effects that show either changes in heat capacity or a latent heat. Calorimetry takes a special place among other methods. In addition to its simplicity and universality, the energy characteristics (heat capacity C(P) and its integral over temperature T--enthalpy H), measured via calorimetry, have a clear physical meaning even though sometimes interpretation may be difficult. With introduction of differential scanning calorimeters (DSC) in the early 1960s calorimetry became a standard tool in polymer science. The advantage of DSC compared with other calorimetric techniques lies in the broad dynamic range regarding heating and cooling rates, including isothermal and temperature-modulated operation. Today 12 orders of magnitude in scanning rate can be covered by combining different types of DSCs. Rates as low as 1 microK s(-1) are possible and at the other extreme heating and cooling at 1 MK s(-1) and higher is possible. The broad dynamic range is especially of interest for semicrystalline polymers because they are commonly far from equilibrium and phase transitions are strongly time (rate) dependent. Nevertheless, there are still several unsolved problems regarding calorimetry of polymers. I try to address a few of these, for example determination of baseline heat capacity, which is related to the problem of crystallinity determination by DSC, or the occurrence of multiple melting peaks. Possible solutions by using advanced calorimetric techniques, for example fast scanning and high frequency AC (temperature-modulated) calorimetry are discussed.

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

Molecular Weight Measurement of Biobased Furan Polyamides via Non-Aqueous Potentiometric Titration

Science.gov (United States)

2013-06-01

electromagnetic fields, all titrations were completed in a chemical hood, which acted as a Faraday cage (a shield used to blocks external static and...while using DMF as a solvent. Additionally, no Faraday cage was used in the experimental setup, so the titrations were conducted inside the chemical...monomer was becoming more soluble in glacial acetic acid and the amount of chlorobenzene had less of an effect on the solution properties (i.e

Computer controlled titration with piston burette or peristaltic pump - a comparison.

Science.gov (United States)

Hoffmann, W

1996-09-01

The advantages and problems of the use of piston burettes and peristaltic pumps for dosage of titrant solutions in automatic titrations are shown. For comparison, only the dosing devices were exchanged and all other components and conditions remained unchanged. The results of continuous acid base titration show good agreement and comparable reproducibility. Potentiometric sensors (glass electrodes) with different equilibration behaviour influence the results. The capability of such electrodes was tested. Conductometric measurements allow a much faster detection because there is no equilibration of electrodes. Piston burettes should be used for titration with very high precision, titration with organic solvents and slow titrations. Peristaltic pumps seem to be more suitable for continuous titrations and long time operation without service.

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.

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

The uncertainty evaluation of measurement for uranium in UF_6 hydrolysate by potentiometric titration

International Nuclear Information System (INIS)

Jiang Haiying; Cheng Ruoyu; Meng Xiujun

2014-01-01

Based on the building of mathematical model, this paper analyzed the origin of component of indeterminacy of which the measurement result for uranium in uranium hexafluoride hydrolysate by potentiometric titration, also each uncertainty was calculated and the expanded uncertainty was given. By evaluation the result of the uranium concentration is that: (158.88 + 1.22) mgU/mL, K = 2, P = 95%. (authors)

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

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.

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.

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

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

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...... 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....... In Periods 1 and 5 all animals were fed a diet with a high quality fish meal (FISH; n=12), while in Period 3 half of the animals received the FISH diet (n=6) and the other half a diet with soy protein concentrate (SOY; n=6) as main protein source. An intraperitoneal injection of 1-13C-leucine was given...

Laser-flash calorimetry

International Nuclear Information System (INIS)

Takahashi, Y.; Nakamura, J.-I.

1982-01-01

The heat capacity of vanadium has been measured by laser-flash calorimetry in the temperature region from 80 to 1000 K. The results are compared with available low- and high-temperature heat capacities, and revised thermodynamic values of vanadium are given. No heat-capacity anomaly has been found in the pure vanadium sample over the temperature range investigated, while a small heat-capacity discontinuity, less than 1.2 J.K -1 .mol -1 , has been observed at 220 to 230 K on the same sample but electropolished before measurement. This anomaly disappeared after annealing at 1000 K in vacuo for 1 h and is attributable to the introduction of a small amount of hydrogen during electropolishing. (author)

Scintillator plate calorimetry

International Nuclear Information System (INIS)

Price, L.E.

1990-01-01

Calorimetry using scintillator plates or tiles alternated with sheets of (usually heavy) passive absorber has been proven over multiple generations of collider detectors. Recent detectors including UA1, CDF, and ZEUS have shown good results from such calorimeters. The advantages offered by scintillator calorimetry for the SSC environment, in particular, are speed (<10 nsec), excellent energy resolution, low noise, and ease of achieving compensation and hence linearity. On the negative side of the ledger can be placed the historical sensitivity of plastic scintillators to radiation damage, the possibility of nonuniform response because of light attenuation, and the presence of cracks for light collection via wavelength shifting plastic (traditionally in sheet form). This approach to calorimetry is being investigated for SSC use by a collaboration of Ames Laboratory/Iowa State University, Argonne National Laboratory, Bicron Corporation, Florida State University, Louisiana State University, University of Mississippi, Oak Ridge National Laboratory, Virginia Polytechnic Institute and State University, Westinghouse Electric Corporation, and University of Wisconsin

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

Direct measurement of the interaction energy between solids and gases--3. Comparison of the calorimetric titration method with the amine titration method for the determination of acid strength distribution of the silica-alumina surface

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, H.; Masuda, T.; Tsutsumi, K.; Takahashi, H.

1978-07-01

Comparison of the calorimetric titration method with the amine titration method for the determination of acid strength distribution of the silica-alumina surface was carried out for a catalyst containing 13% by wt alumina and evacuated at 400/sup 0/C at 0.00001 mm Hg for five hours. The heats of adsorption of ammonia on silica-alumina poisoned with Hammett indicators of 8.2 to 3.3 pK/sub a/ were also measured to obtain the relation between the dissociation constant of the acid (pK/sub a/) and the heat of adsorption. At pK/sub a/ values of -5.6 and +3.3, the differential heats of adsorption were 76.1 and 55.1 kj/mole, respectively. The number of acid sites calculated from the heat vs. adsorbed-amount curve was about twice as large as that determined by amine titration. The discrepancy is discussed.

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

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

Structure, Dynamics, and Kinetics of Weak Protein-Protein Complexes from NMR Spin Relaxation Measurements of Titrated Solutions

International Nuclear Information System (INIS)

Salmon, L.; Licinio, A.; Jensen, M.R.; Blackledge, M.; Ortega Roldan, J.L.; Van Nuland, N.; Lescop, E.

2011-01-01

We have recently presented a titration approach for the determination of residual dipolar couplings (RDCs) from experimentally inaccessible complexes. Here, we extend this approach to the measurement of 15 N spin relaxation rates and demonstrate that this can provide long-range structural, dynamic, and kinetic information about these elusive systems. (authors)

Optical calorimetry in microfluidic droplets.

Science.gov (United States)

Chamoun, Jacob; Pattekar, Ashish; Afshinmanesh, Farzaneh; Martini, Joerg; Recht, Michael I

2018-05-29

A novel microfluidic calorimeter that measures the enthalpy change of reactions occurring in 100 μm diameter aqueous droplets in fluoropolymer oil has been developed. The aqueous reactants flow into a microfluidic droplet generation chip in separate fluidic channels, limiting contact between the streams until immediately before they form the droplet. The diffusion-driven mixing of reactants is predominantly restricted to within the droplet. The temperature change in droplets due to the heat of reaction is measured optically by recording the reflectance spectra of encapsulated thermochromic liquid crystals (TLC) that are added to one of the reactant streams. As the droplets travel through the channel, the spectral characteristics of the TLC represent the internal temperature, allowing optical measurement with a precision of ≈6 mK. The microfluidic chip and all fluids are temperature controlled, and the reaction heat within droplets raises their temperature until thermal diffusion dissipates the heat into the surrounding oil and chip walls. Position resolved optical temperature measurement of the droplets allows calculation of the heat of reaction by analyzing the droplet temperature profile over time. Channel dimensions, droplet generation rate, droplet size, reactant stream flows and oil flow rate are carefully balanced to provide rapid diffusional mixing of reactants compared to thermal diffusion, while avoiding thermal "quenching" due to contact between the droplets and the chip walls. Compared to conventional microcalorimetry, which has been used in this work to provide reference measurements, this new continuous flow droplet calorimeter has the potential to perform titrations ≈1000-fold faster while using ≈400-fold less reactants per titration.

Potentiometric titration of plutonium

International Nuclear Information System (INIS)

Silver, G.L.

1978-01-01

In the potentiometric titration of plutonium(III), it has been customary to take the equivalence point as the inflection point on a plot of potential vs. volume of titrant. It have not been, however, demonstrated, that the stoichiometric end point corresponds to the inflection point. Suggestions are made according to which these points may not correspond in the potentiometric titration of plutonium(III), as these titrations are ordinarily concluded in a period of time which is short compared to the time required for valence state rearrangement through disproportionation. (T.G.)

Inherent limitations of fixed time servo-controlled radiometric calorimetry

International Nuclear Information System (INIS)

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

1987-01-01

There has been some interest in low precision, short run time calorimetry measurements. This type of calorimetry measurement has been proposed for use when high precision measurements are not required, for example, to screen scrap containers to determine if there is enough material to be measured more accurately of for confirmatory measurements that only require low precision results. The equipment needed to make these measurements is a servo-controlled calorimeter with a sample preequilibration bath. The preequilibration bath temperature is set to the internal temperature of the calorimeter running at a fixed servo-controlled wattage level. The sample power value is determined at a fixed time form the sample loading into the calorimeter. There are some limitations and areas of uncertainties in the use of data obtained by this method. Data collected under controlled conditions demonstrate the limitations. Sample packaging, preequilibration time, and item wattage were chosen as the variables most likely to be encountered in a plant environment

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

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

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...

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.

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.

Comparison of methods for accurate end-point detection of potentiometric titrations

Science.gov (United States)

Villela, R. L. A.; Borges, P. P.; Vyskočil, L.

2015-01-01

Detection of the end point in potentiometric titrations has wide application on experiments that demand very low measurement uncertainties mainly for certifying reference materials. Simulations of experimental coulometric titration data and consequential error analysis of the end-point values were conducted using a programming code. These simulations revealed that the Levenberg-Marquardt method is in general more accurate than the traditional second derivative technique used currently as end-point detection for potentiometric titrations. Performance of the methods will be compared and presented in this paper.

Comparison of methods for accurate end-point detection of potentiometric titrations

International Nuclear Information System (INIS)

Villela, R L A; Borges, P P; Vyskočil, L

2015-01-01

Detection of the end point in potentiometric titrations has wide application on experiments that demand very low measurement uncertainties mainly for certifying reference materials. Simulations of experimental coulometric titration data and consequential error analysis of the end-point values were conducted using a programming code. These simulations revealed that the Levenberg-Marquardt method is in general more accurate than the traditional second derivative technique used currently as end-point detection for potentiometric titrations. Performance of the methods will be compared and presented in this paper

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

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  Direct calorimetry and indirect calorimetry gave similar estimates of energy expenditure. Energy expenditure was 10% lower in the prone position than in the supine position. Thieme Medical Publishers 333 Seventh Avenue, New York, NY 10001, USA.

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.

Complex coacervates of hyaluronic acid and lysozyme

DEFF Research Database (Denmark)

Water, Jorrit J.; Schack, Malthe M.; Velazquez-Campoy, Adrian

2014-01-01

stoichiometry was determined using solution depletion and isothermal titration calorimetry. The binding stoichiometry of lysozyme to hyaluronic acid (870 kDa) determined by solution depletion was found to be 225.9 ± 6.6 mol, or 0.1 bound lysozyme molecules per hyaluronic acid monomer. This corresponded well...... with that obtained by isothermal titration calorimetry of 0.09 bound lysozyme molecules per hyaluronic acid monomer. The complexation did not alter the secondary structure of lysozyme measured by Fourier-transform infrared spectroscopy overlap analysis and had no significant impact on the Tm of lysozyme determined...

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.

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

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.

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

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.

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.

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...

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.

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.

[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.

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.

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...

Irreversible denaturation of maltodextrin glucosidase studied by differential scanning calorimetry, circular dichroism, and turbidity measurements.

Science.gov (United States)

Goyal, Megha; Chaudhuri, Tapan K; Kuwajima, Kunihiro

2014-01-01

Thermal denaturation of Escherichia coli maltodextrin glucosidase was studied by differential scanning calorimetry, circular dichroism (230 nm), and UV-absorption measurements (340 nm), which were respectively used to monitor heat absorption, conformational unfolding, and the production of solution turbidity. The denaturation was irreversible, and the thermal transition recorded at scan rates of 0.5-1.5 K/min was significantly scan-rate dependent, indicating that the thermal denaturation was kinetically controlled. The absence of a protein-concentration effect on the thermal transition indicated that the denaturation was rate-limited by a mono-molecular process. From the analysis of the calorimetric thermograms, a one-step irreversible model well represented the thermal denaturation of the protein. The calorimetrically observed thermal transitions showed excellent coincidence with the turbidity transitions monitored by UV-absorption as well as with the unfolding transitions monitored by circular dichroism. The thermal denaturation of the protein was thus rate-limited by conformational unfolding, which was followed by a rapid irreversible formation of aggregates that produced the solution turbidity. It is thus important to note that the absence of the protein-concentration effect on the irreversible thermal denaturation does not necessarily means the absence of protein aggregation itself. The turbidity measurements together with differential scanning calorimetry in the irreversible thermal denaturation of the protein provided a very effective approach for understanding the mechanisms of the irreversible denaturation. The Arrhenius-equation parameters obtained from analysis of the thermal denaturation were compared with those of other proteins that have been reported to show the one-step irreversible thermal denaturation. Maltodextrin glucosidase had sufficiently high kinetic stability with a half-life of 68 days at a physiological temperature (37°C).

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

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.

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.

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

Number of independent parameters in the potentiometric titration of humic substances.

Science.gov (United States)

Lenoir, Thomas; Manceau, Alain

2010-03-16

With the advent of high-precision automatic titrators operating in pH stat mode, measuring the mass balance of protons in solid-solution mixtures against the pH of natural and synthetic polyelectrolytes is now routine. However, titration curves of complex molecules typically lack obvious inflection points, which complicates their analysis despite the high-precision measurements. The calculation of site densities and median proton affinity constants (pK) from such data can lead to considerable covariance between fit parameters. Knowing the number of independent parameters that can be freely varied during the least-squares minimization of a model fit to titration data is necessary to improve the model's applicability. This number was calculated for natural organic matter by applying principal component analysis (PCA) to a reference data set of 47 independent titration curves from fulvic and humic acids measured at I = 0.1 M. The complete data set was reconstructed statistically from pH 3.5 to 9.8 with only six parameters, compared to seven or eight generally adjusted with common semi-empirical speciation models for organic matter, and explains correlations that occur with the higher number of parameters. Existing proton-binding models are not necessarily overparametrized, but instead titration data lack the sensitivity needed to quantify the full set of binding properties of humic materials. Model-independent conditional pK values can be obtained directly from the derivative of titration data, and this approach is the most conservative. The apparent proton-binding constants of the 23 fulvic acids (FA) and 24 humic acids (HA) derived from a high-quality polynomial parametrization of the data set are pK(H,COOH)(FA) = 4.18 +/- 0.21, pK(H,Ph-OH)(FA) = 9.29 +/- 0.33, pK(H,COOH)(HA) = 4.49 +/- 0.18, and pK(H,Ph-OH)(HA) = 9.29 +/- 0.38. Their values at other ionic strengths are more reliably calculated with the empirical Davies equation than any existing model fit.

A generalized approach for the calculation and automation of potentiometric titrations Part 2. Redox Titrations

NARCIS (Netherlands)

Stur, J.; Bos, M.; van der Linden, W.E.

1984-01-01

The very fast calculation procedure described earlier is applied to calculate the titration curves of complicated redox systems. The theory is extended slightly to cover inhomogeneous redox systems. Titrations of iodine or 2,6-dichloroindophenol with ascorbic acid are described. It is shown that

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)

Ionic liquids. Combination of combustion calorimetry with high-level quantum chemical calculations for deriving vaporization enthalpies.

Science.gov (United States)

Emel'yanenko, Vladimir N; Verevkin, Sergey P; Heintz, Andreas; Schick, Christoph

2008-07-10

In this work, the molar enthalpies of formation of the ionic liquids [C2MIM][NO3] and [C4MIM][NO3] were measured by means of combustion calorimetry. The molar enthalpy of fusion of [C2MIM][NO3] was measured using differential scanning calorimetry. Ab initio calculations of the enthalpy of formation in the gaseous phase have been performed for the ionic species using the G3MP2 theory. We have used a combination of traditional combustion calorimetry with modern high-level ab initio calculations in order to obtain the molar enthalpies of vaporization of a series of the ionic liquids under study.

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.

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.

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

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.

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

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.

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

Estimating heat transfer bias of kinetic measurement for polymers by differential scanning calorimetry with isothermal mode; Evaluation de l'erreur due au transfert de chaleur lors des mesures cinetiques dans les polymeres par calorimetrie differentielle a balayage en mode isotherme

Energy Technology Data Exchange (ETDEWEB)

Danes, Florin; Garnier, Bertrand [Laboratoire de Thermocinetique, UMR CNRS 6607, Ecole Polytechnique de l' Universite de Nantes, rue C. Pauc, BP50609, 44306 cedex 3, Nantes (France)

2003-06-01

The non-uniformity of temperatures in the DSC sample, and the subsequent difference between mean sample temperature and measured one (in the support of the crucible) are identified as the main source of bias for the isothermal mode determination of kinetic characteristics by differential scanning calorimetry. Chemical reactions under consideration are these with important heat effects into thermal insulators, as for example the reticulation of polymeric materials.By introducing an analytical model of heat transfer in DSC reactive samples, we have performed an estimation for the upper limit of the maximal size of samples which corresponds to a given relative error of the reaction rate, as measured by isothermal DSC calorimetry. For example, with a 5% error and flat samples, we have found admissible sample thicknesses which decrease with temperature and are between 1.9 and 3.1 mm for the sulphur vulcanization of a natural rubber and between 0.6 and 1.1 mm for the reticulation of a pre-polymerized epoxy resin. (authors)

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.

A generalized approach for the calculation and automation of potentiometric titrations Part 1. Acid-Base Titrations

NARCIS (Netherlands)

Stur, J.; Bos, M.; van der Linden, W.E.

1984-01-01

Fast and accurate calculation procedures for pH and redox potentials are required for optimum control of automatic titrations. The procedure suggested is based on a three-dimensional titration curve V = f(pH, redox potential). All possible interactions between species in the solution, e.g., changes

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.

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

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

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

Liquid ionization calorimetry: review and preview

International Nuclear Information System (INIS)

Fabjan, C.W.

1995-01-01

The experimental requirements at existing and planned accelerators, and new facilities for underground or space-borne experimentation have stimulated a wide-ranging R and D programme in liquid ionization calorimetry. Precision sampling calorimetry is approaching ''crystal'' energy resolution whilst their rate capabilities will be able to cope with the highest LHC luminosities. (Quasi)-homogeneous noble-liquid calorimeters are under construction or in the planning stage to address some of the most fundamental physics questions. (orig.)

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.

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.

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

International Nuclear Information System (INIS)

Brandt, K.D.; Schnobrich, K.E.; Johnson, D.K.

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

Fabrication of 12% 240Pu calorimetry standards

International Nuclear Information System (INIS)

Long, S.M.; Hildner, S.; Gutierrez, D.; Mills, C.; Garcia, W.; Gurule, C.

1995-01-01

Throughout the DOE complex, laboratories are performing calorimetric assays on items containing high burnup plutonium. These materials contain higher isotopic range and higher wattages than materials previously encountered in vault holdings. Currently, measurement control standards have been limited to utilizing 6% 240 Pu standards. The lower isotopic and wattage value standards do not complement the measurement of the higher burnup material. Participants of the Calorimetry Exchange (CALEX) Program have identified the need for new calorimetric assay standards with a higher wattage and isotopic range. This paper describes the fabrication and verification measurements of the new CALEX standard containing 12% 240 Pu oxide with a wattage of about 6 to 8 watts

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_m_i_x) was determined by isothermal titration calorimetry (ITC). After the cmc_m_i_x, 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.

Stability of some Cactaceae proteins based on fluorescence, circular dichroism, and differential scanning calorimetry measurements.

Science.gov (United States)

Gorinstein, S; Zemser, M; Vargas-Albores, F; Ochoa, J L; Paredes-Lopez, O; Scheler, C; Aksu, S; Salnikow, J

1999-02-01

Characterization of three cactus proteins (native and denatured) from Machaerocereus gummosus (Pitahaya agria), Lophocereu schottii (Garambullo), and Cholla opuntia (Cholla), was based on electrophoretic, fluorescence, CD (circular dichroism), DSC (differential scanning calorimetry), and FT-IR (Fourier transform infrared) measurements. The obtained results of intrinsic fluorescence, DSC, and CD were dissimilar for the three species of cactus, providing evidence of differences in secondary and tertiary structures. Cactus proteins may be situated in the following order corresponding to their relative stability: Machaerocereus gummosus (Pitahaya agria) > Cholla opuntia (Cholla) > Lophocereu schottii (Garambullo). Thermodynamic properties of proteins and their changes upon denaturation (temperature of denaturation, enthalphy, and the number of ruptured hydrogen bonds) were correlated with the secondary structure of proteins and disappearance of alpha-helix.

Determination of substances by radiothermometric titration

International Nuclear Information System (INIS)

Tolgyessy, J.; Lesny, J.

1976-01-01

For determination, nitrogen is bubbled through a solution containing radioactive Kr, Xe, Rn or another aerogen in addition to the substance determined. A continuous or intermittent addition of the titrating solution results in the release of reaction heat, thus increasing the temperature of the reaction mixture, which releases a radioactive gas. Upon reaching the equivalence point, the cold titrating reagent cools the reaction mixture, thus reducing the radioactive substance release. The equivalence point lies at the point of intersection of the extended linear parts of the curve of the dependence of released radioactivity on the volume of the titrating solution added. (M.K.)

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....

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...

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

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…

Symmetry Properties of Potentiometric Titration Curves.

Science.gov (United States)

Macca, Carlo; Bombi, G. Giorgio

1983-01-01

Demonstrates how the symmetry properties of titration curves can be efficiently and rigorously treated by means of a simple method, assisted by the use of logarithmic diagrams. Discusses the symmetry properties of several typical titration curves, comparing the graphical approach and an explicit mathematical treatment. (Author/JM)

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

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.

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.

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.

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.

Measurement of the enthalpies of vaporization and sublimation of solids aromatic hydrocarbons by differential scanning calorimetry

International Nuclear Information System (INIS)

Rojas, Aaron; Orozco, Eulogio

2003-01-01

An experimental procedure is proposed for direct measurement of the heat involved in the vaporization of a solid organic compound above its normal melting temperature. This technique consists on the fusion of a solid aromatic hydrocarbon, which is then vaporized by a sudden decrease of the pressure. The direct register of heat flow as function of time by differential scanning calorimetry allows the quantifying of the enthalpy of vaporization of compounds such as phenanthrene, β-naphthol, pyrene, and anthracene. Enthalpies of vaporization were measured in an isothermal mode over a range of temperatures from 10 to 20 K above the melting temperatures of each compound, while enthalpies of fusion were determined from separate experiments performed in a scanning mode. Enthalpies of sublimation are computed from results of fusion and vaporization, and then compared with results from the literature, which currently are obtained by calorimetric or indirect techniques

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

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

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).

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)

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

Simple home-made sensors for potentiometric titrations

International Nuclear Information System (INIS)

Selig, W.

1982-04-01

A sensor for potentiometric titrations was prepared by coating a spectroscopic graphite rod with a solution of poly(vinyl chloride) and dioctyphthalate in tetrahydrofuran. The reference electrode was an Ag/AgCl single-junction electrode. The sensor was used in precipitation, acid-base, compleximetric, and redox titrations. Preparation of the coated-graphite sensor is simple and rapid. Moreover, it is quite inexpensive. A limitation is its applicability in aqueous media only, because organic solvents will dissolve the membrane. Various uncoated types of graphite have also been investigated as sensors, particularly in two applications of interest in the analysis of propellants: the titration of nitroform and perchlorate. Obviously, these sensors can be used also in nonaqueous, or partially nonaqueous media. These sensors may also find use in the potentiometric titration of fluoride vs La(III) or Th

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.

Linear Titration Curves of Acids and Bases.

Science.gov (United States)

Joseph, N R

1959-05-29

The Henderson-Hasselbalch equation, by a simple transformation, becomes pH - pK = pA - pB, where pA and pB are the negative logarithms of acid and base concentrations. Sigmoid titration curves then reduce to straight lines; titration curves of polyelectrolytes, to families of straight lines. The method is applied to the titration of the dipeptide glycyl aminotricarballylic acid, with four titrable groups. Results are expressed as Cartesian and d'Ocagne nomograms. The latter is of a general form applicable to polyelectrolytes of any degree of complexity.

Novel titration method for surface-functionalised silica

Energy Technology Data Exchange (ETDEWEB)

Hofen, Kai; Weber, Siegfried [Department of Biotechnology, University of Applied Sciences, Mannheim (Germany); Chan, Chiu Ping Candace [School of Advanced Manufacturing and Mechanical Engineering, Mawson Institute, University of South Australia, Mawson Lakes Blvd, Mawson Lakes 5095 (Australia); Majewski, Peter, E-mail: peter.majewski@unisa.edu.au [School of Advanced Manufacturing and Mechanical Engineering, Mawson Institute, University of South Australia, Mawson Lakes Blvd, Mawson Lakes 5095 (Australia)

2011-01-15

This paper describes three inexpensive and fast analytical methods to characterise grafted particle surfaces. The reaction of silica with (3-aminopropyl)triethoxysilane, (3-mercaptopropyl)trimethoxysilane and N-(phosphonomethyl)iminodiacetic acid hydrate, respectively, leads to NH{sub 2}-, SO{sub 3}H- or COOH-functionalised silica, which were characterised by X-ray photoelectron spectrometry and titration in nonaqueous media as well as with two titration methods in a water-based environment. In the work presented, factors influencing the titrations are pointed out and solutions are presented to overcome these limiting factors are shown.

Novel titration method for surface-functionalised silica

International Nuclear Information System (INIS)

Hofen, Kai; Weber, Siegfried; Chan, Chiu Ping Candace; Majewski, Peter

2011-01-01

This paper describes three inexpensive and fast analytical methods to characterise grafted particle surfaces. The reaction of silica with (3-aminopropyl)triethoxysilane, (3-mercaptopropyl)trimethoxysilane and N-(phosphonomethyl)iminodiacetic acid hydrate, respectively, leads to NH 2 -, SO 3 H- or COOH-functionalised silica, which were characterised by X-ray photoelectron spectrometry and titration in nonaqueous media as well as with two titration methods in a water-based environment. In the work presented, factors influencing the titrations are pointed out and solutions are presented to overcome these limiting factors are shown.

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.

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.

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.

Estimation of uncertainty in pKa values determined by potentiometric titration.

Science.gov (United States)

Koort, Eve; Herodes, Koit; Pihl, Viljar; Leito, Ivo

2004-06-01

A procedure is presented for estimation of uncertainty in measurement of the pK(a) of a weak acid by potentiometric titration. The procedure is based on the ISO GUM. The core of the procedure is a mathematical model that involves 40 input parameters. A novel approach is used for taking into account the purity of the acid, the impurities are not treated as inert compounds only, their possible acidic dissociation is also taken into account. Application to an example of practical pK(a) determination is presented. Altogether 67 different sources of uncertainty are identified and quantified within the example. The relative importance of different uncertainty sources is discussed. The most important source of uncertainty (with the experimental set-up of the example) is the uncertainty of pH measurement followed by the accuracy of the burette and the uncertainty of weighing. The procedure gives uncertainty separately for each point of the titration curve. The uncertainty depends on the amount of titrant added, being lowest in the central part of the titration curve. The possibilities of reducing the uncertainty and interpreting the drift of the pK(a) values obtained from the same curve are discussed.

Potentiometric titration of free acid in uranium solutions

International Nuclear Information System (INIS)

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

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.

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

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

Thermometric titration in investigation of the formation of polyanions of molybdenum(VI), tungsten(VI), vanadium(V), and chromium (VI)-I: comparison of thermometric and potentiometric titration curves.

Science.gov (United States)

Kiba, N; Takeuchi, T

1973-09-01

A new twin-cell thermometric titrator has been devised and used for thermometric titration of solutions of sodium molybdate, sodium tungstate, sodium orthovanadate, ammonium metavanadate, and potassium chromate with perchloric acid. The thermometric titration curves were compared with corresponding pH-titration curves for elucidation of the reactions occurring in the titrations. Thermometric titrimetric methods have been developed for the determination of tungsten, vanadium and chromium.

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. ...

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.

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.

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.

Students' integration of multiple representations in a titration experiment

Science.gov (United States)

Kunze, Nicole M.

A complete understanding of a chemical concept is dependent upon a student's ability to understand the microscopic or particulate nature of the phenomenon and integrate the microscopic, symbolic, and macroscopic representations of the phenomenon. Acid-base chemistry is a general chemistry topic requiring students to understand the topics of chemical reactions, solutions, and equilibrium presented earlier in the course. In this study, twenty-five student volunteers from a second semester general chemistry course completed two interviews. The first interview was completed prior to any classroom instruction on acids and bases. The second interview took place after classroom instruction, a prelab activity consisting of a titration calculation worksheet, a titration computer simulation, or a microscopic level animation of a titration, and two microcomputer-based laboratory (MBL) titration experiments. During the interviews, participants were asked to define and describe acid-base concepts and in the second interview they also drew the microscopic representations of four stages in an acid-base titration. An analysis of the data showed that participants had integrated the three representations of an acid-base titration to varying degrees. While some participants showed complete understanding of acids, bases, titrations, and solution chemistry, other participants showed several alternative conceptions concerning strong acid and base dissociation, the formation of titration products, and the dissociation of soluble salts. Before instruction, participants' definitions of acid, base, and pH were brief and consisted of descriptive terms. After instruction, the definitions were more scientific and reflected the definitions presented during classroom instruction.

A guide to automation techniques in calorimetry

International Nuclear Information System (INIS)

Renz, D.P.; Wetzel, J.R.; Breakall, K.L.; James, S.J.; Kasperski, P.W.

1992-01-01

Many improvements occurring in calorimetry measurement technology in the past few years will help current users of calorimeters to achieve better use of their existing systems. These include a more user friendly operator computer interface, a more detailed printout at the end of each run, improved data processing to eliminate operator error, and improved system monitoring to detect system or environmental problems. In addition, an electrical calibration heater has been developed to replace plutonium-238 heat standards for calibrating calorimeters, and several automation systems allow for easier and safer system operation

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.)

Non-aqueous titration of benzotrifuroxan (BTF)

Energy Technology Data Exchange (ETDEWEB)

Selig, W.

1978-01-01

This compound can be titrated potentiometrically as an acid with tetrabutylammonium hydroxide in dimethylformamide, dimethylsulfoxide, acetone, pyridine, tetramethylguanidine. The solvent of choice is dimethylformamide which yields the steepest titration curve and the lowest standard deviation. The equivalent weight of benzotrifuroxan is dependent on the solvent used indicating a strong interaction with the solvent. In dimethylformamide, the equivalent weight of benzotrifuroxan is 151.3, corresponding to 1.67 equivalents per mole.

Direct measurement of electron beam quality conversion factors using water calorimetry

Energy Technology Data Exchange (ETDEWEB)

Renaud, James, E-mail: james.renaud@mail.mcgill.ca; Seuntjens, Jan [Medical Physics Unit, McGill University, Montréal, Québec H3G 1A4 (Canada); Sarfehnia, Arman [Medical Physics Unit, McGill University, Montréal, Québec H3G 1A4, Canada and Department of Radiation Oncology, University of Toronto, Toronto, Ontario M5S 3E2 (Canada); Marchant, Kristin [Allan Blair Cancer Centre, Saskatchewan Cancer Agency, Regina, Saskatchewan S4T 7T1, Canada and Department of Oncology, University of Saskatchewan, Saskatoon, Saskatchewan S7N 5A1 (Canada); McEwen, Malcolm; Ross, Carl [Ionizing Radiation Standards, National Research Council of Canada, Ottawa, Ontario K1A 0R6 (Canada)

2015-11-15

. General agreement between the relative electron energy dependence of the PTW Roos data measured in this work and a recent MC-based study are also shown. Conclusions: 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 (R{sub 50} = 2.25 cm)

Study of the interactions of PAMAM-NH2 G4 dendrimer with selected natural amino acids in aqueous solutions

International Nuclear Information System (INIS)

Buczkowski, Adam; Palecz, Bartlomiej

2014-01-01

Highlights: • Calorimetric titration and dilution calorimetry show strong interactions between PAMAM-NH 2 G4 dendrimer and amino acids. • The more polar the amino acid side chain, the more exothermic the effects of the direct interactions with dendrimer. • Macromolecule of PAMAM-NH 2 G4 dendrimer can coordinate 20 to 40 molecules of amino acid. -- Abstract: The interactions of PAMAM-NH 2 G4 dendrimer with selected natural amino acids (Gly, Ala, Val, Leu, Ile, Phe, Ser, Thr, Met, Asn, Gln, Pro and Trp) in aqueous solutions were measured with the use of the techniques of calorimetric titration and dilution calorimetry. The results of calorimetric measurements show strong interactions between PAMAM-NH 2 G4 dendrimer and amino acids with polar substituents. A macromolecule of PAMAM-NH 2 G4 dendrimer can coordinate 20 to 40 molecules of amino acid

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.

Pulsating potentiometric titration technique for assay of dissolved oxygen in water at trace level.

Science.gov (United States)

Sahoo, P; Ananthanarayanan, R; Malathi, N; Rajiniganth, M P; Murali, N; Swaminathan, P

2010-06-11

A simple but high performance potentiometric titration technique using pulsating sensors has been developed for assay of dissolved oxygen (DO) in water samples down to 10.0 microg L(-1) levels. The technique involves Winkler titration chemistry, commonly used for determination of dissolved oxygen in water at mg L(-1) levels, with modification in methodology for accurate detection of end point even at 10.0 microg L(-1) levels DO present in the sample. An indigenously built sampling cum pretreatment vessel has been deployed for collection and chemical fixing of dissolved oxygen in water samples from flowing water line without exposure to air. A potentiometric titration facility using pulsating sensors developed in-house is used to carry out titration. The power of the titration technique has been realised in estimation of very dilute solution of iodine equivalent to 10 microg L(-1) O(2). Finally, several water samples containing dissolved oxygen from mg L(-1) to microg L(-1) levels were successfully analysed with excellent reproducibility using this new technique. The precision in measurement of DO in water at 10 microg L(-1) O(2) level is 0.14 (n=5), RSD: 1.4%. Probably for the first time a potentiometric titration technique has been successfully deployed for assay of dissolved oxygen in water samples at 10 microg L(-1) levels. Copyright 2010 Elsevier B.V. All rights reserved.

Pulsating potentiometric titration technique for assay of dissolved oxygen in water at trace level

International Nuclear Information System (INIS)

Sahoo, P.; Ananthanarayanan, R.; Malathi, N.; Rajiniganth, M.P.; Murali, N.; Swaminathan, P.

2010-01-01

A simple but high performance potentiometric titration technique using pulsating sensors has been developed for assay of dissolved oxygen (DO) in water samples down to 10.0 μg L -1 levels. The technique involves Winkler titration chemistry, commonly used for determination of dissolved oxygen in water at mg L -1 levels, with modification in methodology for accurate detection of end point even at 10.0 μg L -1 levels DO present in the sample. An indigenously built sampling cum pretreatment vessel has been deployed for collection and chemical fixing of dissolved oxygen in water samples from flowing water line without exposure to air. A potentiometric titration facility using pulsating sensors developed in-house is used to carry out titration. The power of the titration technique has been realised in estimation of very dilute solution of iodine equivalent to 10 μg L -1 O 2 . Finally, several water samples containing dissolved oxygen from mg L -1 to μg L -1 levels were successfully analysed with excellent reproducibility using this new technique. The precision in measurement of DO in water at 10 μg L -1 O 2 level is 0.14 (n = 5), RSD: 1.4%. Probably for the first time a potentiometric titration technique has been successfully deployed for assay of dissolved oxygen in water samples at 10 μg L -1 levels.

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)

Application of cause-and-effect analysis to potentiometric titration.

Science.gov (United States)

Kufelnicki, A; Lis, S; Meinrath, G

2005-08-01

A first attempt has been made to interpret physicochemical data from potentiometric titration analysis in accordance with the complete measurement-uncertainty budget approach (bottom-up) of ISO and Eurachem. A cause-and-effect diagram is established and discussed. Titration data for arsenazo III are used as a basis for this discussion. The commercial software Superquad is used and applied within a computer-intensive resampling framework. The cause-and-effect diagram is applied to evaluation of seven protonation constants of arsenazo III in the pH range 2-10.7. The data interpretation is based on empirical probability distributions and their analysis by second-order correct confidence estimates. The evaluated data are applied in the calculation of a speciation diagram including uncertainty estimates using the probabilistic speciation software Ljungskile.

Implementation of a pharmacist-managed heart failure medication titration clinic.

Science.gov (United States)

Martinez, Amanda S; Saef, Jerold; Paszczuk, Anna; Bhatt-Chugani, Hetal

2013-06-15

The development, implementation, and initial results of a pharmacist-managed heart failure (HF) medication titration clinic are described. In a quality-improvement initiative at a Veterans Affairs health care system, clinical pharmacists were incorporated into the hospital system's interprofessional outpatient HF clinic. In addition, a separate pharmacist-managed HF medication titration clinic was established, in which pharmacists were granted an advanced scope of practice and prescribing privileges, enabling them to initiate and adjust medication dosages under specific protocols jointly established by cardiology and pharmacy staff. Pharmacists involved in the titration clinic tracked patients' daily body weight, vital signs, and volume status using telephone-monitoring technology and via patient interviews. A retrospective chart review comparing achievement of target doses of angiotensin-converting enzyme inhibitor (ACEI), angiotensin-receptor blocker (ARB), and β-blocker therapies in a group of patients (n = 28) whose dosage titrations were carried out by nurses or physicians prior to implementation of the pharmacist-managed HF medication titration clinic and a group of patients (n = 27) enrolled in the medication titration clinic during its first six months of operation indicated that target ACEI and ARB doses were achieved in a significantly higher percentage of pharmacist-managed titration clinic enrollees (52.9% versus 31%, p = 0.007). Patients enrolled in the pharmacist-managed HF medication titration clinic also had a significantly higher rate of attainment of optimal β-blocker doses (49% versus 24.7%, p = 0.012). Implementation of a pharmacist-managed HF medication titration clinic increased the percentage of patients achieving optimal ACEI, ARB, and β-blocker dosages.

Titration in the treatment of the more troubled patient.

Science.gov (United States)

Winer, J A; Ornstein, E D

2001-01-01

This article defines and discusses a modification of technique recommended by the authors in the psychoanalytic treatment of more troubled patients--a modification they call titration. Titration is defined as a conscious decision by the analyst to increase or decrease assistance (or gratification) gradually, in order to facilitate the analytic process. The authors emphasize the complexity of decisions in treatment by focusing on the decision-making processes that titration requires. Guidelines and a case vignette are presented. The authors conclude by considering some of the politics involved in the introduction of technique modifications, the salience of the titration concept, and directions for further exploration.

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.

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

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.

Chip calorimetry for evaluation of biofilm treatment with biocides, antibiotics, and biological agents.

Science.gov (United States)

Morais, Frida Mariana; Buchholz, Friederike; Maskow, Thomas

2014-01-01

Any growth or bioconversion in biofilms is accompanied by the release of heat. The heat (in J) is tightly related to the stoichiometry of the respective process via law of Hess, and the heat production rate (in W or J/s) is additionally related to the process kinetics. This heat and the heat production rate can nowadays be measured by modern calorimetry with extremely high sensitivity. Flow-through calorimetry allows the measurement of bioprocesses in biofilms in real time, without the need of invasive sample preparation and disturbing of biofilm processes. Furthermore, it can be applied for long-term measurements and is even applicable to turbid media. Chip or miniaturized calorimeters have the additional advantages of extremely short thermal equilibration times and the requirement of very small amounts of media and chemicals. The precision of flow-through chip calorimeters (about 3 mW/L) allows the detection of early stages of biofilm development (about 10(5) bacteria cm(-2)).

Calorimetric approach of ions adsorption; Approche calorimetrique de l'absorption d'ions

Energy Technology Data Exchange (ETDEWEB)

Lantenois, S. [Montpellier-2 Univ., 34 (France)

2006-07-01

The aim of this work is to obtain experimentally thermodynamic data of ions adsorption by micro-calorimetry. Different thermal effects can be measured on different silicon oxides (Spherosil or SBA-15) and with different cations (Cd{sup 2+} and Pb{sup 2+}). The solids are studied in the same experimental conditions in a NaNO{sub 3} solution (10{sup -1} M) at pH of 5 or 7 (adjusted by addition of NaOH or HNO{sub 3}) in terms of the hydrolysis pH of the adsorbed cation. The aqueous solution is a NaNO{sub 3} (10{sup -1} M) solution containing Cd(NO{sub 3}){sub 2} (pH 7.0) or Pb(NO{sub 3}){sub 2} (pH 5.0) at different concentrations (between 5*10{sup -4} and 10{sup -2} M). The thermal effect due to the addition of this solution is measured by titration calorimetry and by flux calorimetry. The complementarity of these two techniques is developed during this study where the titration calorimetry has been used for studying the thermal effects at low concentrations in metallic cations. The flux calorimetry has allowed to analyze systems at stronger concentration in metallic cations and to study the desorption of these cations. This study shows that the thermal effect bound to the surfaces reactivity is composed of a combination of factors. Factors such as surface charges density (pH and protonation deprotonation reactions), the samples preparation (previous calcination) or the capacity of cations to hydrolyze can be revealed by micro-calorimetry. (O.M.)

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.

A reliable and feasible qPCR strategy for titrating AAV vectors.

Science.gov (United States)

Wang, Feng; Cui, Xiuling; Wang, Mingxi; Xiao, Weidong; Xu, Ruian

2013-07-05

Previous studies have revealed that traditional real-time quantitative PCR (qPCR) underestimates adeno-associated virus (AAV) titer. Because the inverted terminal repeat (ITR) exists in all AAV vectors, the only remaining element from the wild genome could form special configurations to interfere with qPCR titration. To solve this problem, a modified and universal qPCR method was tested and established. In this work, there was a great variation in titration of ssAAV2-EGFP (Enhanced Green Fluorescence Protein) and scAAV2-EGFP genome by traditional qPCR. For ssAAV2-EGFP, the highest titer was found by using the targeting EGFP primers and the lowest titer was measured by those targeting bovine growth hormone polyA element (pBGH) primers. Experimental data were reverse for ssAAV2-EGFP and scAAV2-EGFP. Here we report an improved and universal SmaI qPCR method, based on cleaving all ITRs in AAV2 genome by SmaI with several advantages: (1) impact of all ITRs in ssAAV2 and scAAV2 was dismissed; (2) titers increased remarkably, up to 7-fold, especially for scAAV2; (3) the variation of titers was reduced when different primers were applied. A similar phenomenon was also observed in other ssAAV2 and scAAV2 products when the range of titration was at 3×107 to 7×109 V.G/µl in this study. This modified qPCR strategy can increase rAAV' titer and reduce titration variance, possibly become a universal method for titrating AAV vectors.

Differential scanning calorimetry techniques: applications in biology and nanoscience.

Science.gov (United States)

Gill, Pooria; Moghadam, Tahereh Tohidi; Ranjbar, Bijan

2010-12-01

This paper reviews the best-known differential scanning calorimetries (DSCs), such as conventional DSC, microelectromechanical systems-DSC, infrared-heated DSC, modulated-temperature DSC, gas flow-modulated DSC, parallel-nano DSC, pressure perturbation calorimetry, self-reference DSC, and high-performance DSC. Also, we describe here the most extensive applications of DSC in biology and nanoscience.

Differential Scanning Calorimetry Techniques: Applications in Biology and Nanoscience

OpenAIRE

Gill, Pooria; Moghadam, Tahereh Tohidi; Ranjbar, Bijan

2010-01-01

This paper reviews the best-known differential scanning calorimetries (DSCs), such as conventional DSC, microelectromechanical systems-DSC, infrared-heated DSC, modulated-temperature DSC, gas flow-modulated DSC, parallel-nano DSC, pressure perturbation calorimetry, self-reference DSC, and high-performance DSC. Also, we describe here the most extensive applications of DSC in biology and nanoscience.

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.

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 ...

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)

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

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.

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.

Laser Calorimetry Spectroscopy for ppm-level Dissolved Gas Detection and Analysis.

Science.gov (United States)

K S, Nagapriya; Sinha, Shashank; R, Prashanth; Poonacha, Samhitha; Chaudhry, Gunaranjan; Bhattacharya, Anandaroop; Choudhury, Niloy; Mahalik, Saroj; Maity, Sandip

2017-02-20

In this paper we report a newly developed technique - laser calorimetry spectroscopy (LCS), which is a combination of laser absorption spectroscopy and calorimetry - for the detection of gases dissolved in liquids. The technique involves determination of concentration of a dissolved gas by irradiating the liquid with light of a wavelength where the gas absorbs, and measuring the temperature change caused by the absorbance. Conventionally, detection of dissolved gases with sufficient sensitivity and specificity was done by first extracting the gases from the liquid and then analyzing the gases using techniques such as gas chromatography. Using LCS, we have been able to detect ppm levels of dissolved gases without extracting them from the liquid. In this paper, we show the detection of dissolved acetylene in transformer oil in the mid infrared (MIR) wavelength (3021 nm) region.

Synthesized cellulose/succinic anhydride as an ion exchanger. Calorimetry of divalent cations in aqueous suspension

Energy Technology Data Exchange (ETDEWEB)

Melo, Julio C.P. [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil); Silva Filho, Edson C. [LIMAV, Federal University of Piaui, 64049-550 Teresina, Piaui (Brazil); Santana, Sirlane A.A. [Departamento de Quimica/CCET, Universidade Federal do Maranhao, Av. dos Portugueses S/N, Campus do Bacanga, 65080-540 Sao Luiz, MA (Brazil); Airoldi, Claudio, E-mail: airoldi@iqm.unicamp.br [Institute of Chemistry, University of Campinas, UNICAMP, P.O. Box 6154, 13084-971 Campinas, SP (Brazil)

2011-09-20

Highlights: {yields} Synthetic route based on anhydride melting point. {yields} Cellulosic biopolymer/anhydride as ion exchanger. {yields} Calorimetry of cation exchange at solid/liquid interface. {yields} Favorable thermodynamic data of exchanging process. - Abstract: A synthetic route to a biopolymer/anhydride ion exchanger adds cellulose directly to molten succinic anhydride in a quasi solvent-free procedure. An amount of 3.07 {+-} 0.05 mmol of pendant groups incorporated onto the polymeric structure, which was characterized by elemental analysis, solid state carbon NMR, infrared, X-ray and thermogravimetry. The new polysaccharide is able to exchange cations from aqueous solution through a batchwise methodology, to obtain 2.46 {+-} 0.09 mmol g{sup -1} for divalent cobalt and nickel cations. The net thermal effects obtained from calorimetric titrations gave endothermic values of 3.81 {+-} 0.02 and 2.35 {+-} 0.01 kJ mol{sup -1}. The spontaneity of this ion-exchange process reflected in negative Gibbs energies and also a positive entropic contribution. These thermodynamic data at the solid/liquid interface suggests a favorable ion exchange process for this anchored biopolymer, for cation removal from the environment.

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

Energy Technology Data Exchange (ETDEWEB)

Ubelhor, Ryan, E-mail: ryan.ubelhor@navy.mil [Naval Surface Warfare Center, Crane Division, 300 Highway 361, Crane, IN 47522 (United States); Ellison, Daniel [Science Applications International Corporation, 300 Highway 361, Crane, IN 47522 (United States); Pierce, Cecilia [Naval Surface Warfare Center, Crane Division, 300 Highway 361, Crane, IN 47522 (United States)

2015-04-20

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

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

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.

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.

Plutonium titration by controlled potential coulometry; Dosage du plutonium par coulometrie a potentiel impose

Energy Technology Data Exchange (ETDEWEB)

Leguay, N.

2011-07-01

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)

The Potentiometric Titration of Filtrates from the Bachmann Process

Science.gov (United States)

1942-06-23

SCIENTIFIC RESEARCH AND DEVELOP11ENT The Potentiometric Titration of Filtrates from the Bachmann Process (OD-12) by F. C. Whitmore OSRD No. 654... Potentiometric Titration of Synthetic Mixtures. A? Nitric Acid-Acetic Acid. A sample of 60 ml. glacial acetic acid war diluted to 200 ml. with distilled...i4flinflr?fj3 TADLE 1 CO) |S?lDBnTl» POTENTIOMETRIC TITRATION OF SYNTHETIC t’.IXTURES WITH CONCENTRATED AJKDNIUM HYDROXIDE A; unonium HNO-j- AcOfi Ky

A novel approach for high precision rapid potentiometric titrations: application to hydrazine assay.

Science.gov (United States)

Sahoo, P; Malathi, N; Ananthanarayanan, R; Praveen, K; Murali, N

2011-11-01

We propose a high precision rapid personal computer (PC) based potentiometric titration technique using a specially designed mini-cell to carry out redox titrations for assay of chemicals in quality control laboratories attached to industrial, R&D, and nuclear establishments. Using this technique a few microlitre of sample (50-100 μl) in a total volume of ~2 ml solution can be titrated and the waste generated after titration is extremely low comparing to that obtained from the conventional titration technique. The entire titration including online data acquisition followed by immediate offline analysis of data to get information about concentration of unknown sample is completed within a couple of minutes (about 2 min). This facility has been created using a new class of sensors, viz., pulsating sensors developed in-house. The basic concept in designing such instrument and the salient features of the titration device are presented in this paper. The performance of the titration facility was examined by conducting some of the high resolution redox titrations using dilute solutions--hydrazine against KIO(3) in HCl medium, Fe(II) against Ce(IV) and uranium using Davies-Gray method. The precision of titrations using this innovative approach lies between 0.048% and 1.0% relative standard deviation in different redox titrations. With the evolution of this rapid PC based titrator it was possible to develop a simple but high precision potentiometric titration technique for quick determination of hydrazine in nuclear fuel dissolver solution in the context of reprocessing of spent nuclear fuel in fast breeder reactors. © 2011 American Institute of Physics

''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

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.

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.

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)

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.

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

Continuing Studies on Lead/Scintillating Fibres Calorimetry (LFC)

CERN Multimedia

2002-01-01

Starting from the results obtained in the framework of the LAA Project~2B, we propose a continuation of the R&D on lead/scintillating fibres calorimetry (``spaghetti calorimetry''), including further tests on the old calorimeter prototypes and the construction and testing of new prototypes. The main results we pursue concern the performances of a projective calorimeter built with new, cheaper, techniques and the radiation hardness of the scintillating fibres, the optimization of a preshower detector system is also studied.

Acid-base titrations by stepwise addition of equal volumes of titrant with special reference to automatic titrations-III Presentation of a fully automatic titration apparatus and of results supporting the theories given in the preceding parts.

Science.gov (United States)

Pehrsson, L; Ingman, F

1977-02-01

This paper forms Part III of a series in which the first two parts describe methods for evaluating titrations performed by stepwise addition of equal volumes of titrant. The great advantage of these methods is that they do not require an accurate calibration of the electrode system. This property makes the methods very suitable for routine work. e.g., in automatic analysis. An apparatus for performing such titrations automatically is presented. Further, results of titrations of monoprotic acids, a diprotic acid, an ampholyte, a mixture of an acid with its conjugate base, and mixtures of two acids with a small difference between the stability constants are given. Most of these titrations cannot be evaluated by the Gran or Hofstee methods but yield results having errors of the order of 0.1% if the methods proposed in Parts I and II of this series are employed. The advantages of the method of stepwise addition of equal volumes of titrant combined with the proposed evaluation methods, in comparison with common methods such as titration to a preset pH, are that all the data are used in the evaluation, permitting a statistical treatment and giving better possibilities for tracing systematic errors.

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)

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.

Microcalorimetric and potentiometric titration studies on the adsorption of copper by P. putida and B. thuringiensis and their composites with minerals.

Science.gov (United States)

Fang, Linchuan; Cai, Peng; Li, Pengxiang; Wu, Huayong; Liang, Wei; Rong, Xingmin; Chen, Wenli; Huang, Qiaoyun

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 (DeltaH(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. Copyright 2010 Elsevier B.V. All rights reserved.

Potentiometric titration curves of aluminium salt solutions and its ...

African Journals Online (AJOL)

Potentiometric titration curves of aluminium salt solutions and its species conversion ... of aluminium salt solutions under the moderate slow rate of base injection. ... silicate radical, and organic acid radical on the titration curves and its critical ...

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.

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.)

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.

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%

Potentiometric titrations of molybdenum and vanadium in aqueous and mixed so lvents

International Nuclear Information System (INIS)

Das, S.K.; Dhaneshwar, R.G.

1990-01-01

Potentiometric titration method was developed for molybdenum, employing different electrode systems. Molybdenum(VI) is reduced to molybdenum(V) by ferrous solution in presence of phosphoric acid and then titrated with potassium dichromate. It was found that ferrous concentration should be five times more than molybdenum and phosphoric acid should be 1.0 ml for 0.1N titration and 0.5 ml for lower concentration titrations. The method is also applicable to vanadium titrations. Employing Au/SCE and Pt/SCE systems, it was observed that generally curve heights obtained for platinum electrode are higher than those for gold electrode. Also for both the electrode systems, the curve heights for vanadium titrations were found to be more than those for molybdenum. Lower limits of titrations for Au/SCE system are 0.01N for molybdenum and 0.0001N for vanadium, whereas for Pt/SCE system, the lower limits obtained were 0.01N for both molybdenum and vanadium titrations. In order to improve the sensitivities of the method, the bimetallic electrode systems Au/Pt and Pt/Au were employed. Au/Pt system was found to give better results than Pt/Au systems. Addition of organic solvent was found to have beneficial effects for titrations of 0.001N and below. Methanol was found to be a better solvent than ethanol. Molybdenum titrations, at 0.0001N level could be performed in methanol with Au/Pt system, which is to b e generally preferred than Pt/Au system. (author). 7 refs., 3 tabs

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

. 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...

Thermometric titrations of amines with nitrosyl perchlorate in acetonitrile solvent.

Science.gov (United States)

Gündüz, T; Kiliç, E; Cakirer, O

1996-05-01

Thirteen aliphatic and four aromatic amines, namely diethylamine, triethylamine, n-propylamine, di-n-propylamine, tri-n-butylamine, isopropylamine, di-isopropylamine, n-butylamine, di-n-butylamine, tri-n-butylamine, isobutylamine, sec-butylamine, tert-butylamine, aniline, N,N-dimethylaniline, 2-nitroaniline and 4-nitroaniline were titrated thermometrically with nitrosyl perchlorate in acetonitrile solvent. All the aliphatic amines gave very well-shaped thermometric titration curves. The calculated recovery values of the amines were very good. In comparison, the aromatic amines, aniline and N,N-dimethylaniline gave rather well-shaped titration curves, but the recovery values were fairly low. 2-Nitro- and 4-nitro anilines gave no thermometric response at all. The heats of reaction of the amines with nitrosyl perchlorate are rather high. However, the average heat of reaction of the aromatic amines is approximately two-thirds that of the average heat of the aliphatic amines. To support this method all the amines were also titrated potentiometrically and very similar results to those obtained with the thermometric method are seen. The nitrosyl ion is a Lewis acid, strong enough to titrate quantitatively aliphatic amines in acetonitrile solvent, but not strong enough to titrate aromatic amines at the required level in the same solvent.

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.

The determination of the enthalpy of formation and the enthalpy increment of Cd0.5 Te0.5 by Calvet calorimetry

International Nuclear Information System (INIS)

Agarwal, R.; Venugopal, V.; Sood, D.D.

1993-01-01

In the present study the enthalpy of formation of Cd 0.5 Te 0.5 compound at 785 K were determined from the two elements by direct reaction calorimetry using two different types of set-ups. The enthalpy increment values were measured by drop technique in Calvet calorimetry. (author). 3 refs., 4 tabs

Thermometric Titration for Rapid Determination of Trace Water in Jet Fuel

Directory of Open Access Journals (Sweden)

Jian-Qiang Hu

2017-01-01

Full Text Available 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 indicated spiked water contents. The obtained results between TMT and Karl Fischer titration have been proven to be in accord. But, the duration of titration merely spends 3–5 min in the whole process, greatly shortening the detected time. Therefore, rapid and accurate determination of trace water in a jet fuel can be realized by TMT.

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)

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.

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.

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…

Thermodynamics of micellization from heat-capacity measurements.

Science.gov (United States)

Šarac, Bojan; Bešter-Rogač, Marija; Lah, Jurij

2014-06-23

Differential scanning calorimetry (DSC), the most important technique for studying the thermodynamics of structural transitions of biological macromolecules, is seldom used in quantitative thermodynamic studies of surfactant micellization/demicellization. The reason for this could be ascribed to an insufficient understanding of the temperature dependence of the heat capacity of surfactant solutions (DSC data) in terms of thermodynamics, which leads to problems with the design of experiments and interpretation of the output signals. We address these issues by careful design of DSC experiments performed with solutions of ionic and nonionic surfactants at various surfactant concentrations, and individual and global mass-action model analysis of the obtained DSC data. Our approach leads to reliable thermodynamic parameters of micellization for all types of surfactants, comparable with those obtained by using isothermal titration calorimetry (ITC). In summary, we demonstrate that DSC can be successfully used as an independent method to obtain temperature-dependent thermodynamic parameters for micellization. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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)

Extensive studies on CeF3 crystals, a good candidate for electromagnetic calorimetry at future accelerators

International Nuclear Information System (INIS)

Auffray, E.; Baccaro, S.; Beckers, T.; Benhammou, Y.; Belsky, A.N.; Borgia, B.; Boutet, D.; Chipaux, R.; Dafinei, I.; De Notaristefani, F.; Depasse, P.; Dujardin, C.; El Mamouni, H.; Faure, J.L.; Fay, J.; Goyot, M.; Gupta, S.K.; Gurtu, A.; Hillemanns, H.; Ille, B.; Kirn, T.; Lebeau, M.; Lebrun, P.; Lecoq, P.; Mares, J.A.; Martin, J.P.; Mikhailin, V.V.; Moine, B.; Nelissen, J.; Nikl, M.; Pedrini, C.; Raghavan, R.; Sahuc, P.; Schmitz, D.; Schneegans, M.; Schwenke, J.; Tavernier, S.; Topa, V.; Vasil'ev, A.N.; Vivargent, M.; Walder, J.P.

1996-01-01

In the framework of its search for new heavy, fast and radiation hard scintillators for calorimetry at future colliders, the Crystal Clear Collaboration performed a systematic investigation of the properties and of the scintillation and radiation damage mechanisms of CeF 3 monocrystals. Many samples of various dimensions up to 3 x 3 x 28 cm 3 were produced by industry and characterised in the laboratories by different methods such as: optical transmission, light yield and decay time measurements, excitation and emission spectra, gamma and neutron irradiations. The results of these measurements are discussed. The measured light yield is compared to the theoretical expectations. Tests in high energy electron beams on a crystal matrix were also performed. The suitability of CeF 3 for calorimetry at high rate machines is confirmed. Production and economical considerations are discussed. (orig.)

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

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.

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.

Digital movie-based on automatic titrations.

Science.gov (United States)

Lima, Ricardo Alexandre C; Almeida, Luciano F; Lyra, Wellington S; Siqueira, Lucas A; Gaião, Edvaldo N; Paiva Junior, Sérgio S L; Lima, Rafaela L F C

2016-01-15

This study proposes the use of digital movies (DMs) in a flow-batch analyzer (FBA) to perform automatic, fast and accurate titrations. The term used for this process is "Digital movie-based on automatic titrations" (DMB-AT). A webcam records the DM during the addition of the titrant to the mixing chamber (MC). While the DM is recorded, it is decompiled into frames ordered sequentially at a constant rate of 26 frames per second (FPS). The first frame is used as a reference to define the region of interest (ROI) of 28×13pixels and the R, G and B values, which are used to calculate the Hue (H) values for each frame. The Pearson's correlation coefficient (r) is calculated between the H values of the initial frame and each subsequent frame. The titration curves are plotted in real time using the r values and the opening time of the titrant valve. The end point is estimated by the second derivative method. A software written in C language manages all analytical steps and data treatment in real time. The feasibility of the method was attested by application in acid/base test samples and edible oils. Results were compared with classical titration and did not present statistically significant differences when the paired t-test at the 95% confidence level was applied. The proposed method is able to process about 117-128 samples per hour for the test and edible oil samples, respectively, and its precision was confirmed by overall relative standard deviation (RSD) values, always less than 1.0%. Copyright © 2015 Elsevier B.V. All rights reserved.

Radiation damage study for silicon calorimetry: Summary of first year's activity

International Nuclear Information System (INIS)

Russ, J.S.

1988-01-01

In the first contract year of this activity at Carnegie-Mellon we have had two major objectives. These were to devise and test a non-intrusive means to measure the energy and spatial profiles of the neutrons generated in a hadronic cascade at high energy; and to study the calibration systematics of silicon diode detectors as a prelude to their evaluation for SSC calorimetry. These objectives have been carried out, as are described in this paper. In addition we have recoded the ORNL detector simulation program HETC to operate on a VAX and are working on the conversion of the low energy neutron transport program MORSE. These programs are used heavily at Oak Ridge (Gabriel and coworkers) for cascade studies. For silicon calorimetry one wants to have more control over the energy deposition routines, especially in MORSE. Unfortunately, MORSE is heavily-laden with machine code, and its conversion is going slowly. 11 refs., 5 figs

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

When acid-base titrations are carried out in unusual conditions

Directory of Open Access Journals (Sweden)

Domenico De Marco

2012-12-01

Full Text Available Uncommon aspects in acid-base titrations are presented, which occur in titrations between both mono- and/or poly-functional acid and bases but are rarely introduced in ordinary analytical chemistry courses.

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

Spectrophotometric titrations: Application to the determination of some elements in uranium solutions

International Nuclear Information System (INIS)

L'Her, M.

1967-01-01

The aim of this work is the application of spectrophotometric titrations to the analysis of uranium-containing solutions. We have been led to examine the general principles involved in these titrations, and we give a brief outline of these principles. In the first part we deal therefore with spectrophotometric titrations from a general point of view, examining their fundamental principle, their practical execution as well as the various possibilities of the method. The advantage of the titration are examined, in particular that of lending itself simultaneous determination of two species. The possibility of applying these spectrophotometric titrations to the analysis of uranium-containing solutions is the subject of the second part of this report: the dosage of a few species in uranium (VI) solutions is described. To this second part is added an experimental appendix consisting of a description of the apparatus, as well as of the operational techniques used for certain titrations, in particular those involving solutions containing uranium. (author) [fr

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.

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.

Phase behavior and micellar properties of carboxylic acid end group modified pluronic surfactants

NARCIS (Netherlands)

Custers, J.P.A.; Broeke, van den L.J.P.; Keurentjes, J.T.F.

2007-01-01

The micellar behavior of three different carboxylic acid end standing (CAE) surfactants has been characterized using conductometry, differential scanning calorimetry, isothermal titration calorimetry, and dynamic light scattering. The CAE surfactants are modified high molecular weight Pluronic

Kinetics of solid-gas reactions characterized by scanning AC nano-calorimetry with application to Zr oxidation

International Nuclear Information System (INIS)

Xiao, Kechao; Lee, Dongwoo; Vlassak, Joost J.

2014-01-01

Scanning AC nano-calorimetry is a recently developed experimental technique capable of measuring the heat capacity of thin-film samples of a material over a wide range of temperatures and heating rates. Here, we describe how this technique can be used to study solid-gas phase reactions by measuring the change in heat capacity of a sample during reaction. We apply this approach to evaluate the oxidation kinetics of thin-film samples of zirconium in air. The results confirm parabolic oxidation kinetics with an activation energy of 0.59 ± 0.03 eV. The nano-calorimetry measurements were performed using a device that contains an array of micromachined nano-calorimeter sensors in an architecture designed for combinatorial studies. We demonstrate that the oxidation kinetics can be quantified using a single sample, thus enabling high-throughput mapping of the composition-dependence of the reaction rate.

Effect of dissolved oxygen on two bacterial pathogens examined using ATR-FTIR spectroscopy, microelectrophoresis, and potentiometric titration.

Science.gov (United States)

Castro, Felipe D; Sedman, Jacqueline; Ismail, Ashraf A; Asadishad, Bahareh; Tufenkji, Nathalie

2010-06-01

The effects of dissolved oxygen tension during bacterial growth and acclimation on the cell surface properties and biochemical composition of the bacterial pathogens Escherichia coli O157:H7 and Yersinia enterocolitica are characterized. Three experimental techniques are used in an effort to understand the influence of bacterial growth and acclimation conditions on cell surface charge and the composition of the bacterial cell: (i) electrophoretic mobility measurements; (ii) potentiometric titration; and (iii) ATR-FTIR spectroscopy. Potentiometric titration data analyzed using chemical speciation software are related to measured electrophoretic mobilities at the pH of interest. Titration of bacterial cells is used to identify the major proton-active functional groups and the overall concentration of these cell surface ligands at the cell membrane. Analysis of titration data shows notable differences between strains and conditions, confirming the appropriateness of this tool for an overall charge characterization. ATR-FTIR spectroscopy of whole cells is used to further characterize the bacterial biochemical composition and macromolecular structures that might be involved in the development of the net surficial charge of the organisms examined. The evaluation of the integrated intensities of HPO(2)(-) and carbohydrate absorption bands in the IR spectra reveals clear differences between growth protocols. Taken together, the three techniques seem to indicate that the dissolved oxygen tension during cell growth or acclimation can noticeably influence the expression of cell surface molecules and the measurable cell surface charge, though in a strain-dependent fashion.

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

International Nuclear Information System (INIS)

Janot, N.; Benedetti, M. F.; Janot, N.; Reiller, P. E.; Korshin, G. V.

2010-01-01

Potentiometric titration is a common method to characterize dissolved organic matter (DOM) reactivity. Because of the sensitivity of pH electrodes, it is necessary to work with very high DOM (≥1 g/L) concentrations that are unrealistic compared to those found in natural waters (0. 1 to 100 mg/L). To obtain proton binding data for concentrations closer to environmental values, spectroscopic titration methodology is a viable alternative to traditional potentiometric titrations. Spectrophotometric titrations and UV visible spectra of a diluted solution of purified Aldrich humic acid (5 mg(DOC)/L) are used to estimate changes in proton binding moieties as function of pH and ionic strength after calculation of differential absorbance spectra variations. After electrostatic correction of spectrophotometric data, there is a linear operational correlation between spectrophotometric and potentiometric data which can be used as a transfer function between the two properties. Spectrophotometric titrations are then used to determine the changes of humic acid protonation after adsorption onto alpha-alumina. (authors)

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

Energy Technology Data Exchange (ETDEWEB)

Janot, N.; Benedetti, M. F. [Univ Paris Diderot, Lab Geochim Eaux, UMR CNRS 7154, IPGP, F-75025 Paris 13 (France); Janot, N.; Reiller, P. E. [CE Saclay, CEA DEN DANS DPC SECR, Lab Speciat Radionucleides and Mol, F-91191 Gif Sur Yvette (France); Korshin, G. V. [Univ Washington, Dept Civil and Environm Engn, Seattle, WA 98195 (United States)

2010-07-01

Potentiometric titration is a common method to characterize dissolved organic matter (DOM) reactivity. Because of the sensitivity of pH electrodes, it is necessary to work with very high DOM ({>=}1 g/L) concentrations that are unrealistic compared to those found in natural waters (0. 1 to 100 mg/L). To obtain proton binding data for concentrations closer to environmental values, spectroscopic titration methodology is a viable alternative to traditional potentiometric titrations. Spectrophotometric titrations and UV visible spectra of a diluted solution of purified Aldrich humic acid (5 mg(DOC)/L) are used to estimate changes in proton binding moieties as function of pH and ionic strength after calculation of differential absorbance spectra variations. After electrostatic correction of spectrophotometric data, there is a linear operational correlation between spectrophotometric and potentiometric data which can be used as a transfer function between the two properties. Spectrophotometric titrations are then used to determine the changes of humic acid protonation after adsorption onto alpha-alumina. (authors)

Application of calorimetry and thermodynamics to critical problems in materials science

International Nuclear Information System (INIS)

Atake, Tooru

2009-01-01

Calorimetry and thermodynamic studies have long been playing a very important role in the research fields of fundamental science and technology. Some topics and examples of thermodynamics studies are given, and the details are explained on the basis of the present author's experience, focusing attention to application of adiabatic calorimetry and thermodynamics to solve critical problems in materials science: (1) condensed gas calorimetry and third law entropy, (2) phase transition and polymorphism in simple molecular crystals, (3) incommensurate phase transitions, (4) particle size effects on the phase transitions in ferroelectric/ferroelastic crystals, (5) relaxor ferroelectrics and multi-ferroics, and some other topics in materials science and technology

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.

Benefit of slow titration of paroxetine to treat depression in the elderly.

Science.gov (United States)

Olgiati, Paolo; Bajo, Emanuele; Serretti, Alessandro

2014-11-01

Paroxetine is commonly used to treat depression in the elderly; however, titration issues have been raised. Rapid titration may lead to increased anxiety and early dropout. The aim of this cost-utility analysis was to compare the potential benefit of standard (10 mg the first day) versus slow titration (2.5 mg gradually increased). Clinical analysis was based on a naturalistic trial integrated with a decision-analytic model representing second treatments for those who initially did not respond and for dropout cases. Treatment setting was a public outpatient center for mental disorders in Italy. Service use data were estimated from best practice guidelines, whereas costs (Euros; 2012) were retrieved from Italian official sources. Slow titration approach produced 0.031 more quality-adjusted life years (remission rate: 57% vs 44% in standard titration group) at an incremental cost of €5.53 (generic paroxetine) and €54.54 (brand paroxetine syrup). Incremental cost-effectiveness ratio (ICER) values were €159 and €1768, respectively, in favor of slow titration approach. Cost-effectiveness threshold, defined as ICER titration of paroxetine in older depressed patients. However, these findings, in part based on simulated data, need to be replicated in clinical trials. Copyright © 2014 John Wiley & Sons, Ltd.

Graphical evaluation of complexometric titration curves.

Science.gov (United States)

Guinon, J L

1985-04-01

A graphical method, based on logarithmic concentration diagrams, for construction, without any calculations, of complexometric titration curves is examined. The titration curves obtained for different kinds of unidentate, bidentate and quadridentate ligands clearly show why only chelating ligands are usually used in titrimetric analysis. The method has also been applied to two practical cases where unidentate ligands are used: (a) the complexometric determination of mercury(II) with halides and (b) the determination of cyanide with silver, which involves both a complexation and a precipitation system; for this purpose construction of the diagrams for the HgCl(2)/HgCl(+)/Hg(2+) and Ag(CN)(2)(-)/AgCN/CN(-) systems is considered in detail.

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

Sensitivity of the acid-base properties of clays to the methods of preparation and measurement. 2. Evidence from continuous potentiometric titrations.

Science.gov (United States)

Duc, Myriam; Gaboriaud, Fabien; Thomas, Fabien

2005-09-01

The effects of experimental procedures on the acid-base consumption titration curves of montmorillonite suspension were studied using continuous potentiometric titration. For that purpose, the hysteresis amplitudes between the acid and base branches were found to be useful to systematically evaluate the impacts of storage conditions (wet or dried), the atmosphere in titration reactor, the solid-liquid ratio, the time interval between successive increments, and the ionic strength. In the case of storage conditions, the increase of the hysteresis was significantly higher for longer storage of clay in suspension and drying procedures compared to "fresh" clay suspension. The titration carried out under air demonstrated carbonate contamination that could only be cancelled by performing experiments under inert gas. Interestingly, the increase of the time intervals between successive increments of titrant strongly emphasized the amplitude of hysteresis, which could be correlated with the slow kinetic process specifically observed for acid addition in acid media. Thus, such kinetic behavior is probably associated with dissolution processes of clay particles. However, the resulting curves recorded at different ionic strengths under optimized conditions did not show the common intersection point required to define point of zero charge. Nevertheless, the ionic strength dependence of the point of zero net proton charge suggested that the point of zero charge of sodic montmorillonite could be estimated as lower than 5.

[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.

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.

On the binding of calcium by micelles composed of carboxy-modified pluronics measured by means of differential potentiometric titration and modelled with a self-consistent-field theory

NARCIS (Netherlands)

Lauw, Y.; Leermakers, F.A.M.; Cohen Stuart, M.A.; Pinheiro, J.P.; Custers, J.P.A.; Broeke, van den L.J.P.; Keurentjes, J.T.F.

2006-01-01

We perform differential potentiometric titration measurements for the binding of Ca2+ ions to micelles composed of the carboxylic acid end-standing Pluronic P85 block copolymer (i.e., CAE-85 (COOH-(EO)(26)-(PO)(39)-(EO)(26)-COOH)). Two different ion-selective electrodes (ISEs) are used to detect the

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

Initial Evaluation of a Titration Appliance for Temporary Treatment of Obstructive Sleep Apnea.

Science.gov (United States)

Levendowski, Daniel J; Morgan, Todd; Westbrook, Philip

2012-01-01

Custom oral appliances that adjustably advance the mandible provide superior outcomes when treating patients with moderate or severe sleep apnea. Custom appliances, however, are expensive, must be fitted by a dentist, and the likelihood of successful outcomes are difficult to predict. An inexpensive trial appliance, if proven efficacious, might be used to predict custom appliance outcomes or to provide temporary therapeutic benefit. The aim of this initial study was to assess the treatment efficacy of a novel titration oral appliance with that of an optimized custom appliance. Seventeen patients, treated with a custom oral appliance for at least one year, successfully completed a three-night home sleep test. The baseline obstructive sleep apnea severity was established on Night 1 with seven patients exhibiting severe, six moderate and four mild apnea/hypopnea indexes. Patients were randomly assigned to wear their custom appliance or the titration appliance on Nights 2 and 3. Significant reductions in the mean overall and supine apnea indexes (p titration and custom appliances. The proportion of patients who exhibited at least a 50% reduction in the overall apnea index and supine apnea/hypopnea were similar for the titration and custom appliance (~60%). The custom appliance reduced the overall apnea/hypopnea index by 50% in a greater proportion of the patients compared to the titration appliance (77% vs. 53%). The titration appliance significantly reduced the degree of hypoxic exposure across sleep disordered breathing events overall (p titration appliance, but preferred the titration appliance to no therapy. The titration appliance may be useful in assessing oral appliance treatment efficacy. When set to 70% of maximum protrusion, the titration appliance may provide immediate, temporary therapeutic benefit.

Persistent benefits of slow titration of paroxetine in a six-month follow-up.

Science.gov (United States)

Olgiati, Paolo; Serretti, Alessandro

2015-09-01

Paroxetine titration may be difficult in older individuals as they are more sensitive to side effects. The current study extends to 6 months our previously published report in which paroxetine was started at 2.5 mg/day and slowly increased by 2.5 mg on alternate days (slow titration) or rapidly titrated to target dose from 10 mg/day (standard titration) in a naturalistic setting. Here, the follow-up period was extended to 26 weeks. We performed an intent-to-treat analysis of 47 subjects from the original sample (major depressive disorder and/or generalized anxiety disorder (GAD); >60 years of age). Missing evaluations were replaced by last observations carried forward. GAD was included as a stratification factor. Patients in whom paroxetine was slowly up-titrated were more likely to remit (84.0% vs 54.5%; p = 0.028) and had lower core depression (p = 0.0015) and psychic anxiety levels (p = 0.006) after 26 weeks. Dropout rate was 20% in the slow titration group compared with 77.3% in the standard titration arm (p titration groups in the subsample without GAD. Despite some limitations, these findings suggest that paroxetine treatment should be started at lower doses in older depressed patients and slowly up-titrated. This strategy would allow to increase antidepressant response and the likelihood of completing treatment cycle in patients with high anxiety levels and GAD comorbidity. Copyright © 2015 John Wiley & Sons, Ltd.

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

Monitoring Acid–Base Titrations on Wax Printed Paper Microzones Using a Smartphone

Directory of Open Access Journals (Sweden)

Sandro A. Nogueira

2017-05-01

Full Text Available This study describes the use of a smartphone for monitoring acid–base titrations on wax printed paper microzones. An array of twelve microzones of 5 mm diameter each was wax printed on filter paper. The analytical performance of the proposed devices was explored with acid–base titrations examples, where jaboticaba peel extract was used as a natural pH indicator. The color intensity was captured using a smartphone and analyzed through a free App named Photometrix®. Before titrations, color intensity versus pH was calibrated to be used as a reference in titrations as (i strong acid versus strong base; (ii strong base versus strong acid; and (iii weak acid versus strong base. In all examples, images were obtained after the addition of each aliquot of titrant solutions. The obtained titration curves showed the same behavior as the conventional titration curves. After evaluating the feasibility of the proposed methodology, the concentration level of acetic acid was obtained in three vinegar samples. Although the obtained values ranged from 5% to 8% compared to the concentrations on the conventional method, the proposed methodology presented high analytical reliability. The calculated concentrations of acetic acid in three samples ranged from 3.87% to 3.93%, and the proposed methodology did not significantly differ from classic acid–base titration at a confidence level of 95%. The acid–base titration on paper-based devices is outstanding, since any titration can be completed within 5 min using 20 µL volumes. Besides, the use of a smartphone to capture images followed by analysis in a free app offers simplicity to all users. The proposed methodology arises as a new strand to be exploited in the diffusion of the analytical chemistry education field as well as an alternative for quantitative analysis with extremely simplified instrumentation.

Extensive studies on CeF{sub 3} crystals, a good candidate for electromagnetic calorimetry at future accelerators

Energy Technology Data Exchange (ETDEWEB)

Auffray, E.; Baccaro, S.; Beckers, T.; Benhammou, Y.; Belsky, A.N.; Borgia, B.; Boutet, D.; Chipaux, R.; Dafinei, I.; De Notaristefani, F.; Depasse, P.; Dujardin, C.; El Mamouni, H.; Faure, J.L.; Fay, J.; Goyot, M.; Gupta, S.K.; Gurtu, A.; Hillemanns, H.; Ille, B.; Kirn, T.; Lebeau, M.; Lebrun, P.; Lecoq, P.; Mares, J.A.; Martin, J.P.; Mikhailin, V.V.; Moine, B.; Nelissen, J.; Nikl, M.; Pedrini, C.; Raghavan, R.; Sahuc, P.; Schmitz, D.; Schneegans, M.; Schwenke, J.; Tavernier, S.; Topa, V.; Vasil`ev, A.N.; Vivargent, M.; Walder, J.P. [CERN, Geneva (Switzerland)]|[ENEA Casaccia, INFN Rome, Rome (Italy)]|[VUB, Vrije Universiteit Brussels, Brussels (Belgium)]|[IPN of Lyon, IN2P3-CNRS and Universite Claude Bernard, Villeurbanne (France)]|[Synchrotron Radiation Laboratory, Moscow State University, Moscow (Russian Federation)]|[INFN Rome, Rome (Italy)]|[LPCML of Lyon, CNRS and Universite Claude Bernard, Villeurbanne (France)]|[CEA DSM/DAPNIA, CE-Saclay (France)]|[Tara Institute of Fundamental Research, Bombay (India)]|[Physics Institute, RWTH Aachen, Aachen (Germany)]|[LAPP, IN2P3-CNRS, Annecy-le-Vieux (France)]|[Institute of Physics, Academy of Sciences of Czech Republic, Prague (Czech Republic)]|[Institute of Atomic Physics (IFA), Bucharest (Romania)

1996-12-11

In the framework of its search for new heavy, fast and radiation hard scintillators for calorimetry at future colliders, the Crystal Clear Collaboration performed a systematic investigation of the properties and of the scintillation and radiation damage mechanisms of CeF{sub 3} monocrystals. Many samples of various dimensions up to 3 x 3 x 28 cm{sup 3} were produced by industry and characterised in the laboratories by different methods such as: optical transmission, light yield and decay time measurements, excitation and emission spectra, gamma and neutron irradiations. The results of these measurements are discussed. The measured light yield is compared to the theoretical expectations. Tests in high energy electron beams on a crystal matrix were also performed. The suitability of CeF{sub 3} for calorimetry at high rate machines is confirmed. Production and economical considerations are discussed. (orig.).

Thermometric Titration for Rapid Determination of Trace Water in Jet Fuel

OpenAIRE

Hu, Jian-Qiang; Zhang, Jian-Jian; Yang, Shi-Zhao; Xin, Yong-Liang; Guo, Li; Yao, Ting

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...

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

Liquid argon calorimetry for the SSC

International Nuclear Information System (INIS)

Gordon, H.A.

1990-01-01

Liquid argon calorimetry is a mature technique. However, adapting it to the challenging environment of the SSC requires a large amount of R ampersand D. The advantages of the liquid argon approach are summarized and the issues being addressed by the R ampersand D program are described. 18 refs

The predictive value of drug-induced sleep endoscopy for CPAP titration in OSA patients.

Science.gov (United States)

Lan, Ming-Chin; Hsu, Yen-Bin; Lan, Ming-Ying; Huang, Yun-Chen; Kao, Ming-Chang; Huang, Tung-Tsun; Chiu, Tsan-Jen; Yang, Mei-Chen

2017-12-15

The aim of this study was to identify possible upper airway obstructions causing a higher continuous positive airway pressure (CPAP) titration level, utilizing drug-induced sleep endoscopy (DISE). A total of 76 patients with obstructive sleep apnea (OSA) underwent CPAP titration and DISE. DISE findings were recorded using the VOTE classification system. Polysomnographic (PSG) data, anthropometric variables, and patterns of airway collapse during DISE were analyzed with CPAP titration levels. A significant association was found between the CPAP titration level and BMI, oxygen desaturation index (ODI), apnea-hypopnea index (AHI), and neck circumference (NC) (P CPAP titration level (P CPAP titration level and any other collapse at the tongue base or epiglottis. By analyzing PSG data, anthropometric variables, and DISE results with CPAP titration levels, we can better understand possible mechanisms resulting in a higher CPAP titration level. We believe that the role of DISE can be expanded as a tool to identify the possible anatomical structures that may be corrected by oral appliance therapy or surgical intervention to improve CPAP compliance.

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

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...... and EE in the field. In this study, four Shetland ponies were used to explore the effect of feeding on CO(2) production and EE measured simultaneously by IC and (13)C-BT. The ponies were individually housed in respiration chambers and received either a single oral or intravenous (IV) bolus dose of (13)C......-bicarbonate at the three different feeding times. Feeding time affected the CO(2) production (P

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.

Rapid Inpatient Titration of Intravenous Treprostinil for Pulmonary Arterial Hypertension: Safe and Tolerable.

Science.gov (United States)

El-Kersh, Karim; Ruf, Kathryn M; Smith, J Shaun

There is no standard protocol for intravenous treprostinil dose escalation. In most cases, slow up-titration is performed in the outpatient setting. However, rapid up-titration in an inpatient setting is an alternative that provides opportunity for aggressive treatment of common side effects experienced during dose escalation. In this study, we describe our experience with inpatient rapid up-titration of intravenous treprostinil. This was a single-center, retrospective study in which we reviewed the data of subjects with pulmonary arterial hypertension treated at our center who underwent inpatient rapid up-titration of intravenous treprostinil. Our treprostinil dose escalation protocol included initiation at 2 ng·kg·min with subsequent up-titration by 1 ng·kg·min every 6 to 8 hours as tolerated by side effects. A total of 16 subjects were identified. Thirteen subjects were treprostinil naive (naive group), and 3 subjects were receiving subcutaneous treprostinil but were hospitalized for further intravenous up-titration of treprostinil dose (nonnaive group). In the naive group, the median maximum dose achieved was 20 ng·kg·min with an interquartile range (IQR) of 20-23 ng·kg·min. The median up-titration interval was 6 days (IQR: 4-9). In the nonnaive group, the median maximum dose achieved was 20 ng·kg·min (range: 17-30). The median up-titration interval was 8.5 days (range: 1.5-11). Overall, the median maximum dose achieved was 20 ng·kg·min (IQR: 20-23.5), and the median up-titration interval was 6 days (IQR: 4.6-9.25), with no reported significant adverse hemodynamic events. In patients with pulmonary arterial hypertension, rapid inpatient titration of intravenous treprostinil is safe and tolerable.

The determination of titratable acidity and total tannins in red wine

OpenAIRE

Rajković Miloš B.; Sredović Ivana D.

2009-01-01

Titration acidity and content of total tannins in mass-market red wines are analyzed in this paper. The content of total acids in wine, expressed through wine acid, was analyzed by potentiometric titration on 7.00 pH value. According to titratable acidity in analyzed wines, all wines (only) with analyzed parameters according to Regulations about wine quality. The analysis of differential potentiometric curves shows that these curves can give the answer to the question if non organic substance...

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

Direct calorimetry of free-moving eels with manipulated thyroid status

Science.gov (United States)

van Ginneken, Vincent; Ballieux, Bart; Antonissen, Erik; van der Linden, Rob; Gluvers, Ab; van den Thillart, Guido

2007-02-01

In birds and mammals, the thyroid gland secretes the iodothyronine hormones of which tetraiodothyronine (T4) is less active than triiodothyronine (T3). The action of T3 and T4 is calorigenic and is involved in the control of metabolic rate. Across all vertebrates, thyroid hormones also play a major role in differentiation, development and growth. Although the fish thyroidal system has been researched extensively, its role in thermogenesis is unclear. In this study, we measured overall heat production to an accuracy of 0.1 mW by direct calorimetry in a free-moving European eel ( Anguilla anguilla L.) with different thyroid status. Hyperthyroidism was induced by injection of T3 and T4, and hypothyroidism was induced with phenylthiourea. The results show for the first time at the organismal level, using direct calorimetry, that neither overall heat production nor overall oxygen consumption in eels is affected by hyperthyroidism. Therefore, we conclude that the thermogenic metabolism-stimulating effect of thyroid hormones (TH) is not present with a cold-blooded fish species like the European eel. This supports the concept that TH does not stimulate thermogenesis in poikilothermic species.

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

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

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.

Characterization of the phase transformations in shape-memory alloys by modulated differential scanning calorimetry

International Nuclear Information System (INIS)

Wei, Z.G.; Sandstroem, R.

1999-01-01

Modulated differential scanning calorimetry (MDSC) is a recently developed calorimetric technique, which has demonstrated some significant advantages over the conventional differential scanning calorimetry (DSC). By separating the reversing quantity from the non-reversing component in the total thermal events, it provides some new information that can not be obtained from the conventional DSC. The technique has been applied to various polycrystalline and single crystalline shape-memory alloys, including Cu-Zn-Al, Cu-Al-Ni, Ti-Ni(Cu), Ni-Mn-Ga and Fe-Mn-Si, to characterize the martensitic transformations, bainitic transformation, chemical and magnetic ordering transitions, atomic reordering and other kinetic relaxation processes in the alloys. The preliminary results of the MDSC measurements are summarized and the interpretation of the MDSC results and some factors affecting the results are discussed. (orig.)

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.

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.

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.

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

Two-phase titration of cerium(III) by permanganate

International Nuclear Information System (INIS)

Lazarev, A.I.; Lazareva, V.I.; Gerko, V.V.

1987-01-01

This paper presents a method for the two-phase titrimetric determination of cerium(III) with permanganate which does not require an expenditure of sugar and preliminary removal of chlorides and nitrates. The interaction of cerium(III) with permanganate at room temperature was studied as a function of the pH, the concentration of pyrophosphate, tetraphenylphosphonium (TPP), permanganate, and extraneous compounds, the rate of titration, and the time of stay of the solution in air before titration. The investigations were conducted according to the following methodology: water, solution of cerium(III) pyrophosphate, and TPP were introduced into an Erlenmeyer flask with a side branch near the bottom for clearer observation of the color of the chloroform phase. The authors established the given pH value, poured the water into a volume of 50 ml, and added chloroform. The result was titrated with permanganate solutions of various concentrations until a violet color appeared in the chloroform phase

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

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.

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)

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.

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

Advanced ion beam calorimetry for the test facility ELISE

International Nuclear Information System (INIS)

Nocentini, R.; Fantz, U.; Franzen, P.; Fröschle, M.; Heinemann, B.; Riedl, R.; Ruf, B.; Wünderlich, D.; Bonomo, F.; Pimazzoni, A.; Pasqualotto, R.

2015-01-01

The negative ion source test facility ELISE (Extraction from a Large Ion Source Experiment) is in operation since beginning of 2013 at the Max-Planck-Institut für Plasmaphysik (IPP) in Garching bei München. The large radio frequency driven ion source of ELISE is about 1×1 m 2 in size (1/2 the ITER source) and can produce a plasma for up to 1 h. Negative ions can be extracted and accelerated by an ITER-like extraction system made of 3 grids with an area of 0.1 m 2 , for 10 s every 3 minutes. A total accelerating voltage of up to 60 kV is available, i.e. a maximum ion beam power of about 1.2 MW can be produced. ELISE is equipped with several beam diagnostic tools for the evaluation of the beam characteristics. In order to evaluate the beam properties with a high level of detail, a sophisticated diagnostic calorimeter has been installed in the test facility at the end of 2013, starting operation in January 2014. The diagnostic calorimeter is split into 4 copper plates with separate water calorimetry for each of the plates. Each calorimeter plate is made of 15×15 copper blocks, which act as many separate inertial calorimeters and are attached to a copper plate with an embedded cooling circuit. The block geometry and the connection with the cooling plate are optimized to accurately measure the time-averaged power of the 10 s ion beam. The surface of the blocks is covered with a black coating that allows infrared (IR) thermography which provides a 2D profile of the beam power density. In order to calibrate the IR thermography, 48 thermocouples are installed in as many blocks, arranged in two vertical and two horizontal rows. The paper describes the beam calorimetry in ELISE, including the methods used for the IR thermography, the water calorimetry and the analytical methods for beam profile evaluation. It is shown how the maximum beam inhomogeneity amounts to 13% in average. The beam divergence derived by IR thermography ranges between 1° and 4° and

The ion-sensitive field effect transistor in rapid acid-base titrations

NARCIS (Netherlands)

Bos, M.; Bergveld, Piet; van Veen-Blaauw, A.M.W.

1979-01-01

Ion-sensitive field effect transistors (ISFETs) are used as the pH sensor in rapid acid—base titrations. Titration speeds at least five times greater than those with glass electrodes are possible for accuracies better than ±1%.

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.

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

Simultaneous determination of equivalence volumes and acid dissociation constants from potentiometric titration data.

Science.gov (United States)

Papanastasiou, G; Ziogas, I

1995-06-01

New iterative methods for analysis of potentiometric titration data of (a) mixtures of weak monoprotic acids with their conjugate bases, (b) solutions of polyprotic (di- and triprotic) acids, and (c) mixtures of two diprotic acids are presented. These methods, using data exclusively resulting from the acidic region of the titration curve permits the accurate determination of the analytical concentration of one or more acids even if the titration is stopped well before the end point of the titration. For the titration of a solution containing a conjugate acid/base pair, the proposed procedure enables the extraction of the initial composition of the mixture, as well as the dissociation constant of the concerned acid. Thus, it is possible by this type of analysis to distinguish whether a weak acid has been contaminated by a strong base and define the extent of the contamination. On the other hand, for the titration of polyprotic acids, the proposed approach enables the extraction of the accurate values of the equivalence volume and the dissociation constants K(i) even when the ionization stages overlap. Finally, for the titration of a mixture of two diprotic acids the proposed procedure enables the determination of the composition of the mixture even if the sum of the concentrations of the acids is not known. This method can be used in the analysis of solutions containing two diastereoisomeric forms of a weak diprotic acid. The test of the proposed procedures by means of ideal and Monte Carlo simulated data revealed that these methods are fairly applicable even when the titration data are considerably obscured by 'noise' or contain an important systematic error. The proposed procedures were also successfully applied to experimental titration data.

Thermodynamics of the interaction of γ-cyclodextrin and tauro- and glyco-conjugated bile salts

DEFF Research Database (Denmark)

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

2013-01-01

The structural differences in the interaction between natural γ-cyclodextrin and bile salts common in rat, dog and man was were investigated by 1H-ROESY and 13C NMR and molecular modeling and the thermodynamic parameters of the reaction by isothermal titration calorimetry. The γ-cyclodextrin was ......The structural differences in the interaction between natural γ-cyclodextrin and bile salts common in rat, dog and man was were investigated by 1H-ROESY and 13C NMR and molecular modeling and the thermodynamic parameters of the reaction by isothermal titration calorimetry. The γ...

A model for oxygen conservation associated with titration during pediatric oxygen therapy.

Directory of Open Access Journals (Sweden)

Grace Wu

Full Text Available Continuous oxygen treatment is essential for managing children with hypoxemia, but access to oxygen in low-resource countries remains problematic. Given the high burden of pneumonia in these countries and the fact that flow can be gradually reduced as therapy progresses, oxygen conservation through routine titration warrants exploration.To determine the amount of oxygen saved via titration during oxygen therapy for children with hypoxemic pneumonia.Based on published clinical data, we developed a model of oxygen flow rates needed to manage hypoxemia, assuming recommended flow rate at start of therapy, and comparing total oxygen used with routine titration every 3 minutes or once every 24 hours versus no titration.Titration every 3 minutes or every 24 hours provided oxygen savings estimated at 11.7% ± 5.1% and 8.1% ± 5.1% (average ± standard error of the mean, n = 3, respectively. For every 100 patients, 44 or 30 kiloliters would be saved-equivalent to 733 or 500 hours at 1 liter per minute.Ongoing titration can conserve oxygen, even performed once-daily. While clinical validation is necessary, these findings could provide incentive for the routine use of pulse oximeters for patient management, as well as further development of automated systems.

Concentration-related response potentiometric titrations to study the interaction of small molecules with large biomolecules.

Science.gov (United States)

Hamidi-Asl, Ezat; Daems, Devin; De Wael, Karolien; Van Camp, Guy; Nagels, Luc J

2014-12-16

In the present paper, the utility of a special potentiometric titration approach for recognition and calculation of biomolecule/small-molecule interactions is reported. This approach is fast, sensitive, reproducible, and inexpensive in comparison to the other methods for the determination of the association constant values (Ka) and the interaction energies (ΔG). The potentiometric titration measurement is based on the use of a classical polymeric membrane indicator electrode in a solution of the small-molecule ligand. The biomolecule is used as a titrant. The potential is measured versus a reference electrode and transformed into a concentration-related signal over the entire concentration interval, also at low concentrations, where the millivolt (y-axis) versus log canalyte (x-axis) potentiometric calibration curve is not linear. In the procedure, Ka is calculated for the interaction of cocaine with a cocaine binding aptamer and with an anticocaine antibody. To study the selectivity and cross-reactivity, other oligonucleotides and aptamers are tested, as well as other small ligand molecules such as tetrakis(4-chlorophenyl)borate, metergoline, lidocaine, and bromhexine. The calculated Ka compared favorably to the value reported in the literature using surface plasmon resonance. The potentiometric titration approach called "concentration-related response potentiometry" is used to study molecular interaction for seven macromolecular target molecules and four small-molecule ligands.

flower extract as an improvised indicator in acid – base titration

African Journals Online (AJOL)

USER

laboratory practical with an instructional material that is useful, economical, simple and accurate for the said titration. Therefore, it is recommended for integrated science and chemistry instructions. Keywords: Flower, acid, base, indicator, titration. INTRODUCTION. In Nigeria, factors militating against science education.

Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

Energy Technology Data Exchange (ETDEWEB)

Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Gordon Center for Integrated Science, 929 E. 57th Street, Chicago, Illinois 60637 (United States); Nash, P. [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Chen, X.Q.; Wei, P. [Materials processing Modeling Division, Shenyang National Laboratory for Materials Science, Institute of Metals Research, 72 Wenhua Road, Shenyang City (China)

2015-06-05

Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb{sub 3}Sc{sub 5}(−61.3 ± 2.9); PbTi{sub 4}(−16.6 ± 2.4); Pb{sub 3}Y{sub 5}(−64.8 ± 3.6); Pb{sub 3}Zr{sub 5}(−50.6 ± 3.1); PbNb{sub 3}(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd{sub 3}(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available.

Correct titration of non-drugs and some other methodological issues.

Science.gov (United States)

Beneke, M; Rasmus, W; Rød, I S; Fritze, J

1994-01-01

Doctors' prescription and dosing behaviour was investigated using data from 9 clinical trials in 550 patients treated with psychotropics. 7 trials were conducted under double- and 2 under single-blind conditions. In 3 of these trials, oral and i.m. preparations were used demanding a double-dummy design. All patients were evaluated on a weekly or 2-week basis using psychopathological rating scales (i.e. Hamilton Anxiety Scale, Hamilton Depression Scale, Clinical Global Impressions, Simpson and Angus EPS). It was found that (a) oral-medication titration was 3- to 4-fold more broad-ranging than i.m. medication titration, (b) oral placebo was titrated to the same extent as the oral investigational drugs, and (c) the titration schedule did not follow protocol requirements. Moreover, the average doses in all drug and placebo groups were the same. Concomitant medication like sleep inducers was found to be more closely related to doctors' habits than to actual medical need. Independent of trial and investigational drug, 10-33% of all patients received additional sleep inducers.

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.

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.)

Protometric thermometric titrations of sparingly soluble compounds in water in the presence of n-octanol.

Science.gov (United States)

Burgot, G; Burgot, J-L

2002-10-15

Thermometric titrimetry permits titration of acido-basic compounds in water in the presence of n-octanol. n-Octanol permits the solubilization of protolytes and moreover may also displace the equilibria of the titration reactions. Hydrochlorides of highly insoluble derivatives such as phenothiazine derivatives can be titrated with satisfactory accuracy and precision by sodium hydroxide despite their high pK(a) values. Likewise barbiturate salts can be titrated by hydrochloric acid. In the case of some salts, the methodology may permit the sequential titration of the ion and counter ion. Copyright 2002 Elsevier Science B.V.

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...

Origin of two time-scale regimes in potentiometric titration of metal oxides. A replica kinetic Monte Carlo study

International Nuclear Information System (INIS)

Zarzycki, Piotr P.; Rosso, Kevin M.

2009-01-01

Replica Kinetic Monte Carlo simulations were used to study the characteristic time scales of potentiometric titration of the metal oxides and (oxy)hydroxides. The effect of surface heterogeneity and surface transformation on the titration kinetics were also examined. Two characteristic relaxation times are often observed experimentally, with the trailing slower part attributed to surface non-uniformity, porosity, polymerization, amorphization, and other dynamic surface processes induced by unbalanced surface charge. However, our simulations show that these two characteristic relaxation times are intrinsic to the proton binding reaction for energetically homogeneous surfaces, and therefore surface heterogeneity or transformation do not necessarily need to be invoked. However, all such second-order surface processes are found to intensify the separation and distinction of the two kinetic regimes. The effect of surface energetic-topographic non-uniformity, as well dynamic surface transformation, interface roughening/smoothing were described in a statistical fashion. Furthermore, our simulations show that a shift in the point-of-zero charge is expected from increased titration speed and the pH-dependence of the titration measurement error is in excellent agreement with experimental studies.

Origin of two time-scale regimes in potentiometric titration of metal oxides. A replica kinetic Monte Carlo study.

Science.gov (United States)

Zarzycki, Piotr; Rosso, Kevin M

2009-06-16

Replica kinetic Monte Carlo simulations were used to study the characteristic time scales of potentiometric titration of the metal oxides and (oxy)hydroxides. The effect of surface heterogeneity and surface transformation on the titration kinetics were also examined. Two characteristic relaxation times are often observed experimentally, with the trailing slower part attributed to surface nonuniformity, porosity, polymerization, amorphization, and other dynamic surface processes induced by unbalanced surface charge. However, our simulations show that these two characteristic relaxation times are intrinsic to the proton-binding reaction for energetically homogeneous surfaces, and therefore surface heterogeneity or transformation does not necessarily need to be invoked. However, all such second-order surface processes are found to intensify the separation and distinction of the two kinetic regimes. The effect of surface energetic-topographic nonuniformity, as well dynamic surface transformation, interface roughening/smoothing were described in a statistical fashion. Furthermore, our simulations show that a shift in the point-of-zero charge is expected from increased titration speed, and the pH-dependence of the titration measurement error is in excellent agreement with experimental studies.

Automated high-pressure titration system with in situ infrared spectroscopic detection

Energy Technology Data Exchange (ETDEWEB)

Thompson, Christopher J., E-mail: chris.thompson@pnnl.gov; Martin, Paul F.; Chen, Jeffrey; Schaef, Herbert T.; Rosso, Kevin M.; Felmy, Andrew R.; Loring, John S. [Pacific Northwest National Laboratory, Richland, Washington 99352 (United States); Benezeth, Pascale [Géosciences Environnement Toulouse (GET), CNRS-Université de Toulouse, 31400 Toulouse (France)

2014-04-15

A fully automated titration system with infrared detection was developed for investigating interfacial chemistry at high pressures. The apparatus consists of a high-pressure fluid generation and delivery system coupled to a high-pressure cell with infrared optics. A manifold of electronically actuated valves is used to direct pressurized fluids into the cell. Precise reagent additions to the pressurized cell are made with calibrated tubing loops that are filled with reagent and placed in-line with the cell and a syringe pump. The cell's infrared optics facilitate both transmission and attenuated total reflection (ATR) measurements to monitor bulk-fluid composition and solid-surface phenomena such as adsorption, desorption, complexation, dissolution, and precipitation. Switching between the two measurement modes is accomplished with moveable mirrors that direct the light path of a Fourier transform infrared spectrometer into the cell along transmission or ATR light paths. The versatility of the high-pressure IR titration system was demonstrated with three case studies. First, we titrated water into supercritical CO{sub 2} (scCO{sub 2}) to generate an infrared calibration curve and determine the solubility of water in CO{sub 2} at 50 °C and 90 bar. Next, we characterized the partitioning of water between a montmorillonite clay and scCO{sub 2} at 50 °C and 90 bar. Transmission-mode spectra were used to quantify changes in the clay's sorbed water concentration as a function of scCO{sub 2} hydration, and ATR measurements provided insights into competitive residency of water and CO{sub 2} on the clay surface and in the interlayer. Finally, we demonstrated how time-dependent studies can be conducted with the system by monitoring the carbonation reaction of forsterite (Mg{sub 2}SiO{sub 4}) in water-bearing scCO{sub 2} at 50 °C and 90 bar. Immediately after water dissolved in the scCO{sub 2}, a thin film of adsorbed water formed on the mineral surface

Automated high-pressure titration system with in situ infrared spectroscopic detection

International Nuclear Information System (INIS)

Thompson, Christopher J.; Martin, Paul F.; Chen, Jeffrey; Schaef, Herbert T.; Rosso, Kevin M.; Felmy, Andrew R.; Loring, John S.; Benezeth, Pascale

2014-01-01

A fully automated titration system with infrared detection was developed for investigating interfacial chemistry at high pressures. The apparatus consists of a high-pressure fluid generation and delivery system coupled to a high-pressure cell with infrared optics. A manifold of electronically actuated valves is used to direct pressurized fluids into the cell. Precise reagent additions to the pressurized cell are made with calibrated tubing loops that are filled with reagent and placed in-line with the cell and a syringe pump. The cell's infrared optics facilitate both transmission and attenuated total reflection (ATR) measurements to monitor bulk-fluid composition and solid-surface phenomena such as adsorption, desorption, complexation, dissolution, and precipitation. Switching between the two measurement modes is accomplished with moveable mirrors that direct the light path of a Fourier transform infrared spectrometer into the cell along transmission or ATR light paths. The versatility of the high-pressure IR titration system was demonstrated with three case studies. First, we titrated water into supercritical CO 2 (scCO 2 ) to generate an infrared calibration curve and determine the solubility of water in CO 2 at 50 °C and 90 bar. Next, we characterized the partitioning of water between a montmorillonite clay and scCO 2 at 50 °C and 90 bar. Transmission-mode spectra were used to quantify changes in the clay's sorbed water concentration as a function of scCO 2 hydration, and ATR measurements provided insights into competitive residency of water and CO 2 on the clay surface and in the interlayer. Finally, we demonstrated how time-dependent studies can be conducted with the system by monitoring the carbonation reaction of forsterite (Mg 2 SiO 4 ) in water-bearing scCO 2 at 50 °C and 90 bar. Immediately after water dissolved in the scCO 2 , a thin film of adsorbed water formed on the mineral surface, and the film thickness increased with time as the

SU-E-T-267: Development of the Compact Graphite Calorimetry System for the High Energy Photon Beam

Energy Technology Data Exchange (ETDEWEB)

Kim, B. C.; Kim, I. J.; Kim, J. H.; Yi, C. Y. [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2015-06-15

Purpose: Graphite calorimeter systems are used for the absolute photon dosimetry. But many electronics are demanded in order to measure the tiny temperature changes. Minimizing the control system is needed to make a portable graphite calorimeter. Methods: A Domen-type graphite calorimetry system is constructing to measure the absorbed dose of the high energy photon beam. The graphite calorimeter divided into three parts, Core, Jacket, and Shield. In order to measure the temperature rising of the core due to the radiation accurately, the temperatures of the jacket and the shield should be controlled properly. A commercial temperature controller (Model 350, Lake Shore Cryogenics) was used to minimize the size of control system for making a portable graphite calorimetry system at the cost of the measurement uncertainty. The PID control of the jacket is conducted by the software (LabView) and Model 350 maintain the temperature of shield. Results: Our design value of the heat deposition power in the core is 0.04 mW for the dose rate of 3 Gy/min where the temperature sensitivity of the graphite is 1.4 mK/Gy. While the residuals of the Steinhart-hart equation fitting for the core thermistor were less than 0.1 mK, the temperature resolution of Model 350 is 1 mK. The temperature of the shield was kept within the 5 mK when the room temperature variation was about 0.5 K. Conclusion: The resolution of Model 350 for the temperature measurement and control is not good enough as the control system for the compact graphite calorimetry system. But The performance of Model 350 is good enough to maintain the temperature of the shield constantly. The Model 350 will be replaced by the AC resistance bridge (Model 372, Lake Shore Cryogenics) for the core temperature measurement and the jacket control.

Calorimetric Evidence about the Application of the Concept of CMC to Asphaltene Self-Association

DEFF Research Database (Denmark)

Garcia, Daniel Merino; Andersen, Simon Ivar

2005-01-01

that asphaltenes may also have a concentration at which self-association occurs (CMC). This article presents evidence found by calorimetry and spectroscopic techniques, that suggest that this concept may not be adequate for asphaltene self-association in toluene solutions. Isothermal titration calorimetry has been...

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

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

The SimpleMix study with biphasic insulin aspart 30: a randomized controlled trial investigating patient-driven titration versus investigator-driven titration.

Science.gov (United States)

Gao, Yan; Luquez, Cecilia; Lynggaard, Helle; Andersen, Henning; Saboo, Banshi

2014-12-01

The study aimed to confirm the efficacy, through non-inferiority, of patient-driven versus investigator-driven titration of biphasic insulin aspart 30 (BIAsp 30) in terms of glycemic control assessed by HbA1c change. SimpleMix was a 20 week, open-label, randomized, two-armed, parallel-group, multicenter study in five countries (Argentina, China, India, Poland, and the UK). Patients with type 2 diabetes were randomized into either patient-driven or investigator-driven BIAsp 30 titration groups. Non-inferiority of patient-driven vs. investigator-driven titration based on change in HbA1c from baseline to week 20 could not be demonstrated. Mean (SE) estimated change from baseline to week 20 was -0.72 (0.08)% in the patient-driven group and -0.97 (0.08)% in the investigator-driven group; estimated difference 0.25% (95% CI: 0.04; 0.46). Estimated mean change (SE) in fasting plasma glucose from baseline to week 20 was similar between groups: -0.94 (0.21) mmol/L for patient-driven and -1.07 (0.22) mmol/L for investigator-driven (difference non-significant). Both treatment arms were well tolerated, and hypoglycemic episode rates were similar between groups, with a rate ratio of 0.77 (95% CI: 0.54; 1.09; p = 0.143) for all hypoglycemic episodes and 0.78 (95% CI: 0.42; 1.43; p = 0.417) for nocturnal hypoglycemic episodes. Non-inferiority of patient-driven versus investigator-driven titration with regard to change from baseline to end-of-treatment HbA1c could not be confirmed. It is possible that a clinic visit 12 weeks after intensification of treatment with BIAsp 30 in patients with type 2 diabetes inadequately treated with basal insulin may benefit patient-driven titration of BIAsp 30. A limitation of the study was the relatively small number of patients recruited in each country, which does not allow country-specific analyses to be performed. Overall, treatment with BIAsp 30 was well tolerated in both treatment groups.

Insights into optimal basal insulin titration in type 2 diabetes: Results of a quantitative survey.

Science.gov (United States)

Berard, Lori; Bonnemaire, Mireille; Mical, Marie; Edelman, Steve

2018-02-01

Basal insulin (BI) treatment initiation and dose titration in type 2 diabetes (T2DM) are often delayed. Such "clinical inertia" results in poor glycaemic control and high risk of long-term complications. This survey aimed to determine healthcare professional (HCP) and patient attitudes to BI initiation and titration. An online survey (July-August 2015) including HCPs and patients with T2DM in the USA, France and Germany. Patients were ≥18 years old and had been on BI for 6 to 36 months, or discontinued BI within the previous 12 months. Participants comprised 386 HCPs and 318 people with T2DM. While >75% of HCPs reported discussing titration at the initiation visit, only 16% to 28% of patients remembered such discussions, many (32%-42%) were unaware of the need to titrate BI, and only 28% to 39% recalled mention of the time needed to reach glycaemic goals. Most HCPs and patients agreed that more effective support tools to assist BI initiation/titration are needed; patients indicated that provision of such tools would increase confidence in self-titration. HCPs identified fear of hypoglycaemia, failure to titrate in the absence of symptoms, and low patient motivation as important titration barriers. In contrast, patients identified weight gain, the perception that titration meant worsening disease, frustration over the time to reach HbA1c goals and fear of hypoglycaemia as major factors. A disconnect exists between HCP- and patient-perceived barriers to effective BI titration. To optimize titration, strategies should be targeted to improve HCP-patient communication, and provide support and educational tools. © 2017 The Authors. Diabetes, Obesity and Metabolism published by John Wiley & Sons Ltd.

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.

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.

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.

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.)

Molybdenum (6) determination by the method of high-frequency and pH titration

International Nuclear Information System (INIS)

Lukianets, I.G.; Kulish, N.G.

1981-01-01

A possibility to determine Mo(6) using the method of high frequency and pH-metric titration is investigated. By means of the high frequency contact R-cell Mo(6) titration is performed using different precipitators: 8-oxiquinoline, lead nitrate and acetate and silver nitrate. It is established that the best conditions are achieved during titration of 67.2-1343 mg/10 ml Mo(6) with lead acetate (pH 4.5-6.5). Relative standard deviation Ssub(r) constitutes 0.005 pH-metric titration of Mo(6) with complexone 3 is studied. The range of Mo(6) concentrations determined constitutes 13.43-134.3 mg at pH initial value of 3.5-5.5. Relative standard deviation Ssub(r) constitutes 0.003. Techniques of molybdenum determination in ferromolybdenum using the method of high frequency and pH-metric titration are developed [ru

Small-volume potentiometric titrations: EPR investigations of Fe-S cluster N2 in mitochondrial complex I.

Science.gov (United States)

Wright, John J; Salvadori, Enrico; Bridges, Hannah R; Hirst, Judy; Roessler, Maxie M

2016-09-01

EPR-based potentiometric titrations are a well-established method for determining the reduction potentials of cofactors in large and complex proteins with at least one EPR-active state. However, such titrations require large amounts of protein. Here, we report a new method that requires an order of magnitude less protein than previously described methods, and that provides EPR samples suitable for measurements at both X- and Q-band microwave frequencies. We demonstrate our method by determining the reduction potential of the terminal [4Fe-4S] cluster (N2) in the intramolecular electron-transfer relay in mammalian respiratory complex I. The value determined by our method, E m7 =-158mV, is precise, reproducible, and consistent with previously reported values. Our small-volume potentiometric titration method will facilitate detailed investigations of EPR-active centres in non-abundant and refractory proteins that can only be prepared in small quantities. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Study of gamma irradiated polyethylenes by temperature modulated differential scanning calorimetry

International Nuclear Information System (INIS)

Secerov, B.; Galovic, S.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

2011-01-01

Complete text of publication follows. The various polyethylenes (PEs) and effects of high energy radiation on theirs structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we applied the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and nonreversing part enabled to observed the low temperature enthalpy relaxation (related to the existence of the 'rigid amorphous phase') and recrystallization processes as well as to follow their and/or radiation-induced evolution of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

A fully automatic system for acid-base coulometric titrations

OpenAIRE

Cladera, A.; Caro, A.; Estela, J. M.; Cerdà, V.

1990-01-01

An automatic system for acid-base titrations by electrogeneration of H+ and OH- ions, with potentiometric end-point detection, was developed. The system includes a PC-compatible computer for instrumental control, data acquisition and processing, which allows up to 13 samples to be analysed sequentially with no human intervention. The system performance was tested on the titration of standard solutions, which it carried out with low errors and RSD. It was subsequently applied to the analysis o...

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.

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.

Clozapine Titration for People in Early Psychosis: A Chart Review and Treatment Guideline.

Science.gov (United States)

Ballon, Jacob S; Ashfaq, Hera; Noordsy, Douglas L

2018-06-01

The use of clozapine, particularly in young people, is often limited by early treatment-emergent adverse effects including drowsiness and lethargy. Concerns about adverse effects, medication adherence, and the need for blood monitoring often impede the use of clozapine in this population, leading to repeated trials of less effective medications. Current clozapine dosing recommendations are based on people further in the course of their illness and thus reflect different responsiveness and sensitivities to antipsychotic medication. As such, there is a need for evidence-based guidelines for titration and dosing of clozapine among people in early psychosis. We performed a chart review of 14 people treated with clozapine within our early psychosis team. Data regarding dose titration, response, time to discontinuation, symptom severity, weight gain, and other adverse effects were gathered at clozapine initiation, 3 months, and last available visit on clozapine. People treated with slow titration within their first year of psychosis onset achieved sustained response at very low maintenance doses (mean dose = 81 mg/d, mean duration of treatment = 200 weeks) compared with slow titration with longer duration of illness (mean dose = 350 mg/d, mean duration of treatment = 68 weeks) or standard dose titration in early psychosis (mean dose = 112 mg/d, mean duration of treatment = 38 weeks). The most common adverse effects in all groups were weight gain and sedation, with the groups requiring higher mean doses reporting a broader range of adverse effects. There was no apparent difference in the clinical global impression for severity or improvement between the slow titration and standard titration groups in people with early psychosis. These observations are synthesized into a proposed treatment guideline for use of clozapine among people in early psychosis. We describe development of a slow titration approach to initiating clozapine among people in early psychosis. This

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.

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.

Isothermal reaction calorimetry as a tool for kinetic analysis

International Nuclear Information System (INIS)

Zogg, Andreas; Stoessel, Francis; Fischer, Ulrich; Hungerbuehler, Konrad

2004-01-01

Reaction calorimetry has found widespread application for thermal and kinetic analysis of chemical reactions in the context of thermal process safety as well as process development. This paper reviews the most important reaction calorimetric principles (heat-flow, heat-balance, power-compensation, and Peltier principle) and their applications in commercial or scientific devices. The discussion focuses on the different dynamic behavior of the main calorimetric principles during an isothermal reaction measurement. Examples of available reaction calorimeters are further compared considering their detection limit, time constant as well as temperature range. In a second part, different evaluation methods for the isothermally measured calorimetric data are reviewed and discussed. The methods will be compared, focusing especially on the fact that reaction calorimetric data always contains additional informations not directly related to the actual chemical reaction such as heat of mixing, heat of phase-transfer/change processes or simple measurement errors. Depending on the evaluation method applied such disturbances have a significant influence on the calculated reaction enthalpies or rate constants

End-point detection in potentiometric titration by continuous wavelet transform.

Science.gov (United States)

Jakubowska, Małgorzata; Baś, Bogusław; Kubiak, Władysław W

2009-10-15

The aim of this work was construction of the new wavelet function and verification that a continuous wavelet transform with a specially defined dedicated mother wavelet is a useful tool for precise detection of end-point in a potentiometric titration. The proposed algorithm does not require any initial information about the nature or the type of analyte and/or the shape of the titration curve. The signal imperfection, as well as random noise or spikes has no influence on the operation of the procedure. The optimization of the new algorithm was done using simulated curves and next experimental data were considered. In the case of well-shaped and noise-free titration data, the proposed method gives the same accuracy and precision as commonly used algorithms. But, in the case of noisy or badly shaped curves, the presented approach works good (relative error mainly below 2% and coefficients of variability below 5%) while traditional procedures fail. Therefore, the proposed algorithm may be useful in interpretation of the experimental data and also in automation of the typical titration analysis, specially in the case when random noise interfere with analytical signal.

Dose titration of BAF312 attenuates the initial heart rate reducing effect in healthy subjects.

Science.gov (United States)

Legangneux, Eric; Gardin, Anne; Johns, Donald

2013-03-01

Previous studies have shown transient decreases in heart rate (HR) following administration of sphingosine 1-phosphate (S1P) receptor modulators including BAF312. This study was conducted to determine whether dose titration of BAF312 reduces or eliminates these effects. Fifty-six healthy subjects were randomized 1:1:1:1 to receive BAF312 in one of two dose titration (DT) regimens (DT1 and DT2: 0.25-10 mg over 9-10 days), no titration (10 mg starting dose) or placebo. Pharmacodynamic and pharmacokinetic parameters were assessed. Neither DT1 nor DT2 resulted in clinically significant bradycardia or atrioventricular conduction effects. Both titration regimens showed a favourable difference on each of days 1-12 vs. the non-titration regimen on day 1 for HR effects (P titration was 1.18 (95% confidence interval [CI] 1.13, 1.23) and 1.14 (95% CI 1.09, 1.18) for DT2 (both P titration HRs showed considerable separation from placebo throughout the study. There was no statistically significant reduction in HR vs. placebo on day 1 in either titration regimen. On days 3-7 subjects in DT1 and DT2 experienced minor reductions in HR vs. placebo (approximately 5 beats min⁻¹; P ≤ 0.0001). From days 9-12, HRs in both titration regimens were comparable with placebo. Both titration regimens effectively attenuated the initial bradyarrhythmia observed on day 1 of treatment with BAF312 10 mg. © 2012 Novartis Institutes for BioMedical Research (NIBIR). British Journal of Clinical Pharmacology © 2012 The British Pharmacological Society.

Insights into glass transition and relaxation behavior using temperature-modulated differential scanning calorimetry

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, J.C.; Allan, D.C.

Temperature-modulated differential scanning calorimetry (TMDSC) is based on conventional DSC but with a sinusoidally modulated temperature path. Our simulations of TMDSC signals prove that the frequency correction of non-reversing heat flow can give a master curve within a certain range...... of frequencies. This frequency range is dependent not only on the measurement parameters such as linear heating/cooling rate and frequency and amplitude of the modulation, but also on the previous thermal history before the TMDSC measurement. The frequency correction for the reversing heat flow gives more...

Determination of organic bases in non-aqueous solvents by catalytic thermometric titration.

Science.gov (United States)

Vajgand, V J; Kiss, T A; Gaál, F F; Zsigrai, I J

1968-07-01

Catalytic thermometric titrations have been developed for bases (brucine, diethylaniline, potassium acetate and triethylamine) in acetic acid by continuous and discontinuous addition of the standard solution and automatic temperature recording. The determination of weak bases, e.g., antipyrine, unsuccessful in acetic acid by catalytic thermometric titration, has been achieved by using nitromethane or acetic anhydride as solvent. Catalytic thermometric titrations were also performed by coulometric generation of hydrogen ions for the determination of micro amounts of weak bases in a mixture of acetic anhyride and acetic acid.

Simple modification of karl-Fischer titration method for determination of water content in colored samples.

Science.gov (United States)

Tavčar, Eva; Turk, Erika; Kreft, Samo

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 place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD = 4.3%), accuracy, and linearity (R(2) = 0.997).

Linear regression analysis of potentiometric titration data for asymmetric redox reactions

International Nuclear Information System (INIS)

Mar'yanov, B.M.; Gavrilenko, M.A.

1997-01-01

A statistical method of processing the curves of potentiometric titration for homogeneous asymmetric redox reactions has been suggested. The method was tested using a model titrimetric system Mohr's salt-K 2 Cr 2 O 7 and was employed for Te determination in an individual solution, semiconductor alloy and CdTe ceramics. Random error of the equivalence point evaluation by the data of a specific titration of 0.1-0.01 M solutions does not exceed 0.3% in case of titration of 0.001 M solutions it increases up to 1.2%. The value of s r varies from 0.0006 to 0.007

Implementation of 'Davies and Gray/NBL Method' for potentiometric titration of uranium in the Safeguards Laboratory of CNEN by the use of a DL-67 mettler titrator

International Nuclear Information System (INIS)

Araujo, Radier Mario Silveira de; Barros, Pedro Dionisio de

2005-01-01

To meet the requirements of the Brazilian State System of Accounting for and Control of Nuclear Materials - SSAC, the Safeguards Laboratory of CNEN - LASAL has been applying the 'Davies and Gray/NBL' method for potentiometric determination of total uranium concentration in uranium samples taken during safeguards inspections at nuclear facilities since 1984, using a Radiometer ETS 822 titrator. In order to improve the analytical capability and the procedures related to the titration methodology, the same method was also implemented by using a METTLER DL - 67 titrator. This equipment is microprocessor - controlled and can be connected to additional devices such as printers, analytical balances, etc. It also provides accurate and reproducible results for end-point titrations, providing analytical performance according to the current international safeguards requirements. The implementation of the method in such equipment included the addition of analytical data as well as the improvement of the equipment parameters for uranium determination. Parameters like predispensing volume; titrant data and end-point value were studied. Some uranium samples (solids and solutions) were used during the initial tests with the titrator. A solution of pure uranyl nitrate was used as reference sample for this paper. From this, aliquots were analyzed in both Radiometer ETS-822 and METTLER DL-67. Results obtained from each equipment were compared with the reference value of the sample. The comparison showed that results from METTLER DL-67 meets the precision and accuracy requirements for this kind of analysis and led to the conclusion that the performance of this titrator is adequate for the determination of total uranium content in samples of nuclear materials for safeguards purposes. (author)

Apparent heat capacity measurements and thermodynamic functions of D(−)-fructose by standard and temperature-modulated calorimetry

International Nuclear Information System (INIS)

Magoń, A.; Pyda, M.

2013-01-01

Highlights: ► Experimental, apparent heat capacity of fructose was investigated by advanced thermal analysis. ► Equilibrium melting parameters of fructose were determined. ► Decomposition, superheating of crystalline fructose during melting process were presented. ► TGA, DSC, and TMDSC are useful tools for characterisation of fructose. - Abstract: The qualitative and quantitative thermal analyses of crystalline and amorphous D(−)-fructose were studied utilising methods of standard differential scanning calorimetry (DSC), quasi-isothermal temperature-modulated differential scanning calorimetry (quasi-isothermal TMDSC), and thermogravimetric analysis (TGA). Advanced thermal analysis of fructose was performed based on heat capacity. The apparent total and apparent reversing heat capacities, as well as phase transition parameters were examined on heating and cooling. The melting temperature, T m , of crystalline D(−)-fructose shows a heating rate dependency, which increases with raising the heating rate and leads to superheating. The equilibrium melting temperatures: T m ∘ (onset) = 370 K and T m ∘ (peak) = 372 K, and the equilibrium enthalpy of fusion Δ fus H ° = 30.30 kJ · mol −1 , of crystalline D(−)-fructose were estimated on heating for the results at zero heating rate. Anomalies in the heat capacity in the liquid state of D(−)-fructose, assigned as possible tautomerisation equilibrium, were analysed by DSC and quasi-isothermal TMDSC, both on heating and cooling. Thermal stability of crystals in the region of the melting temperature was examined by TGA and quasi-isothermal TMDSC. Melting, mutarotation, and degradation processes occur simultaneously and there are differences in values of the liquid heat capacity of D(−)-fructose with varied thermal history, measured by quasi-isothermal TMDSC. Annealing of amorphous D(−)-fructose between the glass transition temperature, T g , and the melting temperature, T m , also leads to

Determination of free acid in U(VI)-Al(III) solution by Gran plot titration

International Nuclear Information System (INIS)

Suh, Moo Yul; Lee, Chang Heon; Sohn, Se Chul; Kim, Jung Suk; Kim, Won Ho; Eom, Tae Yoon

1999-01-01

The determination method of free acid in spent U-Al nuclear fuel solutions by Gran plot titration was described. Effect of U(VI) and Al(III) on the alkalimetric titration of nitric acid was investigation in oxalate complexing media as well as in noncomplexing media. Positive biases were observed in both titration media when the end-point was estimated by the Gran plot method. It was found that the cause of the bias was U(VI) in the oxalate complexing media, but Al(III) in the noncomplexing media. The relative error was less than 1% in the titration of 0.1 M HNO 3 at a U(VI):Al(III):H + mole ratio of up to 2:12:1 as long as the pH of the oxalate titration media was sustained to be below 5.0 at the beginning of titration. The method was successfully applied to the determination of nitric acid in a solution of HANARO reactor fuel with U:Al mole ratio of 1:6

Investigation of iodine liberation process in redox titration of potassium iodate with sodium thiosulfate

International Nuclear Information System (INIS)

Asakai, Toshiaki; Hioki, Akiharu

2011-01-01

Potassium iodate is often used as a reference material to standardize a sodium thiosulfate solution which is a familiar titrant for redox titrations. In the standardization, iodine (triiodide) liberated by potassium iodate in an acidic potassium iodide solution is titrated with a sodium thiosulfate solution. The iodine liberation process is significantly affected by the amount of acid, that of potassium iodide added, the waiting time for the liberation, and light; therefore, the process plays a key role for the accuracy of the titration results. Constant-voltage biamperometry with a modified dual platinum-chip electrode was utilized to monitor the amount of liberated iodine under several liberation conditions. Coulometric titration was utilized to determine the concentration of a sodium thiosulfate solution on an absolute basis. Potassium iodate was assayed by gravimetric titration with the sodium thiosulfate solution under several iodine liberation conditions. The liberation process was discussed from the changes in the apparent assay of potassium iodate. The information of the appropriate titration procedure obtained in the present study is useful for any analysts utilizing potassium iodate to standardize a thiosulfate solution.

Investigation of iodine liberation process in redox titration of potassium iodate with sodium thiosulfate

Energy Technology Data Exchange (ETDEWEB)

Asakai, Toshiaki, E-mail: t-asakai@aist.go.jp [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 3-9, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563 (Japan); Hioki, Akiharu [National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST), Tsukuba Central 3-9, 1-1-1 Umezono, Tsukuba, Ibaraki 305-8563 (Japan)

2011-03-09

Potassium iodate is often used as a reference material to standardize a sodium thiosulfate solution which is a familiar titrant for redox titrations. In the standardization, iodine (triiodide) liberated by potassium iodate in an acidic potassium iodide solution is titrated with a sodium thiosulfate solution. The iodine liberation process is significantly affected by the amount of acid, that of potassium iodide added, the waiting time for the liberation, and light; therefore, the process plays a key role for the accuracy of the titration results. Constant-voltage biamperometry with a modified dual platinum-chip electrode was utilized to monitor the amount of liberated iodine under several liberation conditions. Coulometric titration was utilized to determine the concentration of a sodium thiosulfate solution on an absolute basis. Potassium iodate was assayed by gravimetric titration with the sodium thiosulfate solution under several iodine liberation conditions. The liberation process was discussed from the changes in the apparent assay of potassium iodate. The information of the appropriate titration procedure obtained in the present study is useful for any analysts utilizing potassium iodate to standardize a thiosulfate solution.

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

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.

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

Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

Science.gov (United States)

Tavčar, Eva; Turk, Erika; Kreft, Samo

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 place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD = 4.3%), accuracy, and linearity (R 2 = 0.997). PMID:22567558

Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

Directory of Open Access Journals (Sweden)

Eva Tavčar

2012-01-01

Full Text Available 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 place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD=4.3%, accuracy, and linearity (2=0.997.

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.

The physics of compensating calorimetry and the new CALOR89 code system

International Nuclear Information System (INIS)

Gabriel, T.A.; Brau, J.E.; Bishop, B.L.

1989-03-01

Much of the understanding of the physics of calorimetry has come from the use of excellent radiation transport codes. A new understanding of compensating calorimetry was introduced four years ago following detailed studies with a new CALOR system. Now, the CALOR system has again been revised to reflect a better comprehension of high energy nuclear collisions by incorporating a modified high energy fragmentation model from FLUKA87. This revision will allow for the accurate analysis of calorimeters at energies of 100's of GeV. Presented in this paper is a discussion of compensating calorimetry, the new CALOR system, the revisions to HETC, and recently generated calorimeter related data on modes of energy deposition and secondary neutron production (E < 50 MeV) in infinite iron and uranium blocks. 38 refs., 5 figs., 5 tabs

Safety and tolerability of different titration rates of retigabine (ezogabine) in patients with partial-onset seizures.

Science.gov (United States)

Biton, Victor; Gil-Nagel, Antonio; Brodie, Martin J; Derossett, Sarah E; Nohria, Virinder

2013-11-01

Retigabine (RTG; international nonproprietary name)/ezogabine (EZG; US adopted name) is an antiepileptic drug (AED) that prolongs neuronal voltage-gated potassium-channel KCNQ2-5 (Kv 7.2-7.5) opening. This double-blind study evaluated different RTG/EZG dose-titration rates. Patients (N=73) with partial-onset seizures receiving concomitant AEDs were randomized to one of three titration groups, all of which were initiated at RTG/EZG 300mg/day divided into three equal doses. Fast-, medium-, and slow-titration groups received dose increments of 150mg/day every 2, 4, and 7 days, respectively, achieving the target dose of 1200mg/day after 13, 25, and 43 days, respectively. Safety assessments were performed throughout. Discontinuation rates due to treatment-emergent adverse events (TEAEs) were numerically higher in the fast- (10/23) and medium- (7/22) titration groups than in the slow-titration group (3/23) but statistical significance was achieved only for the high-titration group compared with the low-titration group (p=0.024). Stratified analysis, with concomitant AEDs divided into enzyme inducers (carbamazepine, phenytoin, oxcarbazepine) or noninducers, showed that the risk of discontinuation due primarily to TEAEs was significantly higher in the fast- (p=0.010) but not in the medium-titration group (p=0.078) when compared with the slow-titration group. Overall, the slow-titration rate appeared to be best tolerated and was used in further efficacy and safety studies with RTG/EZG. Copyright © 2013 Elsevier B.V. All rights reserved.

Further investigation on the degree of deacetylation of chitosan determined by potentiometric titration

OpenAIRE

Kamal Sweidan; Abdel-Motalleb Jaber; Nawzat Al-jbour; Rana Obaidat; Mayyas Al- Remawi; Adnan Badwan

2011-01-01

The degree of deacetylation (DDA) of various low molecular weight chitosan (LMWC) species as the hydrochloride and free base (amine form) was determined by direct and back potentiometric titration, respectively. The DDA values obtained for the chitosan hydrochloride by direct titration were greater than 93% for all oligomers tested (Molecular weight (Mwt) between about 1.3 to 30.0 kDa). However, the DDA values obtained for chitosan amine oligomers using back titration were significantly lower...

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.

Acid-base titrations by stepwise addition of equal volumes of titrant with special reference to automatic titrations-II Theory of titration of mixtures of acids, polyprotic acids, acids in mixture with weak bases, and ampholytes.

Science.gov (United States)

Pehrsson, L; Ingman, F; Johansson, S

A general method for evaluating titration data for mixtures of acids and for acids in mixture with weak bases is presented. Procedures are given that do not require absolute [H]-data, i.e., relative [H]-data may be used. In most cases a very rough calibration of the electrode system is enough. Further, for simple systems, very approximate values of the stability constants are sufficient. As examples, the titration of the following are treated in some detail: a mixture of two acids, a diprotic acid, an acid in presence of its conjugate base, and an ampholyte.

Development of Resistive Micromegas for Sampling Calorimetry

Science.gov (United States)

Geralis, T.; Fanourakis, G.; Kalamaris, A.; Nikas, D.; Psallidas, A.; Chefdeville, M.; Karyotakis, I.; Koletsou, I.; Titov, M.

2018-02-01

Resistive micromegas is proposed as an active element for sampling calorimetry. Future linear collider experiments or the HL-LHC experiments can profit from those developments for Particle Flow Calorimetry. Micromegas possesses remarkable properties concerning gain stability, reduced ion feedback, response linearity, adaptable sensitive element granularity, fast response and high rate capability. Recent developments on Micromegas with a protective resistive layer present excellent results, resolving the problem of discharges caused by local high charge deposition, thanks to its RC-slowed charge evacuation. Higher resistivity though, may cause loss of the response linearity at high rates. We have scanned a wide range of resistivities and performed laboratory tests with X-rays that demonstrate excellent response linearity up to rates of (a few) times 10MHz/cm2, with simultaneous mitigation of discharges. Beam test studies at SPS/CERN with hadrons have also shown a remarkable stability of the resistive Micromegas and low currents for rates up to 15MHz/cm2. We present results from the aforementioned studies confronted with MC simulation

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.

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

Home blood pressure monitoring and self-titration of antihypertensive medications: Proposed patient selection criteria.

Science.gov (United States)

Hill, James R

2016-05-01

Recent studies have demonstrated that home blood pressure monitoring (HBPM), coupled with self-titration of medications is a viable intervention to control hypertension. There are currently no established criteria to evaluate patients for inclusion in such a program. The purpose of this discussion is to propose criteria for determining if a patient is appropriate to participate in a program of HBPM and self-titration. Inclusion criteria for two self-titration trials were examined, and additional factors in clinical practice were identified and discussed. Additional selection criteria were proposed to support the decision to enroll a patient in an antihypertensive self-titration program. Inclusion criteria from self-titration trials provide a reasonable starting point for choosing appropriate patients in clinical practice, but additional research is necessary. Adaptation of these criteria and consideration of the identified factors can be used to develop decision support instruments. Such instruments should be evaluated for effectiveness and reliability prior to use in clinical practice. HBPM combined with self-titration is an effective patient-centered approach for hypertension management. Decision support instruments to determine appropriate patients are necessary for safe and effective use in clinical practice. ©2015 American Association of Nurse Practitioners.

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.

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-...

Free Software Development. 3. Numerical Description of Soft Acid with Soft Base Titration

OpenAIRE

Lorentz JÄNTSCHI; Horea Iustin NAŞCU

2002-01-01

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_titra...

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.

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.

Methodology of hot nucleus calorimetry and thermometry produced by nuclear reactions around Fermi energies; Methodologie de la calorimetrie et de la thermometrie des noyaux chauds formes lors de collisions nucleaires aux energies de Fermi

Energy Technology Data Exchange (ETDEWEB)

Vient, E

2006-12-15

This work deals with the calorimetry and thermometry of hot nuclei produced in collisions Xe + Sn between 25 and 100 MeV/u. The apparatus for hot nucleus physical characterization is the 4{pi} detector array Indra. This study was made by using the event generators Gemini, Simon and Hipse and a data-processing filter simulating the complete operation of the multi-detector. The first chapter presents the different ways of producing hot nuclei. In the second and third chapters, the author presents a critical methodological study of calorimetry and thermometry applied to hot nuclei, different methods are reviewed, their accuracy and application range are assessed. All the calorimetry methods rely on the assumption that we are able to discriminate decay products of the hot nucleus from evaporated particles. In the fourth chapter, the author gives some ways of improving calorimetry characterization of the hot nucleus. An alternative method of calorimetry is proposed in the fifth chapter, this method is based on the experimental determination of an evaporation probability that is deduced from the physical characteristics of the particles present in a restricted domain of the space of velocities.

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.

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

On the binding of calcium by micelles composed of carboxy-modified pluronics measured by means of differential potentiometric titration and modeled with a self-consistent-field theory.

Science.gov (United States)

Lauw, Y; Leermakers, F A M; Cohen Stuart, M A; Pinheiro, J P; Custers, J P A; van den Broeke, L J P; Keurentjes, J T F

2006-12-19

We perform differential potentiometric titration measurements for the binding of Ca2+ ions to micelles composed of the carboxylic acid end-standing Pluronic P85 block copolymer (i.e., CAE-85 (COOH-(EO)26-(PO)39-(EO)26-COOH)). Two different ion-selective electrodes (ISEs) are used to detect the free calcium concentration; the first ISE is an indicator electrode, and the second is a reference electrode. The titration is done by adding the block copolymers to a known solution of Ca2+ at neutral pH and high enough temperature (above the critical micellization temperature CMT) and various amount of added monovalent salt. By measuring the difference in the electromotive force between the two ISEs, the amount of Ca2+ that is bound by the micelles is calculated. This is then used to determine the binding constant of Ca2+ with the micelles, which is a missing parameter needed to perform molecular realistic self-consistent-field (SCF) calculations. It turns out that the micelles from block copolymer CAE-85 bind Ca2+ ions both electrostatically and specifically. The specific binding between Ca2+ and carboxylic groups in the corona of the micelles is modeled through the reaction equilibrium -COOCa+ -COO- + Ca2+ with pKCa = 1.7 +/- 0.06.

A study of gamma-irradiated polyethylenes by temperature modulated differential scanning calorimetry

Science.gov (United States)

Galovic, S.; Secerov, B.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

2012-09-01

Various polyethylenes (PEs) and the effects of high-energy radiation on their structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we used the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of the initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and non-reversing part enabled us to observe the low-temperature enthalpy relaxation (related to the existence of the "rigid amorphous phase") and recrystallisation processes, as well as to follow their radiation-induced evolution and/or that of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

Titrated Misoprostol Versus Dinoprostone for Labor Induction

African Journals Online (AJOL)

Aim: This study designed to compare titrated misoprostol regarding its safety and efficacy with dinoprostone for induction of labor. ... Statistical analysis done using Student's t-test for quantitative data and ..... induction: A pilot study. Rev Bras ...

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,…

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.

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

Determination of dissolved inorganic species of iodine by spectrophotometric titration

Energy Technology Data Exchange (ETDEWEB)

Pesavento, Maria; Profumo, Antonella; Biesuz, Raffaela

1987-09-01

A method for determining iodate and iodine (+1) in aqueous solutions is proposed. The assay is similar to a previously described method for the determination of iodide and iodine (O), which were titrated with standard iodate in hydrochloric acid solution. A sample solution made 0.5-1.5 M in hydrochloric acid is titrated with a standard iodide solution and monitored spectrophotometrically at 230 nm. The species involved have strong absorbances that are well differentiated at this wavelength. By combining the two titrations it is possible to resolve any mixture of species of iodine in different oxidation states. The precision of the method (standard deviation) is the same both when determining a single species (IO/sub 3/-,I+,1/sub 2/ or I-) and a mixture, and is equal to 2 x 10/sup -7/ M. Chloride and bromide, even at very high concentrations, do not interfere.

Determination of dissolved inorganic species of iodine by spectrophotometric titration

International Nuclear Information System (INIS)

Pesavento, Maria; Profumo, Antonella

1987-01-01

A method for determining iodate and iodine (+1) in aqueous solutions is proposed. The assay is similar to a previously described method for the determination of iodide and iodine (O), which were titrated with standard iodate in hydrochloric acid solution. A sample solution made 0.5-1.5 M in hydrochloric acid is titrated with a standard iodide solution and monitored spectrophotometrically at 230 nm. The species involved have strong absorbances that are well differentiated at this wavelength. By combining the two titrations it is possible to resolve any mixture of species of iodine in different oxidation states. The precision of the method (standard deviation) is the same both when determining a single species (IO 3 -,I+,1 2 or I-) and a mixture, and is equal to 2 x 10 -7 M. Chloride and bromide, even at very high concentrations, do not interfere. (author)

Thermometric titration of cadmium with sodium diethyldithiocarbamate, with oxidation by hydrogen peroxide as indicator reaction.

Science.gov (United States)

Hattori, T; Yoshida, H

1987-08-01

A new method of end-point indication is described for thermometric titration of cadmium with sodium diethyldithiocarbamate (DDTC). It is based on the redox reaction between hydrogen peroxide added to the system before titration, and the first excess of DDTC. Amounts of cadmium in the range 10-50 mumoles are titrated within 1% error.

[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.

Quick titration of pergolide in cotreatment with domperidone is safe and effective

NARCIS (Netherlands)

Jansen, PAF; Herings, RMC; Samson, MM; Schuurmans-Daemen, LMPJ; Hovestadt, A; Verhaar, HJJ; Van Laar, T; de Vreede, P.

2001-01-01

The purpose of the study was to analyze efficacy and safety of quick pergolide titration combined with domperidone. In an open-label prospective study, pergolide was titrated in 16 days to a maximum of 3 mg/d doses as adjunctive treatment to L-Dopa in 10 elderly patients with Parkinson's disease.

Randomized cross-over trial of ventilator modes during non-invasive ventilation titration in amyotrophic lateral sclerosis.

Science.gov (United States)

Vrijsen, Bart; Buyse, Bertien; Belge, Catharina; Vanpee, Goele; Van Damme, Philip; Testelmans, Dries

2017-08-01

Non-invasive ventilation (NIV) improves survival, quality of life and sleep in patients with amyotrophic lateral sclerosis (ALS). Nevertheless, NIV titration is conducted in different ways. We aim to provide more insight into NIV titration by comparing the effects of a spontaneous (S) and spontaneous-timed (ST) modes on gas exchange, sleep architecture and patient-ventilator asynchronies (PVAs). After an initial night of NIV titration, patients were randomized to S or ST mode in a cross-over design. NIV was titrated using polysomnography, oximetry (oxygen saturation, SpO 2 %) and transcutaneous carbon dioxide (PtcCO 2 ) measurement. PVAs were analysed breath-by-breath. Thirteen patients were analysed after inclusion. ST mode showed better results in gas exchange (minimal SpO 2 %: 83 (80-89)% vs 87 (84-89)%; oxygen desaturation index: 15 (5-28)/h sleep vs 7 (3-9)/h sleep; PtcCO 2 >55 mm Hg: 20 (0-59)% vs 0 (0-27)% total sleep time for S and ST mode, respectively, all P < 0.05) and respiratory events (obstructive: 8.9 (1.2-18.3)/h sleep vs 1.8 (0.3-4.9)/h sleep and central: 2.6 (0.4-14.1)/h sleep vs 0.2 (0.0-1.1)/h sleep for S and ST mode, respectively, both P < 0.01). No differences in sleep architecture were found. Ineffective efforts and respiratory events were more frequently present in S mode. Nevertheless, four patients were discharged on S mode as these patients showed clinically better results for sleep architecture and PVA during the night on S mode. ST mode shows better results in gas exchange, respiratory events and PVA. Nevertheless, accurate NIV titration remains necessary as some patients show equal or better results when using the S mode. © 2017 Asian Pacific Society of Respirology.

Photometric micro-determination of scandium and lanthanides by direct and successive titration using semi-xylenol orange

International Nuclear Information System (INIS)

Hafez, M.A.E.H.; Eman, M.E.S.M.

1986-01-01

The precision and accuracy attainable in direct titrations of the Sc 3+ , La 3+ or Er 3+ ion with a 0.001 M solution of the disodium salt of EDTA using semi-xylenol orange (SXO) as a metallochromic indicator were studied. Accurate results can be achieved by successive titration. The Sc 3+ ion is titrated at pH 2.4, the pH is adjusted to 5.6-5.9 by adding hexamethylenetetramine buffer solution and the La 3+ ion (or Er 3+ ion) is then titrated. A comparison of SXO and xylenol orange indicators for the successive titration of the Sc 3+ ion and lanthanum or erbium was carried out. (author)

A stable and convenient protein electrophoresis titration device with bubble removing system.

Science.gov (United States)

Zhang, Qiang; Fan, Liu-Yin; Li, Wen-Lin; Cong, Feng-Song; Zhong, Ran; Chen, Jing-Jing; He, Yu-Chen; Xiao, Hua; Cao, Cheng-Xi

2017-07-01

Moving reaction boundary titration (MRBT) has a potential application to immunoassay and protein content analysis with high selectivity. However, air bubbles often impair the accuracy of MRBT, and the leakage of electrolyte greatly decreases the safety and convenience of electrophoretic titration. Addressing these two issues a reliable MRBT device with modified electrolyte chamber of protein titration was designed. Multiphysics computer simulation was conducted for optimization according to two-phase flow. The single chamber was made of two perpendicular cylinders with different diameters. After placing electrophoretic tube, the resident air in the junction next to the gel could be eliminated by a simple fast electrolyte flow. Removing the electrophoretic tube automatically prevented electrolyte leakage at the junction due to the gravity-induced negative pressure within the chamber. Moreover, the numerical simulation and experiments showed that the improved MRBT device has following advantages: (i) easy and rapid setup of electrophoretic tube within 20 s; (ii) simple and quick bubble dissipates from the chamber of titration within 2 s; (iii) no electrolyte leakage from the two chambers: and (iv) accurate protein titration and safe instrumental operation. The developed technique and apparatus greatly improves the performance of the previous MRBT device, and providing a new route toward practical application. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Data processing for potentiometric precipitation titration of mixtures of isovalent ions by linear regression analysis

International Nuclear Information System (INIS)

Mar'yanov, B.M.; Shumar, S.V.; Gavrilenko, M.A.

1994-01-01

A method for the computer processing of the curves of potentiometric differential titration using the precipitation reactions is developed. This method is based on transformation of the titration curve into a line of multiphase regression, whose parameters determine the equivalence points and the solubility products of the formed precipitates. The computational algorithm is tested using experimental curves for the titration of solutions containing Hg(2) and Cd(2) by the solution of sodium diethyldithiocarbamate. The random errors (RSD) for the titration of 1x10 -4 M solutions are in the range of 3-6%. 7 refs.; 2 figs.; 1 tab

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

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....

CALOR2012 XVth International Conference on Calorimetry in High Energy Physics

Energy Technology Data Exchange (ETDEWEB)

Akchurin, Nural .

2015-05-04

The International Conferences on Calorimetry in High Energy Physics, or the CALOR series, have always been where the calorimeter experts come together to review the state of calorimetry and bring forth new ideas every two years. The fteenth conference, CALOR2012, in Santa Fe was no exception. Although they were built roughly a decade ago, we are now witnessing the exceptional power of the LHC calorimeters and the crucial role they have been playing in the discovery of the 125 GeV Higgs-like boson. As we ruminate on the coming generation of experiments at the next (linear) collider and on the upgrades at the LHC, we are heartened by the substantial advances we made in calorimetry in the last decade. These advances will certainly help uncover new physics in the years to come, not only at colliders but also in astroparticle experiments that take advantage of natural elements such as air, water, and ice. The proceedings were published by the IOP in Journal of Physics, Vol 404 2011. The conference web site is calor2012.ttu.edu.

Potentiometric titration of selenic and telluric acids with titanium(III) chloride in nonaqueous solvents

International Nuclear Information System (INIS)

Yoshimura, Chozo; Miyamoto, Kiyoshige

1985-01-01

Selenic and Telluric acids were titrated potentiometrically with titanium(III) chloride solution by using Pt-Cu · Hg bimetallic electrodes in nonaqueous solvents such as N, N-dimethyl-formamide (DMF), dimethyl sulfoxide (DMSO), isopropyl alcohol (IPA) and the mixtures of these solvents. It was found that selenic and telluric acids were titrated directly at room temperature in DMF solution without hydrochloric acid. The molar ratios of selenic and telluric acids to titanium(III) chloride was 1 : 6. However, the corresponding reactions to SeO 4 2- → SeO 3 2- or TeO 4 2- → TeO 3 2- were not confirmed in the titration curve in DMF. In the titration of selenic acid in mixed solvents of DMF and IPA in 1 : 1 or 1 : 2 ratio, two steps were observed. The first and the second steps were appeared on the titration curve at molar ratios of 1 : 2 and 1 : 6, respectively. It was interpreted that the first step corresponded to the intermediate reaction of SeO 4 2- → SeO 3 2- . Mixed solution of selenic and telluric acids were determined by the proposed method. Three steps were observed on the titration curve. It was interpreted that the first, second and third steps corresponded to the reaction of SeO 4 2- → SeO 3 2- , SeO 3 2- → Se(0), and TeO 4 2- → Te(0), respectively. Less than 5 % of water gave no influence on the titration. (author)

Kinetics of bacterial potentiometric titrations: the effect of equilibration time on buffering capacity of Pantoea agglomerans suspensions.

Science.gov (United States)

Kapetas, Leon; Ngwenya, Bryne T; Macdonald, Alan M; Elphick, Stephen C

2011-07-15

Several recent studies have made use of continuous acid-base titration data to describe the surface chemistry of bacterial cells as a basis for accurately modelling metal adsorption to bacteria and other biomaterials of potential industrial importance. These studies do not share a common protocol; rather they titrate in different pH ranges and they use different stability criteria to define equilibration time during titration. In the present study we investigate the kinetics of bacterial titrations and test the effect they have on the derivation of functional group concentrations and acidity constants. We titrated suspensions of Pantoea agglomerans by varying the equilibration time between successive titrant additions until stability of 0.1 or 0.001 mV s(-1) was attained. We show that under longer equilibration times, titration results are less reproducible and suspensions exhibit marginally higher buffering. Fluorescence images suggest that cell lysis is not responsible for these effects. Rather, high DOC values and titration reversibility hysterisis after long equilibration times suggest that variability in buffering is due to the presence of bacterial exudates, as demonstrated by titrating supernatants separated from suspensions of different equilibration times. It is recommended that an optimal equilibration time is always determined with variable stability control and preliminary reversibility titration experiments. Copyright © 2011 Elsevier Inc. All rights reserved.

Determination of Titratable Acidity in Wine Using Potentiometric, Conductometric, and Photometric Methods

Science.gov (United States)

Volmer, Dietrich A.; Curbani, Luana; Parker, Timothy A.; Garcia, Jennifer; Schultz, Linda D.; Borges, Endler Marcel

2017-01-01

This experiment describes a simple protocol for teaching acid-base titrations using potentiometry, conductivity, and/or photometry to determine end points without an added indicator. The chosen example examines the titratable acidity of a red wine with NaOH. Wines contain anthocyanins, the colors of which change with pH. Importantly, at the…

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.

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.)

Thermodynamics and structure of inclusion compounds of tauro- and glyco-conjugated bile salts and beta-cyclodextrin

DEFF Research Database (Denmark)

Holm, Rene; Shi, Wei; Andersen Hartvig, Rune

2009-01-01

The interaction between natural beta-cyclodextrin and bile salts common in rat, dog and man, taurocholate, tauro-beta-muricholate, taurodeoxycholate, taurochenodeoxycholate, glycocholate, glycodeoxycholate and glycochenodeoxycholate, was studied using isothermal titration calorimetry, and the str......The interaction between natural beta-cyclodextrin and bile salts common in rat, dog and man, taurocholate, tauro-beta-muricholate, taurodeoxycholate, taurochenodeoxycholate, glycocholate, glycodeoxycholate and glycochenodeoxycholate, was studied using isothermal titration calorimetry......, and the structural differences in the interaction were investigated by H-1-ROESY NMR and molecular modeling. The beta-cyclodextrin was selected based upon its frequent use in preformulation and drug formulation as oral excipients for the solubilization of drug substances with low aqueous solubility. All...

Determination of the protonation enthalpy of humic acid by calorimetric titration technique

International Nuclear Information System (INIS)

Kimuro, Shingo; Kirishima, Akira; Sato, Nobuaki

2015-01-01

Graphical abstract: The thermodynamic quantities of protonation of humic acid were determined by the combination of potentiometric titration and calorimetric titration. It was observed that the protonation enthalpy and Gibbs free energy had been affected by pH of solution. As a result, the thermodynamics of the protonation reaction of humic acid is influenced by the polyelectrolyte effect and the heterogeneity. - Highlights: • We applied calorimetric titration technique to the protonation of humic acid. • The thermodynamic quantities of protonation of humic acid were determined. • The protonation enthalpy of humic acid is affected by the heterogeneity. • Gibbs free energy of the protonation is affected by the polyelectrolyte effect. - Abstract: In this study, the calorimetric titration technique was used to determine the protonation enthalpy of two reference humic acids and polyacrylic acid. First, we obtained the apparent protonation constant of two kinds of humic acid purchased from IHSS (International Humic Substances Society) and polyacrylic acid by potentiometric titration. Second, we obtained the protonation enthalpy of them by calorimetric titration. The protonation enthalpy of humic acid was affected by pH and the ionic strength of bulk solution. From the comparison of ΔH between humic acid and polyacrylic acid, it was concluded that the pH dependence of ΔH is attributed to the heterogeneity of humic acid. And ΔH of phenolic hydroxyl group in humic acid is strongly influenced by the electric double layer of humic acid’s surface. This is considered to be a reason of the ionic strength dependence of ΔH. On the other hand, Gibbs free energy of the protonation of humic acid is affected by the electrostatic attraction with the progress of dissociation of functional groups such as carboxyl group and phenolic hydroxyl group. Consequently, the thermodynamics of the protonation of humic acid is affected by the polyelectrolyte effect and the

Value of routine investigations to predict loop diuretic down-titration success in stable heart failure.

Science.gov (United States)

Martens, Pieter; Verbrugge, Frederik H; Boonen, Levinia; Nijst, Petra; Dupont, Matthias; Mullens, Wilfried

2018-01-01

Guidelines advocate down-titration of loop diuretics in chronic heart failure (CHF) when patients have no signs of volume overload. Limited data are available on the expected success rate of this practice or how routine diagnostic tests might help steering this process. Fifty ambulatory CHF-patients on stable neurohumoral blocker/diuretic therapy for at least 3months without any clinical sign of volume overload were prospectively included to undergo loop diuretic down-titration. All patients underwent a similar pre-down-titration evaluation consisting of a dyspnea scoring, physical examination, transthoracic echocardiography (diastolic function, right ventricular function, cardiac filling pressures and valvular disease), blood sample (serum creatinine, plasma NT-pro-BNP and neurohormones). Loop diuretic maintenance dose was subsequently reduced by 50% or stopped if dose was ≤40mg furosemide equivalents. Successful down-titration was defined as a persistent dose reduction after 30days without weight increase >1.5kg or new-onset symptoms of worsening heart failure. At 30-day follow-up, down-titration was successful in 62% (n=31). In 12/19 patients exhibiting down-titration failure, this occurred within the first week. Physical examination, transthoracic echocardiography and laboratory analysis had limited predictive capability to detect patients with down-titration success/failure (positive likelihood-ratios below 1.5, or area under the curve [AUC] non-statically different from AUC=0.5). Loop diuretic down-titration is feasible in a majority of stable CHF patients in which the treating clinician felt continuation of loops was unnecessary to sustain euvolemia. Importantly, routine diagnostics which suggest euvolemia, have limited diagnostic impact on the post-test probability. Copyright © 2017 Elsevier B.V. All rights reserved.

Clinical, polysomnographic, and CPAP titration features of obstructive sleep apnea: Mixed versus purely obstructive type.

Science.gov (United States)

Lee, Sang-Ahm; Lee, Gha-Hyun; Chung, Yoo-Sam; Kim, Woo Sung

2015-08-15

To determine whether obstructive sleep apnea syndrome (OSAS) patients with mixed sleep apnea (MSA) have different clinical, polysomnographic, and continuous positive airway pressure (CPAP) titration findings compared to OSAS patients without MSA. We retrospectively reviewed the records of OSAS patients who had undergone CPAP titration and categorized them into pure-OSA and mixed-OSA groups. Demographic features, daytime sleepiness, and apnea severity were compared between the two groups using univariate and multivariate analyses. CPAP titration findings were also compared between the two groups. One hundred and ninety-five subjects (n=126 pure-OSA; n=69 mixed-OSA) were included in the analysis. Compared to the pure-OSA group, the mixed-OSA group had a higher percentage of males (p=0.003) and a higher body mass index (p=0.044), Epworth Sleepiness Scale score (p=0.028), and apnea-hypopnea index (AHI) (ptitration, and a higher titrated pressure than the pure-OSA group. Severe OSA, older age, male sex, obesity, and daytime sleepiness were related to mixed-OSA. Complex sleep apnea, less optimal titration, and a higher titrated CPAP were also associated with MSA in OSAS patients. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of uranium and plutonium by sequential potentiometric titration

International Nuclear Information System (INIS)

Kato, Yoshiharu; Takahashi, Masao

1976-01-01

The determination of uranium and plutonium in mixed oxide fuels has been developed by sequential potentiometric titration. A weighed sample of uranium and plutonium oxides is dissolved in a mixture of nitric and hydrofluoric acids and the solution is fumed with sulfuric acid. After the reduction of uranium and plutonium to uranium(IV) and plutonium(III) by chromium(II) sulfate, 5 ml of buffer solution (KCl-HCl, pH 1.0) is added to the solution. Then the solution is diluted to 30 ml with water and the pH of the solution is adjusted to 1.0 -- 1.5 with 1 M sodium hydroxide. The solution is stirred until the oxidation of the excess of chromium(II) by air is completed. After the removal of dissolved oxygen by bubbling nitrogen through the solution for 10 minutes, uranium (IV) is titrated with 0.1 N cerium(IV) sulfate. Then, plutonium is titrated by 0.02 N cerium(IV) sulfate. When a mixture of uranium and plutonium is titrated with 0.1 N potassium dichromate potentiometrically, the potential change at the end point of plutonium is very small and the end point of uranium is also unclear when 0.1 N potassium permanganate is used as a titrant. In the present method, nitrate, fluoride and copper(II) interfere with the determination of plutonium and uranium. Iron interferes quantitatively with the determination of plutonium but not of uranium. Results obtained in applying the proposed method to 50 mg of mixtures of plutonium and uranium ((7.5 -- 50))% Pu were accurate to within 0.15 mg of each element. (auth.)

Determination of polyhexamethylene biguanide hydrochloride using photometric colloidal titration with crystal violet as a color indicator.

Science.gov (United States)

Masadome, Takashi; Miyanishi, Takaaki; Watanabe, Keita; Ueda, Hiroshi; Hattori, Toshiaki

2011-01-01

A solution of polyhexamethylene biguanide hydrochloride (PHMB-HCl) was titrated with a standard solution of potassium poly(vinyl sulfate) (PVSK) using crystal violet (CV) as an photometric indicator cation. The end point was detected by a sharp absorbance change due to an abrupt decrease in the concentration of CV. A linear relationship between the concentration of PHMB-HCl and the end-point volume of the titrant existed in the concentration range from 2 to 10 × 10(-6) eq mol L(-1). Back-titration was based on adding an excess amount of PVSK to a sample solution containing CV, which was titrated with a standard solution of poly(diallyldimethylammonium chloride) (PDADMAC). The calibration curve of the PHMB-HCl concentration to the end point volume of the titrant was also linear in the concentration range from 2 to 8 × 10(-6) eq mol L(-1). Both photometric titrations were applied to the determination of PHMB-HCl in a few contact-lens detergents. Back-titration showed a clear end point, but direct titration showed an unclear end point. The results of the back-titration of PHMB-HCl were compared with the content registered in its labels. 2011 © The Japan Society for Analytical Chemistry

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

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.

Particle flow calorimetry at the international linear collider

Indian Academy of Sciences (India)

Particle flow calorimetry at the international linear ... It is widely believed that the most promising strategy for achieving a jet ... this level of performance for two main reasons. Firstly ... (i) Tracking: For the studies presented in this paper, the track pattern ... that particles propagating outward from the interaction region will cross ...

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

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

Optical fibre temperature sensor technology and potential application in absorbed dose calorimetry

International Nuclear Information System (INIS)

Allen, P.D.; Hargrave, N.J.

1992-09-01

Optical fibre based sensors are proposed as a potential alternative to the thermistors traditionally used as temperature sensors in absorbed dose calorimetry. The development of optical fibre temperature sensor technology over the last ten years is reviewed. The potential resolution of various optical techniques is assessed with particular reference to the requirements of absorbed dose calorimetry. Attention is drawn to other issues which would require investigation before the development of practical optical fibre sensors for this purpose could occur. 192 refs., 5 tabs., 4 figs

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.

SPECIAL CONSIDERATIONS REGARDING WARFARIN DOSE TITRATION IN PATIENTS WITH ATRIAL FIBRILLATION DEPENDING ON CLINICAL FACTORS

Directory of Open Access Journals (Sweden)

E. L. Artanova

2011-01-01

Full Text Available 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, amiodarone therapy were considered among clinical characteristics. Results. Adjusted warfarin dose was significantly higher in obesity , and it was lower in case of experienced myocardial infarction. The INR highest levels and maximal amplitudes of its fluctuations were observed in patients with thyroid gland nodes and smokers. Period of warfarin dose titration was longer in patients treated with amiodarone. Conclusion. Warfarin dose titration in patients with atrial fibrillation depends on the presence of myocardial infarction, obesity , thyroid nodular changes, smoking and amiodarone treatment.

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...

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...

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

On the Frequency Correction in Temperature-Modulated Differential Scanning Calorimetry of Glass Transition

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, J.C.; Allan, D.C.

2012-01-01

Temperature-modulated differential scanning calorimetry (TMDSC) is based on conventional DSC but with a sinusoidally modulated temperature path. Simulations of TMDSC signals were performed for Corning EAGLE XG® glass over a wide range of modulation frequencies. Our results reveal that the frequency...... correction commonly used in the interpretation of TMDSC signals leads to a master nonreversing heat flow curve independent of modulation frequency, provided that sufficiently high frequencies are employed in the TMDSC measurement. A master reversing heat flow curve can also be generated through the frequency...

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.

A knowledge based advisory system for acid/base titrations in non-aqueous solvents

NARCIS (Netherlands)

Bos, M.; van der Linden, W.E.

1996-01-01

A computer program was developed that could advice on the choice of solvent and titrant for acid/base titrations in nonaqueous media. It is shown that the feasibility of a titration in a given solvent can be calculated from solvent properties and intrinsic acid/base properties of the sample

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

Accuracy and precision of protein-ligand interaction kinetics determined from chemical shift titrations.

Science.gov (United States)

Markin, Craig J; Spyracopoulos, Leo

2012-12-01

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

Pilot study of a new device to titrate oxygen flow in hypoxic patients on long-term oxygen therapy.

Science.gov (United States)

Cirio, Serena; Nava, Stefano

2011-04-01

The O(2) Flow Regulator (Dima, Bologna, Italy) is a new automated oxygen regulator that titrates the oxygen flow based on a pulse-oximetry signal to maintain a target S(pO(2)). We tested the device's safety and efficacy. We enrolled 18 subjects with chronic lung disease, exercise-induced desaturation, and on long-term oxygen therapy, in a randomized crossover study with 2 constant-work-load 15-min cycling exercise tests, starting with the patient's previously prescribed usual oxygen flow. In one test the oxygen flow was titrated manually by the respiratory therapist, and in the other test the oxygen flow was titrated by the O(2) Flow Regulator, to maintain an S(pO(2)) of 94%. We measured S(pO(2)) throughout each test, the time spent by the respiratory therapist to set the device or to manually regulate the oxygen flow, and the total number of respiratory-therapist titration interventions during the trial. There were no differences in symptoms or heart rate between the exercise tests. Compared to the respiratory-therapist-controlled tests, during the O(2) Flow Regulator tests S(pO(2)) was significantly higher (95 ± 2% vs 93 ± 3%, P = .04), significantly less time was spent below the target S(pO(2)) (171 ± 187 s vs 340 ± 220 s, P less respiratory therapist time (5.6 ± 3.7 min vs 2.0 ± 0.1 min, P = .005). The O(2) Flow Regulator may be a safe and effective alternative to manual oxygen titration during exercise in hypoxic patients. It provided stable S(pO(2)) and avoided desaturations in our subjects.

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)

High frequency titration in non-aqueous solvents. Application to HF and UF6

International Nuclear Information System (INIS)

Neveu, Claude

1965-01-01

In this research thesis, the author first presents the main theoretical notions regarding high frequency titration, notably by studying characteristic curves, i.e. the titration meter indication with respect to conductibility. He reports the use of this method for the study of various reactions in non-aqueous medium: reaction of AlCl 3 with pyridine in acetonitrile, of AlCl 3 with HCl in tetrachloroethane and in nitromethane. He also reports the attempt of application of this method to the titration of HF in presence of UF 6 in CCl 4 as solvent, or by using F acceptors like BF 3 , PF 5 or ClF 3 as reactants [fr

Standard test method for uranium by Iron (II) reduction in phosphoric acid followed by chromium (VI) titration in the presence of vanadium

CERN Document Server

American Society for Testing and Materials. Philadelphia

2011-01-01

1.1 This test method, commonly referred to as the Modified Davies and Gray technique, covers the titration of uranium in product, fuel, and scrap materials after the material is dissolved. The test method is versatile and has been ruggedness tested. With appropriate sample preparation, this test method can give precise and unbiased uranium assays over a wide variety of material types (1, 2). Details of the titration procedure in the presence of plutonium with appropriate modifications are given in Test Method C1204. 1.2 Uranium levels titrated are usually 20 to 50 mg, but up to 200 mg uranium can be titrated using the reagent volumes stated in this test method. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determ...

Acid-base titrations using microfluidic paper-based analytical devices.

Science.gov (United States)

Karita, Shingo; Kaneta, Takashi

2014-12-16

Rapid and simple acid-base titration was accomplished using a novel microfluidic paper-based analytical device (μPAD). The μPAD was fabricated by wax printing and consisted of ten reservoirs for reaction and detection. The reaction reservoirs contained various amounts of a primary standard substance, potassium hydrogen phthalate (KHPth), whereas a constant amount of phenolphthalein was added to all the detection reservoirs. A sample solution containing NaOH was dropped onto the center of the μPAD and was allowed to spread to the reaction reservoirs where the KHPth neutralized it. When the amount of NaOH exceeded that of the KHPth in the reaction reservoirs, unneutralized hydroxide ion penetrated the detection reservoirs, resulting in a color reaction from the phenolphthalein. Therefore, the number of the detection reservoirs with no color change determined the concentration of the NaOH in the sample solution. The titration was completed within 1 min by visually determining the end point, which required neither instrumentation nor software. The volumes of the KHPth and phenolphthalein solutions added to the corresponding reservoirs were optimized to obtain reproducible and accurate results for the concentration of NaOH. The μPADs determined the concentration of NaOH at orders of magnitude ranging from 0.01 to 1 M. An acid sample, HCl, was also determined using Na2CO3 as a primary standard substance instead of KHPth. Furthermore, the μPAD was applicable to the titrations of nitric acid, sulfuric acid, acetic acid, and ammonia solutions. The μPADs were stable for more than 1 month when stored in darkness at room temperature, although this was reduced to only 5 days under daylight conditions. The analysis of acidic hot spring water was also demonstrated in the field using the μPAD, and the results agreed well with those obtained by classic acid-base titration.

Implementation of the automated potentiometric titration method for total U at the CNEN Safeguard Laboratory, Brazil

International Nuclear Information System (INIS)

Cristiano, Barbara F.G.; Delgado, Jose U.; Araujo, Radier M.S. de; Silva, Jose W.S. da; Barros, Pedro D. de

2009-01-01

Brazilian nuclear facilities, in accordance with the regulation CNEN-NN-2.02, must have available measurement systems which allow to determine their nuclear material inventories. For the evaluation and the follow up the performance of the involved laboratories in those measurement systems, the accomplishment of interlaboratory comparison programmes becomes fundamental. Therefore, the implementation of the potentiometric titration viewing the characterization of uranium samples, represents an reference element for the Brazilian programs

Current status of tritium calorimetry at TLK

Energy Technology Data Exchange (ETDEWEB)

Buekki-Deme, A.; Alecu, C.G.; Kloppe, B.; Bornschein, B. [Institute of Technical Physics, Tritium Laboratory Karsruhe - TLK, Karlsruhe Institute of Technology - KIT, Karlsruhe (Germany)

2015-03-15

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)

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)

Calorimetry measurements in less than 20 minutes

International Nuclear Information System (INIS)

Perry, R.B.; Cremers, T.

1991-01-01

Argonne National Laboratory has developed a new series of 10 watt Bulk Plutonium Assay Calorimeters (BPAC10). The calorimeter measures bulk samples of plutonium bearing material in containers up to 5in. in diameter and 7in. high. The average measurement time is 19.7 minutes compared to 2--9 hours for the same sample measured in a water bath calorimeter. Measurement precision in the range of 1--10 watts is 1% to 0.1% and it is 0.010 watt for sample power less than 1 watt. BPAC10 series calorimeters are in use in two plutonium facilities at the EG ampersand G Rocky Flats Plant and at the Los Alamos National Laboratory TA55 Plutonium Facility. The paper presents a description of the calorimeter, discusses operating experience at Los Alamos, and presents a comparison of data on typical samples measured with both types of calorimeters. 5 refs., 5 figs., 1 tab

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.

Acid Rain Analysis by Standard Addition Titration.

Science.gov (United States)

Ophardt, Charles E.

1985-01-01

The standard addition titration is a precise and rapid method for the determination of the acidity in rain or snow samples. The method requires use of a standard buret, a pH meter, and Gran's plot to determine the equivalence point. Experimental procedures used and typical results obtained are presented. (JN)

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.

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%

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

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.).

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...