Science.gov

Sample records for cations potentiometric titration

  1. Simple sensor for potentiometric titrations

    SciTech Connect

    Selig, W.

    1982-01-01

    A sensor for potentiometric titrations was prepared by coating a spectroscopic graphite rod with a solution of poly(vinyl chloride) and dioctylphthalate in tetrahydrofuran. The reference was an Ag/AgCl single-junction electrode. The sensor was used in the following potentiometric titrations: (1) precipitation titrations, (2) acid-base titrations, (3) compleximetric titrations, and (4) redox titrations. A survey of its use in such titrations is presented. 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. 5 figures, 4 tables.

  2. Potentiometric titrations using pencil and graphite sensors

    SciTech Connect

    Selig, W.S.

    1984-01-01

    The cost of various commercial indicating electrodes ranges from about $40 for pH electrodes to as much as $355 for a potassium ion-selective electrode. This cost can be reduced to less than $1.50, and in some cases to mere pennies by making sensors from graphite rods and pencils for use in potentiometric titrations. The same sensor can be used for many types of these titrations (acid/base, compleximetric, precipitation, and redox). 8 references, 2 tables.

  3. [Semiautomatic potentiometric titration of gastric juice].

    PubMed

    Mnuskina, M M; Meerov, G I; Nadezhina, L S; Semenov, V P; Chekanina, M I; Savchenko, V P; Grinzaĭd, E L

    1990-01-01

    Using commercial equipment manufactured in this country, the authors have assembled a unit for semiautomatic potentiometric titration and developed a method for such titration, permitting a rapid determination of free and bound HCl and the total acidity of the gastric juice. The equipment and method are recommended for wide use at laboratories of therapeutic institutions, of biologic factories manufacturing medicinal commercial gastric juice, and of research institutes.

  4. The use of graphite electrodes in potentiometric titrations

    SciTech Connect

    Selig, W.S.

    1987-04-01

    The use of various types of graphite as indicator electrodes in potentiometry has been limited to acid-base and redox titrations. We have expanded the range of feasible titrations to: (1) precipitation titrations; (2) acid-base titrations; (3) compleximetric titrations; and (4) redox titrations. Graphite covered with an organic membrane containing poly(vinyl chloride) (PVC) and a plasticizer is particularly useful in monitoring the endpoints of titrations in which insoluble ion-pairs are formed. The potentiometric titration of fluoride vs La(III) or Th(IV), or of sulfate vs Pb (II) or Ba(II), which can be monitored with a plain carbon rod, is discussed.

  5. A computer-controlled potentiometric/spectrophotometric titrator

    PubMed Central

    Stong, John D.

    1988-01-01

    A laboratory computer controlled potentiometric titrator interfaced to a diode array spectrophotometer is described. The titrator consists of widely used, commercially available components; therefore, major attention is given to modes of interconnection and software implementation in data format and system control. Replicate potentiometric titrations of glycines gave a relative standard deviation in titre of 1.035% and a relative standard deviation in pH of 0.745%. Replicate spectrophotometric titrations of bromophenol blue were analysed at three wavelengths to yield pKa= 3.898 ± 0.075 (1.9% rsd). Methods of data presentation and manipulation are presented. PMID:18925194

  6. Potentiometric Acid-Base Titrations with Activated Graphite Electrodes

    NASA Astrophysics Data System (ADS)

    Riyazuddin, P.; Devika, D.

    1997-10-01

    Dry cell graphite (DCG) electrodes activated with potassium permanganate are employed as potentiometric indicator electrodes for acid-base titrations. Special attention is given to an indicator probe comprising activated DCG-non-activiated DCG electrode couple. This combination also proves suitable for the titration of strong or weak acids.

  7. Potentiometric/turbidometric titration of antiperspirant actives.

    PubMed

    Johnston, Clifford T; Hem, Stanley L; Guenin, Eric; Mattai, Jairajh; Afflito, John

    2003-01-01

    A titration procedure that simultaneously monitors the pH and turbidity of an antiperspirant solution during neutralization with sodium hydroxide was developed to characterize antiperspirant actives. Aluminum chloride, aluminum chlorohydrate (ACH), and aluminum zirconium glycine complex (AZG) gave distinctive pH/turbidity profiles. The activated forms of aluminum chlorohydrate (ACH') and aluminum zirconium glycine complex (AZG') produced more turbidity than the non-activated forms. On an equimolar basis, AZG' produced more turbidity than any of the antiperspirant actives tested. PMID:12715089

  8. Potentiometric titration and equivalent weight of humic acid

    USGS Publications Warehouse

    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.

  9. Surface characterization of hydroxyapatite: potentiometric titrations coupled with solubility measurements.

    PubMed

    Skartsila, Kyriaki; Spanos, Nikos

    2007-04-15

    The acid-base properties of synthetically prepared and well-characterized hydroxyapatite (HAP) in contact with KNO3 solutions were investigated at 25 degrees C, through potentiometric titrations, zeta-potential measurements, and surface complex modeling. Aliquots of suspension were withdrawn every 0.5 pH unit during the titration procedure and analyzed for calcium and phosphate. It was found that, even for rapid titration experiments, a remarkable amount of H+ ions (H+dissol.) is consumed in the bulk solution in reacting with species coming from the dissolution of HAP. These H+ ions must be taken into account in the H+ mass balance, in order for true value for the point of zero charge (pzc=6.5+/-0.2) and consequently true value for the surface charge (sigma0) to be obtained. Besides the conventional potentiometric titration technique, it was found that pzc may be determined much more easily as the intersection point of the suspension titration curve and the blank one modified to include the amount of H+dissol. obtained at one ionic strength. Finally, a surface complexation model was proposed for the development of surface charge. Experimental data were satisfactorily fitted by using the value of 4.2 F m-2 for the capacitance.

  10. Semi-automated potentiometric titration method for uranium characterization.

    PubMed

    Cristiano, B F G; Delgado, J U; da Silva, J W S; de Barros, P D; de Araújo, R M S; Lopes, R T

    2012-07-01

    The manual version of the potentiometric titration method has been used for certification and characterization of uranium compounds. In order to reduce the analysis time and the influence of the analyst, a semi-automatic version of the method was developed in the Brazilian Nuclear Energy Commission. The method was applied with traceability assured by using a potassium dichromate primary standard. The combined standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization.

  11. Semi-automated potentiometric titration method for uranium characterization.

    PubMed

    Cristiano, B F G; Delgado, J U; da Silva, J W S; de Barros, P D; de Araújo, R M S; Lopes, R T

    2012-07-01

    The manual version of the potentiometric titration method has been used for certification and characterization of uranium compounds. In order to reduce the analysis time and the influence of the analyst, a semi-automatic version of the method was developed in the Brazilian Nuclear Energy Commission. The method was applied with traceability assured by using a potassium dichromate primary standard. The combined standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization. PMID:22154105

  12. Charge characteristics of humic and fulvic acids: comparative analysis by colloid titration and potentiometric titration with continuous pK-distribution function model.

    PubMed

    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.

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

    PubMed

    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.

  14. Characterization of Sea Lettuce Surface Functional Groups by Potentiometric Titrations

    NASA Astrophysics Data System (ADS)

    Ebling, A. M.; Schijf, J.

    2008-12-01

    In pursuit of our ultimate goal to better understand the prodigious capacity of the marine macroalga Ulva lactuca (sea lettuce) for adsorbing a broad range of dissolved trace metals from seawater, we performed an initial characterization of its surface functional groups. Specifically, the number of distinct functional groups as well as their individual bulk concentrations and acid dissociation constants (pKas) were determined by potentiometric titrations in NaCl solutions of various ionic strengths (I = 0.01-5.0 M), under inert nitrogen atmosphere at 25°C. Depending on the ionic strength, Ulva samples were manually titrated down to pH 2 or 3 with 1 N HCl and then up to pH 10 with 1 N NaOH in steps of 0.1-0.2 units, continuously monitoring pH with a glass combination electrode. Titrations of a dehydrated Ulva standard reference material (BCR-279) were compared with fresh Ulva tissue cultured in our laboratory. A titration in filtered natural seawater was also compared with one in an NaCl solution of equal ionic strength. Equilibrium constants for the ionization of water in NaCl solutions as a function of ionic strength were obtained from the literature. Fits to the titration data ([H]T vs. pH) were performed with the FITEQL4.0 computer code using non-electrostatic 3-, 4-, and 5-site models, either by fixing ionic strength at its experimental value or by allowing it to be extrapolated to zero, while considering all functional group pKas and bulk concentrations as adjustable parameters. Since pKas and bulk concentrations were found to be strongly correlated, the latter were also fixed in some cases to further constrain the pKas. Whereas these calculations are currently ongoing, preliminary results point to three, possibly four, functional groups with pKas of about 4.1, 6.3, and 9.5 at I = 0. Bulk concentrations of the three groups are very similar, about 5-6×10-4 mol/g based on dry weight, which suggests that all are homogeneously distributed over the surface and

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

    NASA Astrophysics Data System (ADS)

    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.

  16. Analysis of the sorption properties of different soils using water vapour adsorption and potentiometric titration methods

    NASA Astrophysics Data System (ADS)

    Skic, Kamil; Boguta, Patrycja; Sokołowska, Zofia

    2016-07-01

    Parameters of specific surface area as well as surface charge were used to determine and compare sorption properties of soils with different physicochemical characteristics. The gravimetric method was used to obtain water vapour isotherms and then specific surface areas, whereas surface charge was estimated from potentiometric titration curves. The specific surface area varied from 12.55 to 132.69 m2 g-1 for Haplic Cambisol and Mollic Gleysol soil, respectively, and generally decreased with pH (R=0.835; α = 0.05) and when bulk density (R=-0.736; α = 0.05) as well as ash content (R=-0.751; α = 0.05) increased. In the case of surface charge, the values ranged from 63.00 to 844.67 μmol g-1 Haplic Fluvisol and Mollic Gleysol, respecively. Organic matter gave significant contributions to the specific surface area and cation exchange capacity due to the large surface area and numerous surface functional groups, containing adsorption sites for water vapour molecules and for ions. The values of cation exchange capacity and specific surface area correlated linearly at the level of R=0.985; α = 0.05.

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

    PubMed

    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.

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

    PubMed

    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.

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

    PubMed

    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. PMID:27444048

  20. A numerical method of finding potentiometric titration end-points by use of approximative spline functions.

    PubMed

    Ren, K

    1990-07-01

    A new numerical method of determining potentiometric titration end-points is presented. It consists in calculating the coefficients of approximative spline functions describing the experimental data (e.m.f., volume of titrant added). The end-point (the inflection point of the curve) is determined by calculating zero points of the second derivative of the approximative spline function. This spline function, unlike rational spline functions, is free from oscillations and its course is largely independent of random errors in e.m.f. measurements. The proposed method is useful for direct analysis of titration data and especially as a basis for construction of microcomputer-controlled automatic titrators. PMID:18964999

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

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

    PubMed

    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.

  4. Nonaqueous potentiometric titration and elemental analysis of high-boiling distillates of Saudi Arabian crude oils

    SciTech Connect

    Ali, M.F.; Ali, M.A. )

    1988-12-01

    Nonaqueous potentiometric titration and elemental analysis were used to study basic and nonbasic functionalities present in high-boiling distillates of four Saudi Arabian crude oils. Model nitrogen compounds were titrated under similar titration conditions to differentiate them into strong, weak and nonbasic species. The strong bses titrated were due to the presence of of pyridine and its benzologs like acridines, phenanthridines and quionolines. The weak bases titrated were due to phenazxines and amides whereas the pyrroles, indoles and carbazoles were found to be nonbasic in nature. The total nitrogen and the total basic nitrogen compounds were generally found to be in very low concentration in the four crude oil distillates. A gradual decrease in the basicity of the distillates was found from Arab Heavy to Arab Extra Light through Arab Medium and Arab Light crude oils.

  5. Determination of sulfur compounds in hydrotreated transformer base oil by potentiometric titration.

    PubMed

    Chao, Qiu; Sheng, Han; Cheng, Xingguo; Ren, Tianhui

    2005-06-01

    A method was developed to analyze the distribution of sulfur compounds in model sulfur compounds by potentiometric titration, and applied to analyze hydrotreated transformer base oil. Model thioethers were oxidized to corresponding sulfoxides by tetrabutylammonium periodate and sodium metaperiodate, respectively, and the sulfoxides were titrated by perchloric acid titrant in acetic anhydride. The contents of aliphatic thioethers and total thioethers were then determined from that of sulfoxides in solution. The method was applied to determine the organic sulfur compounds in hydrotreated transformer base oil.

  6. Semi-automatic version of the potentiometric titration method for characterization of uranium compounds.

    PubMed

    Cristiano, Bárbara F G; Delgado, José Ubiratan; da Silva, José Wanderley S; de Barros, Pedro D; de Araújo, Radier M S; Dias, Fábio C; Lopes, Ricardo T

    2012-09-01

    The potentiometric titration method was used for characterization of uranium compounds to be applied in intercomparison programs. The method is applied with traceability assured using a potassium dichromate primary standard. A semi-automatic version was developed to reduce the analysis time and the operator variation. The standard uncertainty in determining the total concentration of uranium was around 0.01%, which is suitable for uranium characterization and compatible with those obtained by manual techniques. PMID:22406220

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

    PubMed

    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.

  8. Determination of peroxyl radical scavenging activity of flavonoids and plant extracts using an automatic potentiometric titrator.

    PubMed

    Sano, Mitsuaki; Yoshida, Risa; Degawa, Masakuni; Miyase, Toshio; Yoshino, Kyoji

    2003-05-01

    A novel potentiometric method for evaluation of peroxyl radical scavenging activity of flavonoids and plant extracts was developed. The oxidation of potassium iodide (KI) was performed in acetonitrilephosphate buffer (1:1) containing antioxidant using 2,2'-azobis(2-amidinopropane) dihydrochloride as a peroxyl radical generator. The amount of iodine released from KI during a 20-min free radical oxidation was determined quantitatively using an automatic potentiometric titrator with sodium thiosulfate. The radical scavenging activity of the sample was expressed as the inhibition ratio for iodine release of the control group mediated by the radical. The results obtained from some authentic polyphenols correlated well with those of previous reports. This is a simple, time-saving method requiring less than 30 min and is useful in assessing the radical scavenging activity of antioxidants in plant extracts. We describe the radical scavenging activities of various flavonoids including 21 kinds of tea catechins and vegetable extracts by this method.

  9. Iodine--iodide reference electrode for potentiometric titrations of bases in acetic acid.

    PubMed

    Maccà, Carlo; Soldà, Lidia

    2002-03-01

    The suitability of the half-cell Pt/I2, KI in glacial acetic acid as reference electrode for potentiometric titrations of weak bases in the same medium was investigated. This electrode is easily prepared. It has been found very convenient in use and performing at least as well as the best electrodes used for the same purpose. Some phenomenological aspects of the behaviour of the above half-cell, of interest for the use as the reference electrode in the laboratory practice have been observed, that show important differences respect aqueous medium and other organic solvents.

  10. A comparison of coulometric titration and potentiometric determination of chloride concentration in rumen fluid.

    PubMed

    Cebra, Christopher K.; Tornquist, Susan J.; Vap, Lomda M.; Dodson, Linda A.

    2001-01-01

    The concentration of chloride ions in rumen fluid is a useful measure of obstructive gastrointestinal disease in ruminants and camelids. However, rumen fluid is very different from other biological fluids in its bacterial populations, consistency, and concentrations of various anions. Two methods of determining the chloride concentration in biological fluids were compared using centrifuged and filtered rumen fluid containing different amounts of sodium chloride. Although coulometric titration and potentiometric electrode analysis yielded results that had a strong linear relationship, the results of potentiometry were consistently and significantly higher, by about 20 mEq/L. This difference was investigated further by analyzing a series of fluids containing different concentrations of sodium acetate. Acetate was detected as chloride (0.21 chloride molecules per acetate molecule) by potentiometry but not by coulometric titration. Therefore, the acetate concentration of rumen fluid was the most likely cause of the discrepancy between tests in the original trial. In conclusion, the coulometric procedure may be more accurate than the potentiometric procedure for measuring rumen chloride when the concentrations of possible confounding ions are unknown.

  11. Spectrophotometric study and potentiometric titration between sulfite and nitrite ions using acetaldehyde complex of nitroprusside as a carrier

    SciTech Connect

    Ahmed, Y.Z.; Abd-Elmottalb, M.

    1985-11-01

    A complex between sodium nitroprusside (NP) and acetaldehyde of 1:1 in aqueous solution of pH 10 has been prepared and used as an analytical reagent for the spectrophotometric determination of sulfite and nitrite ions. Nitrite ion can be titrated against sulfite ion and vise versa in equivalent amounts with high accuracy in the presence of the acetaldehyde complex of nitroprusside as a carrier using a potentiometric titration technique. 9 references, 3 figures, 2 tables.

  12. Protein-salt binding data from potentiometric titrations of lysozyme in aqueous solutions containing KCl

    SciTech Connect

    Engmann, J.; Blanch, H.W.; Prausnitz, J.M. |

    1997-03-01

    An existing method for potentiometric titrations of proteins was improved, tested and applied to titrations of the enzyme hen-egg-white lysozyme in aqueous solutions containing KCl at ionic strengths from 0.1 M to 2.0 M at 25 C. Information about the protein`s net charge dependence on pH and ionic strength were obtained and salt binding numbers for the system were calculated using a linkage concept. For the pH range 2.5--11.5, the net charge slightly but distinctly increases with increasing ionic strength between 0.1 M and 2.0 M. The differences are most distinct in the pH region below 5. Above pH 11.35, the net charge decreases with increasing ionic strength. Preliminary calculation of binding numbers from titration curves at 0.1 M and 1.0 M showed selective association of chloride anions and expulsion of potassium ions at low pH. Ion-binding numbers from this work will be used to evaluate thermodynamic properties and to correlate crystallization or precipitation phase-equilibrium data in terms of a model based on the integral-equation theory of fluids which is currently under development.

  13. Determination of vanadium(V) by direct automatic potentiometric titration with EDTA using a chemically modified electrode as a potentiometric sensor.

    PubMed

    Quintar, S E; Santagata, J P; Cortinez, V A

    2005-10-15

    A chemically modified electrode (CME) was prepared and studied as a potentiometric sensor for the end-point detection in the automatic titration of vanadium(V) with EDTA. The CME was constructed with a paste prepared by mixing spectral-grade graphite powder, Nujol oil and N-2-naphthoyl-N-p-tolylhydroxamic acid (NTHA). Buffer systems, pH effects and the concentration range were studied. Interference ions were separated by applying a liquid-liquid extraction procedure. The CME did not require any special conditioning before using. The electrode was constructed with very inexpensive materials and was easily made. It could be continuously used, at least two months without removing the paste. Automatic potentiometric titration curves were obtained for V(V) within 5 x 10(-5) to 2 x 10(-3)M with acceptable accuracy and precision. The developed method was applied to V(V) determination in alloys for hip prosthesis. PMID:18970248

  14. A new numerical method of finding potentiometric titration end-points by use of rational spline functions.

    PubMed

    Ren, K; Ren-Kurc, A

    1986-08-01

    A new numerical method of determining the position of the inflection point of a potentiometric titration curve is presented. It consists of describing the experimental data (emf, volume data-points) by means of a rational spline function. The co-ordinates of the titration end-point are determined by analysis of the first and second derivatives of the spline function formed. The method also allows analysis of distorted titration curves which cannot be interpreted by Gran's or other computational methods. PMID:18964159

  15. Potentiometric study of reaction between periodate and iodide as their tetrabutylammonium salts in chloroform. Application to the determination of iodide and potentiometric detection of end points in acid-base titrations in chloroform.

    PubMed

    Pournaghi-Azar, M H; Farhadi, K

    1995-03-01

    A potentiometric method for the titration of tetrabutylammonium iodide (TBAI) in chloroform using tetrabutylammonium periodate (TBAPI) as a strong and suitable oxidizing reagent is described. The potentiometric conditions were optimized and the equilibrium constants of the reactions occurring during the titration were determined. The method was used for the determination of iodide both in chloroform and aqueous solutions after extraction into chloroform as ion-association with tetraphenylarsonium. The reaction between TBAPI and TBAI was also used as acid indicator for the potentiometric detection of end points of acid-base titrations in chloroform.

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

    PubMed

    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.

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

    PubMed

    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. PMID:21140668

  18. Studies of Mg2+/Ca2+ complexes of naturally occurring dinucleotides: potentiometric titrations, NMR, and molecular dynamics.

    PubMed

    Stern, Noa; Major, Dan Thomas; Gottlieb, Hugo Emilio; Weizman, Daniel; Sayer, Alon Haim; Blum, Eliav; Fischer, Bilha

    2012-08-01

    Dinucleotides (Np(n)N'; N and N' are A, U, G, or C, n = 2-7) are naturally occurring physiologically active compounds. Despite the interest in dinucleotides, the composition of their complexes with metal ions as well as their conformations and species distribution in living systems are understudied. Therefore, we investigated a series of Mg(2+) and Ca(2+) complexes of Np(n)N's. Potentiometric titrations indicated that a longer dinucleotide polyphosphate (N is A or G, n = 3-5) linker yields more stable complexes (e.g., log K of 2.70, 3.27, and 3.73 for Ap(n)A-Mg(2+), n = 3, 4, 5, respectively). The base (A or G) or ion (Mg(2+) or Ca(2+)) has a minor effect on K(M)(ML) values. In a physiological medium, the longer Ap(n)As (n = 4, 5) are predicted to occur mostly as the Mg(2+)/Ca(2+) complexes. (31)P NMR monitored titrations of Np(n)N's with Mg(2+)/Ca(2+) ions showed that the middle phosphates of the dinucleotides coordinate with Mg(2+)/Ca(2+). Multidimensional potential of mean force (PMF) molecular dynamics (MD) simulations suggest that Ap(2)A and Ap(4)A coordinate Mg(2+) and Ca(2+) ions in both inner-sphere and outer-sphere modes. The PMF MD simulations additionally provide a detailed picture of the possible coordination sites, as well as the cation binding process. Moreover, both NMR and MD simulations showed that the conformation of the nucleoside moieties in Np(n)N'-Mg(2+)/Ca(2+) complexes remains the same as that of free mononucleotides.

  19. Determination of phosphorous in titanium bearing minerals by potentiometric titration using Pb-ion selective electrode.

    PubMed

    Ramadoss, K; Murty, D S; Mahanta, P L; Gomathy, B; Rangaswamy, R

    2000-01-24

    A method for phosphorous determination in titanium bearing minerals by potentiometric titration using a Pb-ion selective electrode has been developed. Sample decomposition is achieved by means of K(2)CO(3) fusion in a platinum crucible at 800 degrees C for 30 min in a muffle furnace, and subsequent leaching with water of the fused melt. The aqueous leachate is neutralised with HClO(4) and subsequent boiling. The obtained solution is used for titration with Pb(ClO(4))(2), and the Pb-ion selective electrode detects the end point. The lowest concentration determinable is 0.02% P(2)O(5) in a solid sample. The method was applied on in-house titanium bearing mineral samples and on IGS-31 ilmenite sample (British Geological Survey, UK). Synthetic samples were prepared and analysed, and phosphorous recovery is in the range 98-106%. The recovery and accuracy of the present method have been validated by spiking experiments and by comparing with the spectrophotometric values, respectively. The precision of the proposed method in terms of relative standard deviation is 2.0%. PMID:18967837

  20. Potentiometric titrations of five synthetic tetraacids as models for indigenous C80 tetraacids.

    PubMed

    Sundman, Ola; Nordgård, Erland L; Grimes, Brian; Sjöblom, Johan

    2010-02-01

    The acid/base properties, critical micelle concentrations (cmcs), and pH-dependent solubility of five synthetic tetraacids have been studied at several ionic strengths (20-600 mM NaCl) and in the pH range of 1.5-11 using high precision potentiometric titrations, tensiometer measurements, and UV spectroscopy, respectively. The molecular weight of the tetraacids ranged between 478 and 983 g/mol. The potentiometric titration data was evaluated in terms of thermodynamic equilibrium models, developed in the light of relevant solubility data, Langmuir monolayer compressions and cmc of the different tetraacids. The results indicate that for two of the tetraacids, called BP5 and BP7, two chemical forms fully dominate the speciation of the monomers; the insoluble fully protonated form, and the soluble fully deprotonated form. The partly protonated species, only play a very minor role in the speciation of these tetraacids. For the other tetraacids the results are more complicated; for the smallest tetraacid, called BP1, all species seem to play important roles, and for the most hydrophobic, BP10, the formation of micelles and aggregates severely complicates the evaluation of the speciation. For the tetraacid BP3 one of the partly deprotonated forms seems to be important, thus confirming the structure to properties relationship. In spite of the complicated micelle formation chemistry, and although not actually measured, the acid/base properties for the monomers of BP10 were interpreted by means of surface charge densities of the micellar aggregates. The modeling indicates an increase of the aggregation number of the micelle upon acidification, a result of formation of mixed micelles incorporating the fully protonated and deprotonated species. An intrinsic pK(a) of 5.4 for BP5 was used to model the monomer pK(a) of BP10, and corresponded well with a monolayer acidity constant pK(s)(a) of 5.5 obtained from surface collapse pressures of Langmuir monolayers as a function of pH.

  1. Estimating the organic acid contribution to coastal seawater alkalinity by potentiometric titrations in a closed cell.

    PubMed

    Muller, François L L; Bleie, Bjørn

    2008-07-01

    This paper examines the performance of a previously reported, closed cell, potentiometric titration technique [J.M. Hernández-Ayón, S.L. Belli, A. Zirino, Anal. Chim. Acta 394 (1999) 101] for the simultaneous determination of pH, total inorganic carbon (TCO2), total alkalinity (TA), and organic alkalinity (OA) in coastal seawater samples. A novel interpretation of the titration data, as recently proposed by Hernández-Ayón et al. [J.M. Hernández-Ayón, A. Zirino, A.G. Dickson, T. Camiro-Vagas, E. Valenzuela-Espinoza, Limnol. Oceanogr.: Methods 5 (2007) 225] who applied it to waters of unusually high organic matter content, was applied here to fjord surface waters collected over the duration of a phytoplankton bloom. The parameters pH and TCO2--combined with knowledge of boric, phosphate and silicate species concentrations--allowed calculation of all inorganic species that contributed to TA. This inorganic alkalinity term was then subtracted from TA to produce an estimation of OA. Although the OA values obtained were very small (2-22+/-3 micromol L(-1)), they showed a reproducible trend over time in two simultaneous experiments. The organic acids that may have contributed to OA were characterised in back titrations of acidified and CO2-stripped samples with CO2-free NaOH. Two classes of organic titratable species, with pK(a) values around 4.0+/-0.2 and 9.1+/-0.2 were detected. The first occurred in concentrations that co-varied linearly (r2=0.75) with protein-like fluorescence, indicating a marine biological source, but were only weakly correlated (r2=0.46) to OA. By contrast, Class 2 organic species were not significantly correlated to any fluorescence component of either marine or terrestrial origin but were linearly correlated to OA (r2=0.69). These new results reveal that the method proposed by Hernández-Ayón et al. [J.M. Hernández-Ayón, A. Zirino, A.G. Dickson, T. Camiro-Vagas, E. Valenzuela-Espinoza, Limnol. Oceanogr.: Methods 5 (2007) 225] for

  2. Polypyrrole-calcion film as a membrane and solid-contact in an indicator electrode for potentiometric titrations.

    PubMed

    Blaz, T; Migdalski, J; Lewenstam, A

    2000-06-21

    This paper shows the application of conducting polymers (CPs) for constructing potentiometric indicator electrodes. Two types of polypyrrole (PPy)-based calcium sensors are presented, one sensor with PPy-calcion film as the active part and the other sensor with PPy-calcion as a solid-state contact coated with a conventional membrane selective towards calcium ions. It is shown that the PPy-calcion film, due to the complexing properties of calcion ensuring high loading of the film with calcium, is sufficiently selective to be used as the active part or as a mediating layer of the indicator electrode. The electrode, with PPy-calcion film as the active part, was used as the indicator electrode in potentiometric titrations of calcium in mixed solvents, where conventional PVC-based electrode can not be used. For the first time, the practical applicability of PPy-based electrodes in titrations is demonstrated.

  3. Cell wall reactivity of acidophilic and alkaliphilic bacteria determined by potentiometric titrations and Cd adsorption experiments.

    PubMed

    Kenney, Janice P L; Fein, Jeremy B

    2011-05-15

    In this study, we used potentiometric titrations and Cd adsorption experiments to determine the binding capacities of two acidophilic (A. cryptum and A. acidophilum) and two alkaliphilic (B. pseudofirmus and B. circulans) bacterial species in order to determine if any consistent trends could be observed relating bacterial growth environment to proton and Cd binding properties and to compare those binding behaviors to those of neutrophilic bacteria. All of the bacterial species studied exhibited significant proton buffering over the pH range in this study, with the alkaliphiles exhibiting significantly higher acidity constants than the acidophiles as well as the neutrophilic bacterial consortia. The calculated average site concentrations for each of the bacteria in this study are within 2σ experimental error of each other, with the exception of A. cryptum, which has a significantly higher Site 2 concentration than the other species. Despite differing acidity constants between the acidophiles and alkaliphiles, all bacteria except A. cryptum exhibited remarkably similar Cd adsorption behavior to each other, and the observed extent of adsorption was also similar to that predicted from a generalized model derived using neutrophilic bacterial consortia. This study demonstrates that bacteria that grow under extreme conditions exhibit similar proton and metal adsorption behavior to that of previously studied neutrophilic species and that a single set of proton and metal binding constants can be used to model the behavior of bacterial adsorption under a wide range of environmental conditions.

  4. Micellar acid-base potentiometric titrations of weak acidic and/or insoluble drugs.

    PubMed

    Gerakis, A M; Koupparis, M A; Efstathiou, C E

    1993-01-01

    The effect of various surfactants [the cationics cetyl trimethyl ammonium bromide (CTAB) and cetyl pyridinium chloride (CPC), the anionic sodium dodecyl sulphate (SDS), and the nonionic polysorbate 80 (Tween 80)] on the solubility and ionization constant of some sparingly soluble weak acids of pharmaceutical interest was studied. Benzoic acid (and its 3-methyl-, 3-nitro-, and 4-tert-butyl-derivatives), acetylsalicylic acid, naproxen and iopanoic acid were chosen as model examples. Precise and accurate acid-base titrations in micellar systems were made feasible using a microcomputer-controlled titrator. The response curve, response time and potential drift of the glass electrode in the micellar systems were examined. The cationics CTAB and CPC were found to increase considerably the ionization constant of the weak acids (delta pKa ranged from -0.21 to -3.57), while the anionic SDS showed negligible effect and the nonionic Tween 80 generally decreased the ionization constants. The solubility of the acids in aqueous micellar and acidified micellar solutions was studied spectrophotometrically and it was found increased in all cases. Acetylsalicylic acid, naproxen, benzoic acid and iopanoic acid could be easily determined in raw material and some of them in pharmaceutical preparations by direct titration in CTAB-micellar system instead of using the traditional non-aqueous or back titrimetry. Precisions of 0.3-4.3% RSD and good correlation with the official tedious methods were obtained. The interference study of some excipients showed that a preliminary test should be carried out before the assay of formulations.

  5. On the accuracy of acid-base determinations from potentiometric titrations using only a few points from the titration curve.

    PubMed

    Olin, A; Wallén, B

    1977-05-01

    There are several procedures which use only a few points on the titration curve for the calculation of equivalence volumes in acid-base titrations. The accuracy of such determinations will depend on the positions of the points on the titration curve. The effects of errors in the stability constants and in the pH measurements on the accuracy of the analysis have been considered, and the results are used to establish the conditions under which these errors are minimized.

  6. Analysis of variance in determinations of equivalence volume and of the ionic product of water in potentiometric titrations.

    PubMed

    Braibanti, A; Bruschi, C; Fisicaro, E; Pasquali, M

    1986-06-01

    Homogeneous sets of data from strong acid-strong base potentiometric titrations in aqueous solution at various constant ionic strengths have been analysed by statistical criteria. The aim is to see whether the error distribution matches that for the equilibrium constants determined by competitive potentiometric methods using the glass electrode. The titration curve can be defined when the estimated equivalence volume VEM, with standard deviation (s.d.) sigma (VEM), the standard potential E(0), with s.d. sigma(E(0)), and the operational ionic product of water K(*)(w) (or E(*)(w) in mV), with s.d. sigma(K(*)(w)) [or sigma(E(*)(w))] are known. A special computer program, BEATRIX, has been written which optimizes the values of VEM, E(0) and K(*)(w) by linearization of the titration curve as a Gran plot. Analysis of variance applied to a set of 11 titrations in 1.0M sodium chloride medium at 298 K has demonstrated that the values of VEM belong to a normal population of points corresponding to individual potential/volume data-pairs (E(i); v(i)) of any titration, whereas the values of pK(*)(w) (or of E(*)(w)) belong to a normal population with members corresponding to individual titrations, which is also the case for the equilibrium constants. The intertitration variation is attributable to the electrochemical component of the system and appears as signal noise distributed over the titrations. The correction for junction-potentials, introduced in a further stage of the program by optimization in a Nernst equation, increases the noise, i.e., sigma(pK(*)(w)). This correction should therefore be avoided whenever it causes an increase of sigma(pK(*)(w)). The influence of the ionic medium has been examined by processing data from acid-base titrations in 0.1M potassium chloride and 0.5M potassium nitrate media. The titrations in potassium chloride medium showed the same behaviour as those in sodium chloride medium, but with an s.d. for pK(*)(w) that was smaller and close to the

  7. Comparison of a miniaturized shake-flask solubility method with automated potentiometric acid/base titrations and calculated solubilities.

    PubMed

    Glomme, A; März, J; Dressman, J B

    2005-01-01

    Solubility is one of the most important parameters for lead selection and optimization during drug discovery. Its determination should therefore take place as early as possible in the process. Because of the large numbers of compounds involved and the very low amounts of each compound available in the early development stage, it is highly desirable to measure the solubility with as little compound as possible and to be able to improve the throughput of the methods used. In this work, a miniaturized shake-flask method was developed and the solubility results were compared with those measured by semiautomated potentiometric acid/base titrations and computational methods for 21 poorly soluble compounds with solubilities mostly in the range 0.03-30 microg/mL. The potentiometric method is very economical (approximately 100 microg of a poorly soluble compound is needed) and is able to create a pH/solubility profile with one single determination, but is limited to ionizable compounds. The miniaturized shake-flask method can be used for all compounds and a wide variety of media. Its precision and throughput proved superior to the potentiometric method for very poorly soluble compounds. Up to 20 compounds a week can be studied with one set-up. Calculated solubility data seem to be sufficient for a first estimate of the solubility, but they cannot currently be used as a substitute for experimental measurements at key decision points in the development process.

  8. A potential high-throughput method for the determination of lipase activity by potentiometric flow injection titrations.

    PubMed

    Vahl, Katja; Kahlert, Heike; Böttcher, Dominique; Wardenga, Rainer; Komorsky-Lovrić, Sebojka; Bornscheuer, Uwe; Scholz, Fritz

    2008-03-01

    Potentiometric FIA titrations were performed to determine enzyme activities of lipase type B from Candida antarctica, CAL-B. Two substrates, triacetin and tributyrin were hydrolyzed in phosphate buffer solutions, and the concentration change of the base component of the buffer was titrated in a carrier solution containing hydrochloric acid and potassium chloride. The system was calibrated with butyric acid and acetic acid, respectively. FIA titration peaks were evaluated with respect to peak height and peak area. Butyric acid and acetic acid could be titrated in the buffer solution from 3x10(-3) mol L(-1) to 0.1 mol L(-1). The detection limit of enzyme activity was determined to be 0.07 U mL(-1) (15 min reaction time) and the minimum activity was calculated to be 0.035 units corresponding to 35 nmol min(-1). The specific activities of lipase B for the hydrolysis of tributyrin and triacetin were determined as 16+/-2 U mg(-1) and 2+/-0.2 U mg(-1) (per mg commercial lipase preparation), respectively.

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

    SciTech Connect

    Zarzycki, Piotr P.; 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 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.

  10. Investigating the early stages of mineral precipitation by potentiometric titration and analytical ultracentrifugation.

    PubMed

    Kellermeier, Matthias; Cölfen, Helmut; Gebauer, Denis

    2013-01-01

    Despite the importance of crystallization for various areas of research, our understanding of the early stages of the mineral precipitation from solution and of the actual mechanism of nucleation is still rather limited. Indeed, detailed insights into the processes underlying nucleation may enable a systematic development of novel strategies for controlling mineralization, which is highly relevant for fields ranging from materials chemistry to medicine. In this work, we describe experimental aspects of a quantitative assay, which relies on pH titrations combined with in situ metal ion potentiometry and conductivity measurements. The assay has originally been designed to study the crystallization of calcium carbonate, one of the most abundant biominerals. However, the developed procedures can also be readily applied to any compound containing cations for which ion-selective electrodes are available. Besides the possibility to quantitatively assess ion association prior to nucleation and to directly determine thermodynamic solubility products of precipitated phases, the main advantage of the crystallization assay is the unambiguous identification of the different stages of precipitation (i.e., prenucleation, nucleation, and early postnucleation) and the characterization of the multiple effects of additives. Furthermore, the experiments permit targeted access to distinct precursor species and intermediate stages, which thus can be analyzed by additional methods such as cryo-electron microscopy or analytical ultracentrifugation (AUC). Regarding ion association in solution, AUC detects entities significantly larger than simple ion pairs, so-called prenucleation clusters. Sedimentation coefficient values and distributions obtained for the calcium carbonate system are discussed in light of recent insights into the structural nature of prenucleation clusters.

  11. Characterization of acid functional groups of carbon dots by nonlinear regression data fitting of potentiometric titration curves

    NASA Astrophysics Data System (ADS)

    Alves, Larissa A.; de Castro, Arthur H.; de Mendonça, Fernanda G.; de Mesquita, João P.

    2016-05-01

    The oxygenated functional groups present on the surface of carbon dots with an average size of 2.7 ± 0.5 nm were characterized by a variety of techniques. In particular, we discussed the fit data of potentiometric titration curves using a nonlinear regression method based on the Levenberg-Marquardt algorithm. The results obtained by statistical treatment of the titration curve data showed that the best fit was obtained considering the presence of five Brønsted-Lowry acids on the surface of the carbon dots with constant ionization characteristics of carboxylic acids, cyclic ester, phenolic and pyrone-like groups. The total number of oxygenated acid groups obtained was 5 mmol g-1, with approximately 65% (∼2.9 mmol g-1) originating from groups with pKa < 6. The methodology showed good reproducibility and stability with standard deviations below 5%. The nature of the groups was independent of small variations in experimental conditions, i.e. the mass of carbon dots titrated and initial concentration of HCl solution. Finally, we believe that the methodology used here, together with other characterization techniques, is a simple, fast and powerful tool to characterize the complex acid-base properties of these so interesting and intriguing nanoparticles.

  12. Effect of Surface Site Interactions on Potentiometric Titration of Hematite (α-Fe2O3) Crystal Faces

    SciTech Connect

    Chatman, Shawn ME; Zarzycki, Piotr P.; Preocanin, Tajana; Rosso, Kevin M.

    2013-02-01

    Time dependent potentiometric pH titrations were used to study the effect of atomic scale surface structure on the protonation behavior of the structurally well defined hematite/aqueous electrolyte interfaces. Our recently proposed thermodynamic model [1,23] was applied to measured acidimetric and alkalimetric titration hysteresis loops, collected from highly organized (001), (012), and (113) crystal face terminations using pH equilibration times ranging from 15 to 30 mins. Hysteresis loop areas indicate that (001) faces equilibrate faster than the (012) and (113) faces, consistent with the different expected ensembles of singly, doubly, and triply coordinated surface sites on each face. Strongly non-linear hysteretic pH-potential relationships were found, with slopes exceeding Nernstian, collectively indicating that protonation and deprotonation is much more complex than embodied in present day surface complexation models. The asymmetrical shape of the acidimetric and alkalimetric titration branches were used to illustrate a proposed steric "leaky screen" repulsion/trapping interaction mechanism that stems from high affinity singly-coordinated sites electrostatically and sterically screening lower affinity doubly and triply coordinated sites. Our data indicate that site interaction is the dominant phenomenon defining surface potential accumulation behavior on single crystal faces of metal oxide minerals.

  13. Determination of the degree of substitution of sodium carboxymethylcellulose by potentiometric titration and use of the extended henderson-hasselbalch equation and the simplex method for the evaluation.

    PubMed

    Aggeryd, I; Olin, A

    1985-08-01

    Determination of the degree of substitution, D.S., of purified sodium carboxymethylcellulose, CMC, by potentiometric titration has been studied. Different mathematical descriptions of the acid-base properties of polyelectrolytes were tested on the titration curve. It was found that the extended Henderson-Hasselbalch equation reproduced the measured data well. It was therefore used as a basis for evaluating D.S. by the simplex method. The influence of ionic strength, I, on the shape of the titration curve was investigated and the effect of I on the precision of the titrations was evaluated. The titrations showed a precision of +/- 0.004 D.S.-units and the results were in agreement with those obtained from a dry-ashing method, within +/- 0.02 D.S.-units. The whole method, including preparation of solutions and titration, showed a precision of +/- 0.01 D.S.-units.

  14. Potentiometric titrations in acetonitrile-water mixtures: evaluation of aqueous ionisation constant of ketoprofen.

    PubMed

    Herrador, M Angeles; González, A Gustavo

    2002-03-11

    Non ideality of acetonitrile-water mixtures was studied from data on the excess of molar volumes and viscosities. pH and autoprotolisis constants were evaluated at the standard state of the mixed solvent from titrations of a strong acid with a strong base. In order to illustrate the evaluation of the aqueous ionisation constant of water insoluble compounds from pH titrations in ACN-water mixtures, a typical insoluble arylpropionic acid, ketoprofen, was chosen. Ketoprofen was titrated in mixtures from 10 to 70% w/w of acetonitrile against a strong base. From the titration data, the ionisation constant of ketoprofen was evaluated at the standard state of the solvent mixture (pK(a)(*)). Aqueous pK(a) was determined by extrapolation, as the intercept of the plot of pK(a)(*) versus ACN mole fraction.

  15. Automated potentiometric titrations in KCl/water-saturated octanol: method for quantifying factors influencing ion-pair partitioning.

    PubMed

    Scherrer, Robert A; Donovan, Stephen F

    2009-04-01

    The knowledge base of factors influencing ion pair partitioning is very sparse, primarily because of the difficulty in determining accurate log P(I) values of desirable low molecular weight (MW) reference compounds. We have developed a potentiometric titration procedure in KCl/water-saturated octanol that provides a link to log P(I) through the thermodynamic cycle of ionization and partitioning. These titrations have the advantage of being independent of the magnitude of log P, while maintaining a reproducibility of a few hundredths of a log P in the calculated difference between log P neutral and log P ion pair (diff (log P(N - I))). Simple model compounds can be used. The titration procedure is described in detail, along with a program for calculating pK(a)'' values incorporating the ionization of water in octanol. Hydrogen bonding and steric factors have a greater influence on ion pairs than they do on neutral species, yet these factors are missing from current programs used to calculate log P(I) and log D. In contrast to the common assumption that diff (log P(N - I)) is the same for all amines, they can actually vary more than 3 log units, as in our examples. A major factor affecting log P(I) is the ability of water and the counterion to approach the charge center. Bulky substituents near the charge center have a negative influence on log P(I). On the other hand, hydrogen bonding groups near the charge center have the opposite effect by lowering the free energy of the ion pair. The use of this titration method to determine substituent ion pair stabilization values (IPS) should bring about more accurate log D calculations and encourage species-specific QSAR involving log D(N) and log D(I). This work also brings attention to the fascinating world of nature's highly stabilized ion pairs.

  16. Phosphorus-doped and undoped glassy carbon indicator electrodes in controlled-current potentiometric titrations of bromide- or chloride-containing active ingredients in some pharmaceutical preparations.

    PubMed

    Abramović, Biljana F; Guzsvány, Valéria J; Gaál, Ferenc F

    2005-02-23

    Phosphorus-doped glassy carbon (as a novel material) and glassy carbon (Sigri commercial sample) were applied as potentiometric indicator electrodes in the titrimetric determination of active components with bromide or chloride in their molecules in different pharmaceutical preparations (Buscopan, Prostigmine, Isoptin, Bedoxin, Akineton and Trodon). After the necessary pre-treatment of the electrode surfaces and sample dissolution, the halide was titrated with a standard solution of silver nitrate (indirect determination). Amounts of 10-20 micromol of the investigated active ingredients per titration were determined with a relative standard deviation that, depending on the nature of indicator electrode, determined molecules and filler components, was in the range of 0.3-2.7%. The results obtained were compared with those of the official methods and with those obtained by potentiometric titrations using silver electrode. The titrimetric procedures developed are relatively fast, easy, economical and can be used to analyse of a large number of pharmaceutical products.

  17. Hydrogen bonding and molecular association in 2-(quinuclidinium)-butyric acid bromide hydrate studied by X-ray diffraction, DFT calculations, FTIR and NMR spectroscopy, and potentiometric titration

    NASA Astrophysics Data System (ADS)

    Dega-Szafran, Z.; Katrusiak, A.; Szafran, M.; Barczyński, P.

    2010-06-01

    The structure of 2-(quinuclidinium)-butyric acid bromide hydrate (QNBu·H 2O·HBr, 3) has been determined by X-ray diffraction, DFT calculations and characterized by FTIR and NMR spectroscopy. Crystals of 3 are monoclinic, space group P2 1. The water molecule interacts with the carboxylic group of 2-(quinuclidinium)-butyric acid and with the bromide anion by the COOH⋯OH 2 and HOH⋯Br hydrogen bonds of 2.575(3) and 3.293(2) Å, respectively. The structures of monomer ( 4) and dimeric cation ( 5) of the title complex have been optimized by the B3LYP/6-31G(d,p) approach, yielding conformations consistent with this in the crystal. The solid-state FTIR spectra of 3 and its deuterated analogue have been measured and compared with the theoretical spectrum of 4. The assignments of the observed and predicted bands have been proposed. The molecule of 3 has a chiral center at the C(9) atom, which is responsible for the non-magnetically equivalence of the α-ring and C(11)H 2 methylene protons in 1H NMR spectrum. The values of p Ka of quinuclidinium-acetate (quinuclidine betaine), 2-(quinuclidinium)-propionate and 2-(quinuclidinium)-butyrate have been determined by the potentiometric titration of their hydrohalides.

  18. The dissociation constants of the cytostatic bosutinib by nonlinear least-squares regression of multiwavelength spectrophotometric and potentiometric pH-titration data.

    PubMed

    Meloun, Milan; Nečasová, Veronika; Javůrek, Milan; Pekárek, Tomáš

    2016-02-20

    Potentiometric and spectrophotometric pH-titration of the multiprotic cytostatics bosutinib for dissociation constants determination were compared. Bosutinib treats patients with positive chronic myeloid leukemia. Bosutinib exhibits four protonatable sites in a pH range from 2 to 11, where two pK are well separated (ΔpK>3), while the other two are near dissociation constants. In the neutral medium, bosutinib occurs in the slightly water soluble form LH that can be protonated to the soluble cation LH4(3+). The molecule LH can be dissociated to still difficultly soluble anion L(-). The set of spectra upon pH from 2 to 11 in the 239.3-375.0nm was divided into two absorption bands: the first one from 239.3 to 290.5nm and the second from 312.3 to 375.0nm, which differ in sensitivity of chromophores to a pH change. Estimates of pK of the entire set of spectra were compared with those of both absorption bands. Due to limited solubility of bosutinib the protonation in a mixed aqueous-methanolic medium was studied. In low methanol content of 3-6% three dissociation constants can be reliably determined with SPECFIT/32 and SQUAD(84) and after extrapolation to zero content of methanol they lead to pKc1=3.43(12), pKc2=4.54(10), pKc3=7.56(07) and pKc4=11.04(05) at 25°C and pKc1=3.44(06), pKc2=5.03(08) pKc3=7.33(05) and pKc4=10.92(06) at 37°C. With an increasing content of methanol in solvent the dissociation of bosutinib is suppressed and the percentage of LH3(2+) decreases and LH prevails. From the potentiometric pH-titration at 25°C the concentration dissociation constants were estimated with ESAB pKc1=3.51(02), pKc2=4.37(02), pKc3=7.97(02) and pKc4=11.05(03) and with HYPERQUAD: pKc1=3.29(12), pKc2=4.24(10), pKc3=7.95(07) and pKc4=11.29(05).

  19. The dissociation constants of the cytostatic bosutinib by nonlinear least-squares regression of multiwavelength spectrophotometric and potentiometric pH-titration data.

    PubMed

    Meloun, Milan; Nečasová, Veronika; Javůrek, Milan; Pekárek, Tomáš

    2016-02-20

    Potentiometric and spectrophotometric pH-titration of the multiprotic cytostatics bosutinib for dissociation constants determination were compared. Bosutinib treats patients with positive chronic myeloid leukemia. Bosutinib exhibits four protonatable sites in a pH range from 2 to 11, where two pK are well separated (ΔpK>3), while the other two are near dissociation constants. In the neutral medium, bosutinib occurs in the slightly water soluble form LH that can be protonated to the soluble cation LH4(3+). The molecule LH can be dissociated to still difficultly soluble anion L(-). The set of spectra upon pH from 2 to 11 in the 239.3-375.0nm was divided into two absorption bands: the first one from 239.3 to 290.5nm and the second from 312.3 to 375.0nm, which differ in sensitivity of chromophores to a pH change. Estimates of pK of the entire set of spectra were compared with those of both absorption bands. Due to limited solubility of bosutinib the protonation in a mixed aqueous-methanolic medium was studied. In low methanol content of 3-6% three dissociation constants can be reliably determined with SPECFIT/32 and SQUAD(84) and after extrapolation to zero content of methanol they lead to pKc1=3.43(12), pKc2=4.54(10), pKc3=7.56(07) and pKc4=11.04(05) at 25°C and pKc1=3.44(06), pKc2=5.03(08) pKc3=7.33(05) and pKc4=10.92(06) at 37°C. With an increasing content of methanol in solvent the dissociation of bosutinib is suppressed and the percentage of LH3(2+) decreases and LH prevails. From the potentiometric pH-titration at 25°C the concentration dissociation constants were estimated with ESAB pKc1=3.51(02), pKc2=4.37(02), pKc3=7.97(02) and pKc4=11.05(03) and with HYPERQUAD: pKc1=3.29(12), pKc2=4.24(10), pKc3=7.95(07) and pKc4=11.29(05). PMID:26730513

  20. A combination of synchronous fluorescence spectroscopy with chemometric treatment and internal standards in non-aqueous potentiometric titrations of fulvic acids.

    PubMed

    Esteves da Silva, J C; Machado, A A

    1994-12-01

    The acid properties of a soil fulvic acid (sfua) were characterized by potentiometric titration with tetrabutylammonium hydroxide in two non-aqueous solvents with high acid-base resolution power N,N-dimethylformamide (DMF) and acetonitrile. Synchronous fluorescence spectroscopy (SyF) was also used to monitor directly the sfua status during the potentiometric titration in DMF. The potentiometric titration curves showed no clear end-point and the analysis of the sets of spectra obtained at increasing neutralization degree, with a self-modeling curve resolution method (SIMPLISMA), revealed the existence of two components with featureless concentration profiles. Internal standards (maleic, salicylic and p-hydroxylbenzoic acids) were used to determine the amounts of acid groups with different acid strengths in the two non-aqueous solvents. It was shown that the variations observed in the SyF spectra sets of the internal standards are not correlated with those observed in the sfua data. The splitting of the sfua groups in the non-aqueous titration curves seems to be forced artificially depending on the standards used.

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

    PubMed

    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. PMID

  2. Limitations of the potentiometric titration technique in determining the proton active site density of goethite surfaces

    NASA Astrophysics Data System (ADS)

    Lützenkirchen, Johannes; Boily, Jean-François; Lövgren, Lars; Sjöberg, Staffan

    2002-10-01

    Density of proton active surface sites at mineral surfaces is a property of fundamental importance in equilibrium modeling of surface complexation reactions. In this article, methods for an experimental determination of these sites at the surface of α-FeOOH (goethite) are explored. It is shown that previously obtained saturation data of goethite with respect to protons do not yield a site density that can be considered as an intrinsic sorbent property: the results are below crystallographically expected values and values for different ionic media in terms of composition and concentration yield different numbers - for example, chloride would yield higher values than nitrate at the same concentration, and higher electrolyte concentration would favor higher apparent maxima. Although site saturation might be explained by electrostatic repulsion, which is more efficient at high electrolyte concentration or for certain ions, further independent experimental results show that no saturation occurs on goethite down to ph ≡ -log[H +] = 2.2 and possibly to ph = 1.0 in 0.6 M NaCl. For those very low pH values, the experimental charging curve was obtained by coulometric back titration (using the Gran plot) or titrations with tris (hydroxymethyl)-aminomethane of the supernatant of acidified goethite suspension. These experimental data are to our knowledge the first high quality data at such low pHs. However, small errors in the determination of proton concentrations (1%) are shown to strongly affect the shape of the charging curve for ph < 2. Furthermore, goethite dissolution (proton consumption and iron reduction in coulometric titrations) and liquid junction effects interfere at low ph, hampering the straightforward application of coulometric Gran titrations over the whole pH range. From these experiments, it can nonetheless be ascertained that a minimum of 2.5 protons/nm 2 can be adsorbed at the goethite surface from the point of zero charge (ph 9.4) to pH 0.9. Although

  3. Analysis of potentiometric titrations of heterogeneous natural polyelectrolytes in terms of counterion condensation theory: application to humic acid.

    PubMed

    Porasso, R D; Benegas, J C; van den Hoop, M; Paoletti, S

    2000-07-31

    A model, developed within the framework of the counterion condensation theory of linear polyelectrolytes, is presented in this paper to describe the acid-base properties of linear polyelectrolytes, consisting of several types of functional ionizable groups. This formalism has been successfully applied to Fluka humic acid under salt-free conditions, as well as in the presence of supporting simple 1:1 salt (KNO3) at three different concentrations. As part of this approach, the charge density of the humic acid is obtained from the activity coefficient measurements of potassium counterions at different humic acid concentrations at a constant degree of dissociation of the polyelectrolyte. The humic acid average charge density was found to be 0.80 +/- 0.05. Using the present model, we are able to satisfactorily describe the experimental data obtained from acid-base potentiometric titrations. Four main functional groups making up the polymer are determined through their fractional abundances (Xi) and intrinsic pK (pK0i) values. The fractional abundances remained constant and independent of the ionic strength, indicating that the humic acid constitution does not depend on the concentration of excess salts. The pK0i values show a small change with ionic strength, which can be explained by the polyelectrolytic behavior of the solution.

  4. Predicting proton titration in cationic micelle and bilayer environments

    SciTech Connect

    Morrow, Brian H.; Shen, Jana K.; Eike, David M.; Murch, Bruce P.; Koenig, Peter H.

    2014-08-28

    Knowledge of the protonation behavior of pH-sensitive molecules in micelles and bilayers has significant implications in consumer product development and biomedical applications. However, the calculation of pK{sub a}’s in such environments proves challenging using traditional structure-based calculations. Here we apply all-atom constant pH molecular dynamics with explicit ions and titratable water to calculate the pK{sub a} of a fatty acid molecule in a micelle of dodecyl trimethylammonium chloride and liquid as well as gel-phase bilayers of diethyl ester dimethylammonium chloride. Interestingly, the pK{sub a} of the fatty acid in the gel bilayer is 5.4, 0.4 units lower than that in the analogous liquid bilayer or micelle, despite the fact that the protonated carboxylic group is significantly more desolvated in the gel bilayer. This work illustrates the capability of all-atom constant pH molecular dynamics in capturing the delicate balance in the free energies of desolvation and Coulombic interactions. It also shows the importance of the explicit treatment of ions in sampling the protonation states. The ability to model dynamics of pH-responsive substrates in a bilayer environment is useful for improving fabric care products as well as our understanding of the side effects of anti-inflammatory drugs.

  5. Predicting proton titration in cationic micelle and bilayer environments

    NASA Astrophysics Data System (ADS)

    Morrow, Brian H.; Eike, David M.; Murch, Bruce P.; Koenig, Peter H.; Shen, Jana K.

    2014-08-01

    Knowledge of the protonation behavior of pH-sensitive molecules in micelles and bilayers has significant implications in consumer product development and biomedical applications. However, the calculation of pKa's in such environments proves challenging using traditional structure-based calculations. Here we apply all-atom constant pH molecular dynamics with explicit ions and titratable water to calculate the pKa of a fatty acid molecule in a micelle of dodecyl trimethylammonium chloride and liquid as well as gel-phase bilayers of diethyl ester dimethylammonium chloride. Interestingly, the pKa of the fatty acid in the gel bilayer is 5.4, 0.4 units lower than that in the analogous liquid bilayer or micelle, despite the fact that the protonated carboxylic group is significantly more desolvated in the gel bilayer. This work illustrates the capability of all-atom constant pH molecular dynamics in capturing the delicate balance in the free energies of desolvation and Coulombic interactions. It also shows the importance of the explicit treatment of ions in sampling the protonation states. The ability to model dynamics of pH-responsive substrates in a bilayer environment is useful for improving fabric care products as well as our understanding of the side effects of anti-inflammatory drugs.

  6. Predicting proton titration in cationic micelle and bilayer environments

    PubMed Central

    Morrow, Brian H.; Eike, David M.; Murch, Bruce P.; Koenig, Peter H.; Shen, Jana K.

    2014-01-01

    Knowledge of the protonation behavior of pH-sensitive molecules in micelles and bilayers has significant implications in consumer product development and biomedical applications. However, the calculation of pKa’s in such environments proves challenging using traditional structure-based calculations. Here we apply all-atom constant pH molecular dynamics with explicit ions and titratable water to calculate the pKa of a fatty acid molecule in a micelle of dodecyl trimethylammonium chloride and liquid as well as gel-phase bilayers of diethyl ester dimethylammonium chloride. Interestingly, the pKa of the fatty acid in the gel bilayer is 5.4, 0.4 units lower than that in the analogous liquid bilayer or micelle, despite the fact that the protonated carboxylic group is significantly more desolvated in the gel bilayer. This work illustrates the capability of all-atom constant pH molecular dynamics in capturing the delicate balance in the free energies of desolvation and Coulombic interactions. It also shows the importance of the explicit treatment of ions in sampling the protonation states. The ability to model dynamics of pH-responsive substrates in a bilayer environment is useful for improving fabric care products as well as our understanding of the side effects of anti-inflammatory drugs. PMID:25173037

  7. Characterization of the cell surface and cell wall chemistry of drinking water bacteria by combining XPS, FTIR spectroscopy, modeling, and potentiometric titrations.

    PubMed

    Ojeda, Jesús J; Romero-Gonzalez, María E; Bachmann, Robert T; Edyvean, Robert G J; Banwart, Steven A

    2008-04-15

    Aquabacterium commune, a predominant member of European drinking water biofilms, was chosen as a model bacterium to study the role of functional groups on the cell surface that control the changes in the chemical cell surface properties in aqueous electrolyte solutions at different pH values. Cell surface properties of A. commune were examined by potentiometric titrations, modeling, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy. By combining FTIR data at different pH values and potentiometric titration data with thermodynamic model optimization, the presence, concentration, and changes of organic functional groups on the cell surface (e.g., carboxyl, phosphoryl, and amine groups) were inferred. The pH of zero proton charge, pH(zpc) = 3.7, found from titrations of A. commune at different electrolyte concentrations and resulting from equilibrium speciation calculations suggests that the net surface charge is negative at drinking water pH in the absence of other charge determining ions. In situ FTIR was used to describe and monitor chemical interactions between bacteria and liquid solutions at different pH in real time. XPS analysis was performed to quantify the elemental surface composition, to assess the local chemical environment of carbon and oxygen at the cell wall, and to calculate the overall concentrations of polysaccharides, peptides, and hydrocarbon compounds of the cell surface. Thermodynamic parameters for proton adsorption are compared with parameters for other gram-negative bacteria. This work shows how the combination of potentiometric titrations, modeling, XPS, and FTIR spectroscopy allows a more comprehensive characterization of bacterial cell surfaces and cell wall reactivity as the initial step to understand the fundamental mechanisms involved in bacterial adhesion to solid surfaces and transport in aqueous systems.

  8. Thermodynamics of cationic lipid-DNA complex formation as studied by isothermal titration calorimetry.

    PubMed Central

    Pozharski, Edwin; MacDonald, Robert C

    2002-01-01

    The detailed analysis of the cationic lipid-DNA complex formation by means of isothermal titration calorimetry is presented. Most experiments were done using 1,2-dioleyl-sn-glycero-3-ethylphosphocholine (EDOPC), but basic titrations were also done using DOTAP, DOTAP:DOPC, and DOTAP:DOPE mixtures. Complex formation was endothermic with less than 1 kcal absorbed per mole of lipid or DNA charge. This enthalpy change was attributed to DNA-DNA mutual repulsion within the lamellar complex. The exception was DOTAP:DOPE-containing lipoplex for which the enthalpy of formation was exothermic, presumably because of DOPE amine group protonation. Experimental conditions, namely, direction and titration increment as well as concentration of titrant, which dictate the structure of resulting lipoplex (whether lamellar complex or DNA-coated vesicle), were found to affect the apparent thermodynamics of complex formation. The structure, in turn, influences the biological properties of the lipoplex. If the titration of lipid into DNA was carried out in large increments, the DeltaH was larger than when the injection increments were smaller, a finding that is consistent with increased vesicle disruption under large increments and which is expected theoretically. Cationic lipid-DNA binding was weak in high ionic strength solutions, however, the effective binding constant is within micromolar range because of macromolecular nature of the interaction. PMID:12080142

  9. Diagrams of the formation of In2S3 and In2Se3 films on vitroceramic upon precipitation, according to potentiometric titration

    NASA Astrophysics Data System (ADS)

    Tulenin, S. S.; Bakhteev, S. A.; Yusupov, R. A.; Maskaeva, L. N.; Markov, V. F.

    2013-10-01

    Boundary conditions and ranges of the formation of indium(III) sulfide and selenide upon precipitation by thiocarbamide and selenocarbamide are determined. Potentiometric titration of indium chloride (InCl3) in the concentration range of 0.0001 to 0.100 mol/L by a solution of sodium hydroxide is performed. It is found that the following pH ranges are optimal for In2S3 and In2Se3 film precipitation: from 3.0 to 4.5 and from 9.0 to 14.0. Indium selenide layers 100 to 300 nm thick are prepared on vitroceramic by hydrochemcial precipitation.

  10. Synthesis, potentiometric titration, electrochemical investigation and biological properties of trans-[RuCl2(dinic)4] (dinic = 3,5-pyridinecarboxylic acid).

    PubMed

    Seifriz, I; Konzen, M; Paula, M M; Gonçalves, N S; Spoganickz, B; Creczynski-Pasa, T B; Bonetti, V R; Beirith, A; Calixto, J B; Franco, C V

    1999-09-30

    This work discusses both the synthesis of trans-[RuCl2(dinic)4], dinic = 3,5-pyridinecarboxylic acid, and its main characteristics including potentiometric titration, spectroscopic and electrochemical properties, and some biological properties. The complex was synthesized using ruthenium blue solution as the precursor in a synthetic route. The complex was characterized using electronic spectroscopy, vibrational FT-IR spectroscopy, and Raman spectroscopy, as well as 1H and 13C NMR. The results indicated that the complex exhibits a trans-geometry. Cyclic voltammetry carried out in water:acetone 1:1 solution revealed a quasi-reversible process centered on the Ru(II) atom, as well as a dependence of the redox potential, E1/2, on pH. An analysis of the electronic spectra revealed that the MLCT (metal ligand charge transfer) band underwent a hypsochromic shift as the pH increased. Spectroelectrochemical analysis indicated that the visible region band progressively faded out upon oxidation. The equilibrium constants for the eight protons of the complex were determined by potentiometric titration. The complex neither inhibits the activity of nitrogen monoxide synthase nor acts as a scavenger for nitrogen monoxide. Nevertheless, the complex shows antinociceptive properties and acts as a scavenger for hydroxyl radicals.

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

    PubMed

    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.

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

    PubMed

    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.

  13. New approach in the treatment of data from an acid-base potentiometric titrationI. Monocomponent systems of monofunctional acids and bases.

    PubMed

    Maslarska, Vania; Tencheva, Jasmina; Budevsky, Omortag

    2003-01-01

    Based on precise analysis of the acid-base equilibrium, a new approach in the treatment of experimental data from a potentiometric titration is proposed. A new general formula giving explicitly the relation V=f([H(+)]) is derived, valid for every acid-base titration, which includes mono- and polyfunctional protolytes and their mixtures. The present study is the first practical application of this formula for the simplest case, the analysis of one monofunctional protolyte. The collected mV data during the titration are converted into pH-values by means of an auto pH-calibration procedure, thus avoiding preliminary preparation of the measuring system. The mentioned pH-calibration method is applicable also in water-organic mixtures and allows the quantitative determination of sparingly soluble substances (particularly pharmaceuticals). The treatment of the data is performed by means of ready-to-use software products, which makes the proposed approach accessible for a wide range of applications.

  14. FIA titrations of phenothiazine derivatives in aqueous micellar and non-aqueous media.

    PubMed

    Nemcová, Irena; Nesmerák, Karel; Rychlovský, Petr; Koutníková, Jitka

    2005-02-15

    New methods of flow injection analysis (FIA) neutralization titrations of phenothiazine derivatives in aqueous micellar medium of a cationic surfactant using potentiometric and spectrophotometric detection were proposed; titrations with a mixing gradient chamber and high-speed titrations were compared. The FIA titration method in non-aqueous media based on an official method of determination (titration with perchloric acid in anhydrous acetic acid) was also developed. Under optimized reaction conditions and flow-through parameters, the calibration range and equations, the sensitivity, and the repeatability of all methods were found and discussed. All titrations were assayed for medicinal forms.

  15. Humic substance charge determination by titration with a flexible cationic polyelectrolyte

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

    The anionic charge of humic substances (HS) plays a major role in the interaction of HS with other components. Therefore, the potential of the polyelectrolyte titration technique to obtain the charge density of HS in simple 1-1 electrolyte solutions has been investigated. Titrations are carried out with an automatic titrator combined with the "Mütek particle charge detector" which allows determination of the Mütek potential and the pH as a function of the added amount of titrant which is a solution of poly-diallyldimethylammonium chloride (polyDADMAC), a cationic strong polyelectrolyte. When the Mütek potential reverses its sign the iso-electric point (IEP) of the polyDADMAC-HS complex is reached. The polyDADMAC/HS mass ratio at the IEP gives information on the HS charge density and from the pH changes in solution an estimate of the charge regulation in the HS-polyDADMAC complex can be obtained. In general, for polyDADMAC-HS complexes an increase in the dissociation of the acid groups of HS is found (charge regulation). The charge regulation decreases with increasing concentration of 1-1 background electrolyte. Cation incorporation can be neglected at 1-1 electrolyte concentrations ⩽ 1 mmol L -1 and a 1-1 stoichiometry exists between the polyDADMAC and HS charge. However, at these low salt concentrations the charge regulation is substantial. A detailed analysis of purified Aldrich humic acid (PAHA) at pH 5 and a range of KCl concentrations reveals that the anionic charge of PAHA in the complex increases at 5 mmol L -1 KCl by 30% and at 150 mmol L -1 KCl by 12%. On the other hand, increasing amounts of K + become incorporated in the complex: at 5 mmol L -1 KCl 5% and at 150 mmol L -1 KCl 24% of the PAHA charge is balanced by K +. By comparing at pH 5 the mass ratios polyDADMAC/PAHA in the complex at the IEP with the theoretical mass ratios of polyDADMAC/PAHA required to neutralize PAHA in the absence of charge regulation and K + incorporation, it is found that

  16. Improved methylene blue two-phase titration method for determining cationic surfactant concentration in high-salinity brine.

    PubMed

    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.

  17. Potentiometric determination of potassium cations using a nickel(II) hexacyanoferrate-modified electrode.

    PubMed

    Mortimer, R J; Barbeira, P J; Sene, A F; Stradiotto, N R

    1999-06-14

    Electroactive nickel(II) hexacyanoferrate (NiHCF) thin film modified electrodes are effective potentiometric sensors for the determination of potassium ions. The NiHCF films are deposited onto glassy carbon electrodes by repetitive potential cycling in K(3)Fe(CN)(6)/NaNO(3)/Ni(NO(3))(2) solution. The modified electrodes exhibit a linear response to potassium ions in the concentration range 1x10(-3) to 2.0 mol dm(-3), with a near-Nernstian slope (45-49 mV per decade) at 25 degrees C. In the determination of potassium ion in syrups used for treatment of potassium deficiency, the NiHCF-modified electrode gave comparable results to those obtained using flame emission spectrophotometry. PMID:18967597

  18. Theoretical study of the acid-base properties of the montmorillonite/electrolyte interface: influence of the surface heterogeneity and ionic strength on the potentiometric titration curves.

    PubMed

    Zarzycki, Piotr; Thomas, Fabien

    2006-10-15

    The parallel shape of the potentiometric titration curves for montmorillonite suspension is explained using the surface complexation model and taking into account the surface heterogeneity. The homogeneous models give accurate predictions only if they assume unphysically large values of the equilibrium constants for the exchange process occurring on the basal plane. However, the assumption that the basal plane is energetically heterogeneous allows to fit the experimental data (reported by Avena and De Pauli [M. Avena, C.P. De Pauli, J. Colloid Interface Sci. 202 (1998) 195-204]) for reasonable values of exchange equilibrium constant equal to 1.26 (suggested by Fletcher and Sposito [P. Fletcher, G. Sposito, Clay Miner. 24 (1989) 375-391]). Moreover, we observed the typical behavior of point of zero net proton charge (pznpc) as a function of logarithm of the electrolyte concentration (log[C]). We showed that the slope of the linear dependence, pznpc=f(log[C]), is proportional to the number of isomorphic substitutions in the crystal phase, which was also observed in the experimental studies.

  19. Copper redox transformation and complexation by reduced and oxidized soil humic Acid. 2. Potentiometric titrations and dialysis cell experiments.

    PubMed

    Maurer, Felix; Christl, Iso; Fulda, Beate; Voegelin, Andreas; Kretzschmar, Ruben

    2013-10-01

    Cation binding and electron transfer reactions of humic substances determine copper speciation in redox-dynamic systems, but quantitative studies for Cu+ binding to humic substances are lacking. We investigated reduction of Cu2+ and binding of Cu+ at pH 7.0 in a dialysis cell experiment using reduced and reoxidized soil humic acid (HA) as reductant and sorbent at copper loadings of 9.5-600 mmol kg(-1). The data were used to quantitatively explain the interaction between cation binding and electron transfer processes that determine copper speciation in the presence of HA under anoxic and oxic conditions. Addition of Cu2+ to reduced HA resulted in almost complete reduction to Cu(I) within 1 h. Reduction was also significant under oxic conditions. The slow decrease of the Cu(I) fraction was attributed to formation of Cu(0) based on thermodynamic consideration. Cu+ binding to HA was found to be strong compared to other chalcophile cations like Ag+ or Cd2+. Our results indicate that Cu+ and Cu2+ isotherms exhibit a redox potential-dependent intersection point. According to the differences in Cu+ and Cu2+ binding, the presence of HA was found to extend the stability field of Cu(II) to moderately reducing conditions and to reduce the stability field of Cu(0) due to the formation of Cu(I) complexes.

  20. Potentiometric sensors for the selective determination of sulbutiamine.

    PubMed

    Ahmed, M A; Elbeshlawy, M M

    1999-11-01

    Five novel polyvinyl chloride (PVC) matrix membrane sensors for the selective determination of sulbutiamine (SBA) cation are described. These sensors are based on molybdate, tetraphenylborate, reineckate, phosphotun gestate and phosphomolybdate, as possible ion-pairing agents. These sensors display rapid near-Nernstian stable response over a relatively wide concentration range 1x10(-2)-1x10(-6) M of sulbutiamine, with calibration slopes 28 32.6 mV decade(-1) over a reasonable pH range 2-6. The proposed sensors proved to have a good selectivity for SBA over some inorganic and organic cations. The five potentiometric sensors were applied successfully in the determination of SBA in a pharmaceutical preparation (arcalion-200) using both direct potentiometry and potentiometric titration. Direct potentiometric determination of microgram quantities of SBA gave average recoveries of 99.4 and 99.3 with mean standard deviation of 0.7 and 0.3 for pure SBA and arcalion-200 formulation respectively. Potentiometric titration of milligram quantities of SBA gave average recoveries of 99.3 and 98.7% with mean standard deviation of 0.7 and 1.2 for pure SBA and arcalion-200 formulation, respectively. PMID:10703998

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

    PubMed

    Söderman, Olle; Jönsson, Bengt; Olofsson, Gerd

    2006-02-23

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

  2. Dysprosium selective potentiometric membrane sensor.

    PubMed

    Zamani, Hassan Ali; Faridbod, Farnoush; Ganjali, Mohammad Reza

    2013-03-01

    A novel Dy(III) ion-selective PVC membrane sensor was made using a new synthesized organic compound, 3,4-diamino-N'-((pyridin-2-yl)methylene)benzohydrazide (L) as an excellent sensing element. The electrode showed a Nernstian slope of 19.8 ± 0.6 mV per decade in a wide concentration range of 1.0 × 10(-6)-1.0 × 10(-2) mol L(-1), a detection limit of 5.5 × 10(-7) mol L(-1), a short conditioning time, a fast response time (<10s), and high selectivity towards Dy(III) ion in contrast to other cations. The proposed sensor was successfully used as an indicator electrode in the potentiometric titration of Dy(III) ions with EDTA. The membrane sensor was also applied to the F(-) ion indirect determination of some mouth washing solutions and to the Dy(3+) determination in binary mixtures.

  3. Simultaneous Analysis of Monovalent Anions and Cations with a Sub-Microliter Dead-Volume Flow-Through Potentiometric Detector for Ion Chromatography.

    PubMed

    Dumanli, Rukiye; Attar, Azade; Erci, Vildan; Isildak, Ibrahim

    2016-04-01

    A microliter dead-volume flow-through cell as a potentiometric detector is described in this article for sensitive, selective and simultaneous detection of common monovalent anions and cations in single column ion chromatography for the first time. The detection cell consisted of less selective anion- and cation-selective composite membrane electrodes together with a solid-state composite matrix reference electrode. The simultaneous separation and sensitive detection of sodium (Na(+)), potassium (K(+)), ammonium (NH4 (+)), chloride (Cl(-)) and nitrate (NO3 (-)) in a single run was achieved by using 98% 1.5 mM MgSO4 and 2% acetonitrile eluent with a mixed-bed ion-exchange separation column without suppressor column system. The separation and simultaneous detection of the anions and cations were completed in 6 min at the eluent flow-rate of 0.8 mL/min. Detection limits, at S/N = 3, were ranged from 0.2 to 1.0 µM for the anions and 0.3 to 3.0 µM for the cations, respectively. The developed method was successfully applied to the simultaneous determination of monovalent anions and cations in several environmental and biological samples.

  4. Simultaneous Analysis of Monovalent Anions and Cations with a Sub-Microliter Dead-Volume Flow-Through Potentiometric Detector for Ion Chromatography.

    PubMed

    Dumanli, Rukiye; Attar, Azade; Erci, Vildan; Isildak, Ibrahim

    2016-04-01

    A microliter dead-volume flow-through cell as a potentiometric detector is described in this article for sensitive, selective and simultaneous detection of common monovalent anions and cations in single column ion chromatography for the first time. The detection cell consisted of less selective anion- and cation-selective composite membrane electrodes together with a solid-state composite matrix reference electrode. The simultaneous separation and sensitive detection of sodium (Na(+)), potassium (K(+)), ammonium (NH4 (+)), chloride (Cl(-)) and nitrate (NO3 (-)) in a single run was achieved by using 98% 1.5 mM MgSO4 and 2% acetonitrile eluent with a mixed-bed ion-exchange separation column without suppressor column system. The separation and simultaneous detection of the anions and cations were completed in 6 min at the eluent flow-rate of 0.8 mL/min. Detection limits, at S/N = 3, were ranged from 0.2 to 1.0 µM for the anions and 0.3 to 3.0 µM for the cations, respectively. The developed method was successfully applied to the simultaneous determination of monovalent anions and cations in several environmental and biological samples. PMID:26786906

  5. Rapid determination of the equivalence volume in potentiometric acid-base titrations to a preset pH-I Theory and applications.

    PubMed

    Ivaska, A

    1974-06-01

    A new approach to shorten the time needed for an acid-base titration has been made. The method developed is based on the equation for acid-base titrations derived by Ingman and Still. The equation is transformed into such a form that only one titration point is needed to calculate the equivalence volume when the titration is carried out to a preset pH which can be chosen according to the experimental conditions. The method is used for titration of acetic acid, log K(H)(HA) = 4.65, hydroxylammonium ion, log K(H)(HA) approximately 6.2, and boric acid, log K(H)(HA) approximately 9.1, with an error of 0.1-0.5%. In titration of hydrogen ascorbate ion, log K(H)(HA) approximately 11.3, the error obtained was about 0.3-2%.

  6. A new oxidimetric reagent: potassium dichromate in a strong phosphoric acid medium-VI Potentiometric titration of vanadium(III) alone and in mixture with vanadium(IV).

    PubMed

    Rao, G G; Rao, P K

    1966-09-01

    Vanadium(III) can be titrated at room temperature with potassium dichromate in an 8-12M phosphoric acid medium. Two potential breaks are observed in 12M phosphoric add with 0.2N potassium dichromate, the first corresponding to the oxidation of vanadium(III) to vanadium(IV) and the second to the oxidation of vanadium(IV) to vanadium(V). In titrations with 0.05N dichromate only the first break in potential is clearly observed. The method has been extended to the titration of mixtures of vanadium(III) and vanadium(IV). Conditions have also been found for the visual titration of vanadium(III) using ferroln or barium diphenylamine sulphonate as indicator.

  7. Acid-base properties of humic substances from composted and thermally-dried sewage sludges and amended soils as determined by potentiometric titration and the NICA-Donnan model.

    PubMed

    Fernández, José M; Plaza, César; Senesi, Nicola; Polo, Alfredo

    2007-09-01

    The acid-base properties of humic acids (HAs) and fulvic acids (FAs) isolated from composted sewage sludge (CS), thermally-dried sewage sludge (TS), soils amended with either CS or TS at a rate of 80 t ha(-1)y(-1) for 3y and the corresponding unamended soil were investigated by use of potentiometric titrations. The non-ideal competitive adsorption (NICA)-Donnan model for a bimodal distribution of proton binding sites was fitted to titration data by use of a least-squares minimization method. The main fitting parameters of the NICA-Donnan model obtained for each HA and FA sample included site densities, median affinity constants and widths of affinity distributions for proton binding to low and high affinity sites, which were assumed to be, respectively, carboxylic- and phenolic-type groups. With respect to unamended soil HA and FA, the HAs and FAs from CS, and especially TS, were characterized by smaller acidic functional group contents, larger proton binding affinities of both carboxylic- and phenolic-type groups, and smaller heterogeneity of carboxylic and phenolic-type groups. Amendment with CS or TS led to a decrease of acidic functional group contents and a slight increase of proton binding affinities of carboxylic- and phenolic-type groups of soil HAs and FAs. These effects were more evident in the HA and FA fractions from CS-amended soil than in those from TS-amended soil.

  8. Determination of total fluoride in HF/HNO3/H2SiF6 etch solutions by new potentiometric titration methods.

    PubMed

    Weinreich, Wenke; Acker, Jörg; Gräber, Iris

    2007-03-30

    In the photovoltaic industry the etching of silicon in HF/HNO(3) solutions is a decisive process for cleaning wafer surfaces or to produce certain surface morphologies like polishing or texturization. With regard to cost efficiency, a maximal utilisation of etch baths in combination with highest quality and accuracy is strived. To provide an etch bath control realised by a replenishment with concentrated acids the main constituents of these HF/HNO(3) etch solutions including the reaction product H(2)SiF(6) have to be analysed. Two new methods for the determination of the total fluoride content in an acidic etch solution based on the precipitation titration with La(NO(3))(3) are presented within this paper. The first method bases on the proper choice of the reaction conditions, since free fluoride ions have to be liberated from HF and H(2)SiF(6) at the same time to be detected by a fluoride ion-selective electrode (F-ISE). Therefore, the sample is adjusted to a pH of 8 for total cleavage of the SiF(6)(2-) anion and titrated in absence of buffers. In a second method, the titration with La(NO(3))(3) is followed by a change of the pH-value using a HF resistant glass-electrode. Both methods provide consistent values, whereas the analysis is fast and accurate, and thus, applicable for industrial process control. PMID:19071540

  9. Acid-base titrations by stepwise addition of equal volumes of titrant with special reference to automatic titrations-IV Photometric titration of an acid.

    PubMed

    Pehrsson, L; Ingman, F

    1977-02-01

    In Part I of this series, evaluation methods for potentiometric titrations of acids performed by stepwise addition of titrant were introduced. These methods are non-approximative and may therefore in principle be applied to titrations of acids of any strength. This paper demonstrates that photometric titrations performed by stepwise addition of titrant may also be evaluated by the proposed methods. The photometric method is compared with the potentiometric method of monitoring the course of a titration.

  10. Determination of Chloride in Infant Formula and Adult/Pediatric Nutritional Formula by Potentiometric Titration: Single-Laboratory Validation, First Action 2015.07.

    PubMed

    Bolong, Wu; Fengxia, Zhang; Xiaoning, Ma; Fengjuan, Zhou; Brunelle, Sharon L

    2016-01-01

    A potentiometric method for determination of chloride was validated against AOAC Standard Method Performance Requirement (SMPR(®)) 2014.015. Ten AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) matrixes, including National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 1849a, were tested in duplicate on 6 independent days. The repeatability (RSDr) ranged from 0.43 to 1.34%, and the intermediate reproducibility (RSDiR) ranged from 0.80 to 3.04%. All results for NIST SRM 1849a were within the range of the certified concentration (701 ± 17 mg/100 g). Recovery was demonstrated with two overspike levels, 50 and 100%, in the 10 SPIFAN matrixes. Samples were tested in duplicate on 3 different days, and all results were within the SMPR requirement of 95 to 105%. The LOQs of the method for powdered products and ready-to-feed or reconstituted products were 20 mg/100 g and 2.2 mg/100 mL, respectively. A wide analytical range from the LOQ to 99.5% chlorine content can be reached with an appropriate dilution factor, but in practice, the upper analytical value observed in routine matrix testing was approximately 1080 mg/100 g in skim milk powder. This is a rapid, simple, and reliable chlorine-testing method applicable to infant formula, adult nutritionals, and ingredients used in these dairy-based products, such as skim milk powder, desalted whey powder, whey protein powder, and whole milk powder. PMID:26822885

  11. Going Beyond, Going Further: Knives, Forks, and Beer Cans as Potentiometric Sensors.

    ERIC Educational Resources Information Center

    Selig, Walter S.

    1985-01-01

    Background information, materials needed, and procedures used are provided for potentiometric fluoride, halide, orthophosphate, and sulfate titrations. Typical results obtained are also provided for each type of titration. (JN)

  12. Digital image-based titrations.

    PubMed

    Gaiao, Edvaldo da Nobrega; Martins, Valdomiro Lacerda; Lyra, Wellington da Silva; de Almeida, Luciano Farias; da Silva, Edvan Cirino; Araújo, Mário César Ugulino

    2006-06-16

    The exploitation of digital images obtained from a CCD camera (WebCam) as a novel instrumental detection technique for titration is proposed for the first time. Named of digital image-based (DIB) titration, it also requires, as a traditional titration (for example, spectrophotometric, potentiometric, conductimetric), a discontinuity in titration curves where there is an end point, which is associated to the chemical equivalence condition. The monitored signal in the DIB titration is a RGB-based value that is calculated, for each digital image, by using a proposed procedure based on the red, green, and blue colour system. The DIB titration was applied to determine HCl and H3PO4 in aqueous solutions and total alkalinity in mineral and tap waters. Its results were compared to the spectrophotometric (SPEC) titration and, by applying the paired t-test, no statistic difference between the results of both methods was verified at the 95% confidence level. Identical standard deviations were obtained by both titrations in the determinations of HCl and H3PO4, with a slightly better precision for DIB titration in the determinations of total alkalinity. The DIB titration shows to be an efficient and promising tool for quantitative chemical analysis and, as it employs an inexpensive device (WebCam) as analytical detector, it offers an economically viable alternative to titrations that need instrumental detection.

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

    PubMed

    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.

  14. Interaction of cationic dodecyl-trimethyl-ammonium bromide with oxy-HbGp by isothermal titration and differential scanning calorimetric studies: Effect of proximity of isoelectric point.

    PubMed

    Alves, Fernanda Rosa; Carvalho, Francisco Adriano O; Carvalho, José Wilson P; Tabak, Marcel

    2016-04-01

    In this work, isothermal titration and differential scanning calorimetric methods, in combination with pyrene fluorescence emission and dynamic light scattering have been used to investigate the interaction of dodecyltrimethylammonium bromide (DTAB) with the giant extracellular Glossoscolex paulistus hemoglobin (HbGp) in the oxy-form, at pH values around the isoelectric point (pI ≈ 5.5). Our ITC results have shown that the interaction of DTAB with the hemoglobin is more intense at pH 7.0, with a smaller cac (critical aggregation concentration) value. The increase of protein concentration does not influence the cac value of the interaction, at both pH values. Therefore, the beginning of the DTAB-oxy-HbGp premicellar aggregates formation, in the cac region, is not affected by the increase of protein concentration. HSDSC studies show higher Tm values at pH 5.0, in the absence and presence of DTAB, when compared with pH 7.0. Furthermore, at pH 7.0, an aggregation process is observed with DTAB in the range from 0.75 to 1.5 mmol/L, noticed by the exothermic peak, and similar to that observed for pure oxy-HbGp, at pH 5.0, and in the presence of DTAB. DLS melting curves show a decrease on the hemoglobin thermal stability for the oxy-HbGp-DTAB mixtures and formation of larger aggregates, at pH 7.0. Our present data, together with previous results, support the observation that the protein structural changes, at pH 7.0, occur at smaller DTAB concentrations, as compared with pH 5.0, due to the acidic pI of protein that favors the oxy-HbGp-cationic surfactant interaction at neutral pH.

  15. A hot-cell titration system

    SciTech Connect

    Klatt, L.N.

    1988-07-01

    Operation of nuclear fuel reprocessing plant requires an analytical support laboratory capable of meeting the process control, product quality, and nuclear safeguard requirements. Because of the radioactivity accompanying many of the samples, the analytical instruments must be selected, modified, or specifically developed for use in hot cells. Titrimetric procedures have been successfully used in hot cells and are generally immune to radiation induced bias. This report describes a titration system designed for operation in a hot-cell environment. The potentiometric titration system has operated successfully for four years in support of nuclear fuel reprocessing research and development activities. Details of the hardware, electronic, and software control and data analysis systems are presented. Interchangeable burets with a capacity of 5, 10, and 25 mL are available; the means of the absolute error in delivered volume for these burets are 0.9, 1.1, and 1.8 ..mu..L, respectively. Results of evaluation studies how that the accuracy and precision of analysis results obtained with the potentiometric system are limited by statistical uncertainties associated with the standard titrant, sample preparation procedure, and the equilibrium constant of the titration reaction and not by titrator performance factors. The system is also capable of performing amperometric titrations. Changing between the potentiometric and amperometric modes of operation involves changing the in-cell transducers, the in-cell electronics, and the titrator control program. 22 refs., 13 figs., 9 tabs.

  16. Cation-binding Capacity of Membranes Isolated from Micrococcus lysodeikticus

    PubMed Central

    Cutinelli, C.; Galdiero, F.; Tufano, M. A.

    1969-01-01

    A study was made of H+, Na+, K+, Ca++, and Mg++ binding and ion-exchange properties of the plasma-mesosome membrane system isolated from Micrococcus lysodeikticus strain NCTC 2665. Titration curves were obtained on membranes prepared according to the method of M. R. J. Salton and further exposed to pH 4 for 4 hr (membranes-H). The dissociation coefficients and binding capacities were obtained by applying the mass law equation and the plot of G. Schatchard to the data. The membranes-H possess four kinds of dissociable groups with pK 4.96, 4.18, 3.60, and 3.09, respectively, and a total binding capacity of 0.65 meq/g (dry weight). Potentiometric titrations of cations in the presence and in the absence of membranes-H show that cations (Na+, K+, Ca++, and Mg++) are bound by the dissociated groups of the membrane. The fall in pH value for bivalent cations is greater than that for monovalent cations. Cations of the same valency produce equal diminutions on pH. Furthermore, ion-exchange tests carried out on membranes saturated with Mg++ or Na+ and suspended in a medium containing 45Ca show that the cations are reversibly bound. PMID:5344091

  17. Studies on the complexation of Pr(III) and Nd(III) with glycyl-glycine (gly-gly) using spectral analysis of 4f-4f transitions and potentiometric titrations.

    PubMed

    Ranjana Devi, N; Huidrom, Bimola; Rajmuhon Singh, N

    2012-10-01

    The interaction of gly-gly with Pr(III) and Nd(III) have been studied in different aquated organic solvents like CH(3)OH, CH(3)CN, dioxane and DMF by using 4f-4f transitions spectra. Various energy interaction parameters like Slater Condon (F(k)), Racah (E(k)), Lande (ξ(4f)), nephelauxetic effect (β), bonding (b(1/2)) and percent covalency (δ) parameters have been calculated to explain the nature of complexation. The intensity parameters like oscillator strength (P) and Judd-Ofelt parameters (T(λ), λ=2, 4, 6) also support the mode of binding of gly-gly to metal ions. The results show that Pr(III) and Nd(III) with gly-gly form complexes by ionic linkages with carboxylate anion with weak covalency. The protonation constants and metal-ligand stability constants have also been determined by potentiometric measurements in aqueous medium at different temperatures (290, 300 and 310 K) at constant ionic strength, 0.1 mol dm(-1). The results show the formation of metal-ligand complexes in the stoichiometric ratio 1:1. The stability of complexes is more in Nd(III) complexes as compared to Pr(III) complexes. Thermodynamic parameters (ΔG, ΔH and ΔS) of complexes were also calculated and the negative values of ΔG and ΔH show that the complex reactions are spontaneous and exothermic. The positive values of ΔS indicate high stability of complex reactions which are enthalpy-driven.

  18. Studies on the complexation of Pr(III) and Nd(III) with glycyl-glycine (gly-gly) using spectral analysis of 4f-4f transitions and potentiometric titrations

    NASA Astrophysics Data System (ADS)

    Ranjana Devi, N.; Huidrom, Bimola; Rajmuhon Singh, N.

    2012-10-01

    The interaction of gly-gly with Pr(III) and Nd(III) have been studied in different aquated organic solvents like CH3OH, CH3CN, dioxane and DMF by using 4f-4f transitions spectra. Various energy interaction parameters like Slater Condon (Fk), Racah (Ek), Lande (ξ4f), nephelauxetic effect (β), bonding (b1/2) and percent covalency (δ) parameters have been calculated to explain the nature of complexation. The intensity parameters like oscillator strength (P) and Judd-Ofelt parameters (Tλ, λ = 2, 4, 6) also support the mode of binding of gly-gly to metal ions. The results show that Pr(III) and Nd(III) with gly-gly form complexes by ionic linkages with carboxylate anion with weak covalency. The protonation constants and metal-ligand stability constants have also been determined by potentiometric measurements in aqueous medium at different temperatures (290, 300 and 310 K) at constant ionic strength, 0.1 mol dm-1. The results show the formation of metal-ligand complexes in the stoichiometric ratio 1:1. The stability of complexes is more in Nd(III) complexes as compared to Pr(III) complexes. Thermodynamic parameters (ΔG, ΔH and ΔS) of complexes were also calculated and the negative values of ΔG and ΔH show that the complex reactions are spontaneous and exothermic. The positive values of ΔS indicate high stability of complex reactions which are enthalpy-driven.

  19. Rapid determination of the equivalence volume in potentiometric acid-base titrations to a preset pH-II Standardizing a solution of a strong base, graphic location of equivalence volume, determination of stability constants of acids and titration of a mixture of two weak acids.

    PubMed

    Ivaska, A

    1974-06-01

    A newly proposed method of titrating weak acids with strong bases is applied to standardize a solution of a strong base, to graphic determination of equivalence volume of acetic acid with an error of 0.2%, to calculate the stability constants of hydroxylammonium ion, boric acid and hydrogen ascorbate ion and to analyse a mixture of acetic acid and ammonium ion with an error of 0.2-0.7%.

  20. Microscale Titration in Schools Titration Competition.

    ERIC Educational Resources Information Center

    Clark, Michael J.

    1998-01-01

    Reviews the requirements of the National Titration Competition and describes how a team in a local competition used the technique. Compares microscale titration to conventional titration. Outlines the benefits of employing microscale techniques. (DDR)

  1. Titanium (III) cation selective electrode based on synthesized tris(2pyridyl) methylamine ionophore and its application in water samples

    NASA Astrophysics Data System (ADS)

    Rezayi, Majid; Karazhian, Reza; Abdollahi, Yadollah; Narimani, Leila; Sany, Seyedeh Belin Tavakoly; Ahmadzadeh, Saeid; Alias, Yatimah

    2014-04-01

    The introduction of low detection limit ion selective electrodes (ISEs) may well pave the way for the determination of trace targets of cationic compounds. This research focuses on the detection of titanium (III) cation using a new PVC-membrane sensor based on synthesized tris(2pyridyl) methylamine (tpm) ionophore. The application and validation of the proposed sensor was done using potentiometric titration, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS). The membrane sensor exhibited a Nernstian response to the titanium (III) cation over a concentration range of 1.0 × 10-6-1.0 × 10-2 M and pH range from 1-2.5. The Nernstian slope, the lower of detection (LOD), and the response time (t95%) of the proposed sensor were 29.17 +/- 0.24 mV/dec, 7.9 × 10-7 M, and 20 s, respectively. The direct determination of 4-39 μg/ml of titanium (III) standard solution showed an average recovery of 94.60 and a mean relative standard deviation of 1.8 at 100.0 μg/ml. Finally, the utilization of the electrodes as end-point indicators for potentiometric titration with EDTA solutions for titanium (III) sensor was successfully carried out.

  2. Titanium (III) cation selective electrode based on synthesized tris(2pyridyl) methylamine ionophore and its application in water samples

    PubMed Central

    Rezayi, Majid; Karazhian, Reza; Abdollahi, Yadollah; Narimani, Leila; Sany, Seyedeh Belin Tavakoly; Ahmadzadeh, Saeid; Alias, Yatimah

    2014-01-01

    The introduction of low detection limit ion selective electrodes (ISEs) may well pave the way for the determination of trace targets of cationic compounds. This research focuses on the detection of titanium (III) cation using a new PVC-membrane sensor based on synthesized tris(2pyridyl) methylamine (tpm) ionophore. The application and validation of the proposed sensor was done using potentiometric titration, inductively coupled plasma atomic emission spectrometry (ICP-AES), and atomic absorption spectrometry (AAS). The membrane sensor exhibited a Nernstian response to the titanium (III) cation over a concentration range of 1.0 × 10−6–1.0 × 10−2 M and pH range from 1–2.5. The Nernstian slope, the lower of detection (LOD), and the response time (t95%) of the proposed sensor were 29.17 ± 0.24 mV/dec, 7.9 × 10−7 M, and 20 s, respectively. The direct determination of 4–39 μg/ml of titanium (III) standard solution showed an average recovery of 94.60 and a mean relative standard deviation of 1.8 at 100.0 μg/ml. Finally, the utilization of the electrodes as end-point indicators for potentiometric titration with EDTA solutions for titanium (III) sensor was successfully carried out. PMID:24722576

  3. Interactions of phenol with cationic micelles of hexadecyltrimethylammonium bromide studied by titration calorimetry, conductimetry, and 1H NMR in the range of low additive and surfactant concentrations.

    PubMed

    Chaghi, Radhouane; de Ménorval, Louis-Charles; Charnay, Clarence; Derrien, Gaëlle; Zajac, Jerzy

    2008-10-01

    Interactions of phenol (PhOH) with micellar aggregates of hexadecyltrimethylammonium bromide (HTAB) in aqueous solutions at surfactant concentrations close to the CMC and phenol contents of 1, 5, or 10 mmol kg(-1) have been investigated at 303 K by means of titration calorimetry, solution conductimetry, and (1)H NMR spectroscopy. Estimates of the main thermodynamic parameters related to HTAB micellization were made for PhOH/HTAB/H(2)O systems based on the specific conductivity measurements and calorimetric determination of the cumulative enthalpy of dilution as functions of the surfactant concentration at a fixed additive content. The combined analysis of the results obtained in H(2)O solutions pointed to the preferential location of PhOH in the outer micelle parts by an enthalpy-driven mechanism. Additional PhOH molecules were located increasingly deeper within the micelle core. The (1)H NMR study of PhOH solubilization by 1.5 mmol kg(-1) HTAB solutions in D(2)O indicated that the two categories of the solubilization site became saturated with the solubilizate already at the lowest additive content. Dissimilar amounts of the solubilized material in H(2)O and D(2)O solutions were ascribed to the difference in the initial micelle structures formed in the two solvents, as inferred from calorimetry and (1)H NMR studies of the HTAB micellization in D(2)O and H(2)O.

  4. Modern Directions for Potentiometric Sensors

    PubMed Central

    Bakker, Eric; Chumbimuni-Torres, Karin

    2009-01-01

    This paper gives an overview of the newest developments of polymeric membrane ion-selective electrodes. A short essence of the underlying theory is given, emphasizing how the electromotive force may be used to assess binding constants of the ionophore, and how the selectivity and detection limit are related to the underlying membrane processes. The recent developments in lowering the detection limits of ISEs are described, including recent approaches of developing all solid state ISEs, and breakthroughs in detecting ultra-small quantities of ions at low concentrations. These developments have paved the way to use potentiometric sensors as in ultra-sensitive affinity bioanalysis in conjunction with nanoparticle labels. Recent results establish that potentiometry compares favorably to electrochemical stripping analysis. Other new developments with ion-selective electrodes are also described, including the concept of backside calibration potentiometry, controlled current coulometry, pulsed chronopotentiometry, and localized flash titration with ion-selective membranes to design sensors for the direct detection of total acidity without net sample perturbation. These developments have further opened the field for exciting new possibilities and applications. PMID:19890473

  5. Permian potentiometric analysis

    SciTech Connect

    Devary, J.L.

    1983-09-01

    Pacific Northwest Laboratory (PNL) was requested to analyze potentiometric data from the Wolfcamp Formation of the Permian System to evaluate the recommendations by the University of Texas/Bureau of Economic Geology (UT/BEG) that additional geohydrologic boreholes be drilled into the Wolfcamp. The UT/BEG recommended that two stratigraphic and two geohydrologic borings be drilled into the Permian System during FY83 and that several shallow hydrologic tests be made in the Dockum Formation. A geostatistical technique known as kriging was applied to objectively evaluate these geohydrologic borehole recommendations. The Deaf Smith County location appears to be an excellent choice for a borehole. No high quality potentiometric data are available from Deaf Smith County and a borehole location immediately upgradient from the candidate repository site is needed. Adding this borehole location to the potentiometric data base will significantly reduce field data uncertainty near the location being studied. The Swisher County location does not appear to be the best choice. High quality data values H2206 and H2360 are located immediately upgradient from the proposed repository site. The best placement of additional geohydrological boreholes in the Wolfcamp Formation depends strongly upon the proposed repository location. The variability of the potentiometric data causes estimation errors to rapidly increase away from locations of field measurements. Suggested locations for additional boreholes for the Deaf Smith investigations are in northwest Randall or central Potter Counties. Ideal borehole locations for the Swisher county studies appear to be in southeast Randall and Armstrong Counties.

  6. A comparison of computer methods for seawater alkalinity titrations

    NASA Astrophysics Data System (ADS)

    Barron, J. L.; Dyrssen, D.; Jones, E. P.; Wedborg, M.

    1983-04-01

    Potentiometric hydrochloric acid titration of seawater provides a powerful technique for determining components of the carbonate system. Recently, questions have been raised regarding older computer procedures for extracting the carbonate system parameters from the titration curve. We compare four evaluation methods, an early Gran method, the GEOSECS Gran method, a new modified Gran method, and a curve-fitting method. We conclude that the new modified Gran method and the curve-fitting can result in a precision of better than 0.1% but because of possible problems associated with representing all relevant chemical reactions during titration, an alkalinity standard must be established before accuracies of 0.1% can be achieved.

  7. Determination of borate ion-pair stability constants by potentiometry and non-approximative linearization of titration data.

    PubMed

    Rogers, H R; van den Berg, C M

    1988-04-01

    Borate anions, B(OH)(-)(4), are known to associate with alkali and alkaline-earth metal cations in sea-water. The borate cation ion-pairs are of the general form MB(OH)((n-1)+)(4), where M(n+) is the cation. In this work, the cation borate stability constants (K*(MB)) have been evaluated for Na(+), Li(+), Mg(2+), Ca(2+) and Sr(2+) where K*(MB) = [MB(OH(4))((n-1)+)]/[M(n+)][B(OH)(-)(4)]. The K*(MB) values were obtained from values found for the stability constant of boric acid (K*(B)) in various electrolyte media at 25 degrees and an ionic strength of 0.7. Acid-base potentiometric titrations were performed in the electrolyte media with a standard Pt/H(2) electrode and a junctionless Ag/AgCl reference electrode to monitor the emf. A non-approximative equation was used to linearize the titration data. The values obtained were: K*(Lib) = 0.89 +/- 0.02, K*(NaB) = 0.44 +/- 0.01, K*(MgB) = 13.6 +/- 0.7, K*(CaB) = 11.4 +/- 0.15, K*(SrB) = 3.47 +/- 0.06. The values for K*(MB) correlate with the charge-density parameter z(2)/(r + 0.85), where r is the radius of the cation. The speciation of boron in sea-water was predicted from the K*(MB), data for the major cations present.

  8. Titrations using an apparatus for recording the antilogarithm of pH or pM.

    PubMed

    Johansson, A

    1974-12-01

    A titration apparatus plotting either the concentration of sample ion or the concentration of titrant ion has been tested. An antilog apparatus, converting measured e.m.f. values into concentrations is connected to ordinary titration equipment. The instrument has been tested by means of acid-base titrations (titrations of mixtures of weak acids and of a weak and a strong acid), precipitation titrations (determination of the chloride concentration in tap-water, titration of mixtures of halides), titrations with ion-selective electrodes (determination of the fluoride content of toothpaste) and complexometric titrations (determination of copper with EDTA, using mercuric ion as indicator ion and amalgamated silver rod as indicator electrode, or using a copper-selective indicator electrode). The method considerably simplifies the evaluation of the results as compared to conventional potentiometric titrations.

  9. Thermodynamic analysis of Bacillus subtilis endospore protonation using isothermal titration calorimetry

    NASA Astrophysics Data System (ADS)

    Harrold, Zoë R.; Gorman-Lewis, Drew

    2013-05-01

    Bacterial proton and metal adsorption reactions have the capacity to affect metal speciation and transport in aqueous environments. We coupled potentiometric titration and isothermal titration calorimetry (ITC) analyses to study Bacillus subtilis spore-proton adsorption. We modeled the potentiometric data using a four and five-site non-electrostatic surface complexation model (NE-SCM). Heats of spore surface protonation from coupled ITC analyses were used to determine site specific enthalpies of protonation based on NE-SCMs. The five-site model resulted in a substantially better model fit for the heats of protonation but did not significantly improve the potentiometric titration model fit. The improvement observed in the five-site protonation heat model suggests the presence of a highly exothermic protonation reaction circa pH 7 that cannot be resolved in the less sensitive potentiometric data. From the log Ks and enthalpies we calculated corresponding site specific entropies. Log Ks and site concentrations describing spore surface protonation are statistically equivalent to B. subtilis cell surface protonation constants. Spore surface protonation enthalpies, however, are more exothermic relative to cell based adsorption suggesting a different bonding environment. The thermodynamic parameters defined in this study provide insight on molecular scale spore-surface protonation reactions. Coupled ITC and potentiometric titrations can reveal highly exothermic, and possibly endothermic, adsorption reactions that are overshadowed in potentiometric models alone. Spore-proton adsorption NE-SCMs derived in this study provide a framework for future metal adsorption studies.

  10. Acid-base titrations for polyacids: Significance of the pK sub a and parameters in the Kern equation

    NASA Technical Reports Server (NTRS)

    Meites, L.

    1978-01-01

    A new method is suggested for calculating the dissociation constants of polyvalent acids, especially polymeric acids. In qualitative form the most significant characteristics of the titration curves are demonstrated and identified which are obtained when titrating the solutions of such acids with a standard base potentiometrically.

  11. A non-linear least-squares approach to the refinement of all parameters involved in acid-base titrations.

    PubMed

    Arena, G; Rizzarelli, E; Sammartano, S; Rigano, C

    1979-01-01

    A non-linear least-squares computer program has been written for the refinement of the parameters involved in potentiometric acid-base titrations. The program ACBA (ACid-BAse titrations) is applicable under quite general conditions to solutions containing one or more acids or bases. The method of refinement used gives the program several advantages over the other programs described previously.

  12. Acid-base properties of the alumina surface: influence of the titration procedures on the microcalorimetric results.

    PubMed

    Morel, Jean-Pierre; Marmier, Nicolas; Hurel, Charlotte; Morel-Desrosiers, Nicole

    2009-10-01

    The enthalpy changes associated with the protonation and deprotonation of an alumina surface have been determined on the basis of microcalorimetry experiments and acid-base potentiometric titrations at 25 degrees C. It has been shown that the results may vary significantly according to the experimental procedure. In order to do so, the potentiometric and microcalorimetric titrations have been carried out first from an acidic pH to basic pH and second from a pH near the pH(zpc) of alumina to acidic or basic pH. It has been demonstrated that the pK(a) values deduced from the potentiometric titrations are the same whatever the experimental protocol whereas the only way to obtain meaningful enthalpies of proton exchange is to carry out microcalorimetric titrations by starting around the point of zero charge.

  13. Aluminum(III) selective potentiometric sensor based on morin in poly(vinyl chloride) matrix.

    PubMed

    Gupta, Vinod K; Jain, Ajay K; Maheshwari, Gaurav

    2007-06-15

    Al(3+) selective sensor has been fabricated from poly(vinyl chloride) (PVC) matrix membranes containing neutral carrier morin as ionophore. Best performance was exhibited by the membrane having composition as morin:PVC:sodium tetraphenyl borate:tri-n-butylphosphate in the ratio 5:150:5:150 (w/w, mg). This membrane worked well over a wide activity range of 5.0x10(-7) to 1.0x10(-1)M of Al(3+) with a Nernstian slope of 19.7+/-0.1mV/decade of Al(3+) activity and a limit of detection 3.2x10(-7)M. The response time of the sensor is approximately 5s and membrane could be used over a period of 2 months with good reproducibility. The proposed sensor works well over a pH range (3.5-5.0) and demonstrates good discriminating power over a number of mono-, di- and trivalent cations. The sensor can also be used in partially non-aqueous media having up to 20% (v/v) methanol, ethanol or acetone content with no significant change in the value of slope or working activity range. The sensor has also been used in the potentiometric titration of Al(3+) with EDTA and for its determination in zinc plating mud and red mud.

  14. A fully automatic system for acid-base coulometric titrations.

    PubMed

    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 of various samples of environmental and nutritional interest, specifically waters, soft drinks and wines.

  15. Tripodal Receptors for Cation and Anion Sensors

    PubMed Central

    Kuswandi, Bambang; Nuriman; Verboom, Willem; Reinhoudt, David N.

    2006-01-01

    This review discusses different types of artificial tripodal receptors for the selective recognition and sensing of cations and anions. Examples on the relationship between structure and selectivity towards cations and anions are described. Furthermore, their applications as potentiometric ion sensing are emphasised, along with their potential applications in optical sensors or optodes.

  16. Modeling sorption of divalent metal cations on hydrous manganese oxide using the diffuse double layer model

    USGS Publications Warehouse

    Tonkin, J.W.; Balistrieri, L.S.; Murray, J.W.

    2004-01-01

    Manganese oxides are important scavengers of trace metals and other contaminants in the environment. The inclusion of Mn oxides in predictive models, however, has been difficult due to the lack of a comprehensive set of sorption reactions consistent with a given surface complexation model (SCM), and the discrepancies between published sorption data and predictions using the available models. The authors have compiled a set of surface complexation reactions for synthetic hydrous Mn oxide (HMO) using a two surface site model and the diffuse double layer SCM which complements databases developed for hydrous Fe (III) oxide, goethite and crystalline Al oxide. This compilation encompasses a range of data observed in the literature for the complex HMO surface and provides an error envelope for predictions not well defined by fitting parameters for single or limited data sets. Data describing surface characteristics and cation sorption were compiled from the literature for the synthetic HMO phases birnessite, vernadite and ??-MnO2. A specific surface area of 746 m2g-1 and a surface site density of 2.1 mmol g-1 were determined from crystallographic data and considered fixed parameters in the model. Potentiometric titration data sets were adjusted to a pH1EP value of 2.2. Two site types (???XOH and ???YOH) were used. The fraction of total sites attributed to ???XOH (??) and pKa2 were optimized for each of 7 published potentiometric titration data sets using the computer program FITEQL3.2. pKa2 values of 2.35??0.077 (???XOH) and 6.06??0.040 (???YOH) were determined at the 95% confidence level. The calculated average ?? value was 0.64, with high and low values ranging from 1.0 to 0.24, respectively. pKa2 and ?? values and published cation sorption data were used subsequently to determine equilibrium surface complexation constants for Ba2+, Ca2+, Cd 2+, Co2+, Cu2+, Mg2+, Mn 2+, Ni2+, Pb2+, Sr2+ and Zn 2+. In addition, average model parameters were used to predict additional

  17. Surface Titrations of Perlite Suspensions.

    PubMed

    Alkan; Do

    1998-11-01

    The surface charge behaviour of unexpanded and expanded perlite samples in KNO3 and NaCl solutions were investigated as a function of pH and ionic strength. The solutions of KNO3 and NaCl ranging from 10(-3) to 1.0 M were used. The potentiometric titration method was used to determine the surface charge of perlite samples. It was confirmed that the perlite samples had no the point of zero charge and was negatively charged in the pH range of 3-10. The double extrapolation method was used for determining the intrinsic equilibrium constants for simple ionization and complex ionization reactions. The values obtained are pKinta2 = 2.5 and p*KintK+ = 2.3 in KNO3 solutions and pKinta2 = 3.0 and p*KintNa+ = 2.4 in NaCl solutions for unexpanded perlite, and pKinta2 = 2.6 and p*KintK+ = 2.4 in KNO3 solutions and pKinta2 = 2.7 and pKintNa+ = 2.4 in NaCl solutions for expanded perlite. Copyright 1998 Academic Press.

  18. Surfactant/detergent titration analysis method and apparatus for machine working fluids, surfactant-containing wastewater and the like

    DOEpatents

    Smith, Douglas D.; Hiller, John M.

    1998-01-01

    The present invention is an improved method and related apparatus for quantitatively analyzing machine working fluids and other aqueous compositions such as wastewater which contain various mixtures of cationic, neutral, and/or anionic surfactants, soluble soaps, and the like. The method utilizes a single-phase, non-aqueous, reactive titration composition containing water insoluble bismuth nitrate dissolved in glycerol for the titration reactant. The chemical reaction of the bismuth ion and glycerol with the surfactant in the test solutions results in formation of micelles, changes in micelle size, and the formation of insoluble bismuth soaps. These soaps are quantified by physical and chemical changes in the aqueous test solution. Both classical potentiometric analysis and turbidity measurements have been used as sensing techniques to determine the quantity of surfactant present in test solutions. This method is amenable to the analysis of various types of new, in-use, dirty or decomposed surfactants and detergents. It is a quick and efficient method utilizing a single-phase reaction without needing a separate extraction from the aqueous solution. It is adaptable to automated control with simple and reliable sensing methods. The method is applicable to a variety of compositions with concentrations from about 1% to about 10% weight. It is also applicable to the analysis of waste water containing surfactants with appropriate pre-treatments for concentration.

  19. Surfactant/detergent titration analysis method and apparatus for machine working fluids, surfactant-containing wastewater and the like

    DOEpatents

    Smith, D.D.; Hiller, J.M.

    1998-02-24

    The present invention is an improved method and related apparatus for quantitatively analyzing machine working fluids and other aqueous compositions such as wastewater which contain various mixtures of cationic, neutral, and/or anionic surfactants, soluble soaps, and the like. The method utilizes a single-phase, non-aqueous, reactive titration composition containing water insoluble bismuth nitrate dissolved in glycerol for the titration reactant. The chemical reaction of the bismuth ion and glycerol with the surfactant in the test solutions results in formation of micelles, changes in micelle size, and the formation of insoluble bismuth soaps. These soaps are quantified by physical and chemical changes in the aqueous test solution. Both classical potentiometric analysis and turbidity measurements have been used as sensing techniques to determine the quantity of surfactant present in test solutions. This method is amenable to the analysis of various types of new, in-use, dirty or decomposed surfactants and detergents. It is a quick and efficient method utilizing a single-phase reaction without needing a separate extraction from the aqueous solution. It is adaptable to automated control with simple and reliable sensing methods. The method is applicable to a variety of compositions with concentrations from about 1% to about 10% weight. It is also applicable to the analysis of waste water containing surfactants with appropriate pre-treatments for concentration. 1 fig.

  20. An elevated temperature titration calorimeter

    SciTech Connect

    Smith, J.R.; Zanonato, P.L.; Choppin, G.R. . Dept. of Chemistry)

    1991-06-01

    A variable-temperature (313 K to 353 K) titration calorimeter of high sensitivity has been constructed. The purpose of the calorimeter is to study temperature effects on the enthalpies of complex formation and of other reactions of metal cations such as hydrolysis and precipitation. Operation of the calorimetric system, including that final calculation of the heat released during titration, is automatic via computer control. Calibration tests of the calorimeter using 2-amino-2-hydroxymethyl-1,3-propanediol gave -(46.0 {plus minus} 0.3) kJ mol{sup {minus}1} and -(46.2 {plus minus} 0.2) kJ mol{sup {minus}1} for the enthalpy of protonation, at 318 K and at 343 K, respectively. For titrations of 2-bis(2-hydroxyethyl) amino-2-hydroxymethyl-1,3-propanediol, enthalpy of protonation values of -(28.4 {plus minus} 0.3) kJ mol{sup {minus}1} and -(29.3 {plus minus} 0.2) kJ mol{sup {minus}1} were obtained at 318 K and at 343 K, respectively. 6 refs., 3 figs., 2 tabs.

  1. Micromechanical potentiometric sensors

    SciTech Connect

    Thundat, T.G.

    2000-01-25

    A microcantilever potentiometric sensor utilized for detecting and measuring physical and chemical parameters in a sample of media is described. The microcantilevered spring element includes at least one chemical coating on a coated region, that accumulates a surface charge in response to hydrogen ions, redox potential, or ion concentrations in a sample of the media being monitored. The accumulation of surface charge on one surface of the microcantilever, with a differing surface charge on an opposing surface, creates a mechanical stress and a deflection of the spring element. One of a multitude of deflection detection methods may include the use of a laser light source focused on the microcantilever, with a photo-sensitive detector receiving reflected laser impulses. The microcantilevered spring element is approximately 1 to 100 {mu}m long, approximately 1 to 50 {mu}m wide, and approximately 0.3 to 3.0 {mu}m thick. An accuracy of detection of deflections of the cantilever is provided in the range of 0.01 nanometers of deflection. The microcantilever apparatus and a method of detection of parameters require only microliters of a sample to be placed on, or near the spring element surface. The method is extremely sensitive to the detection of the parameters to be measured.

  2. Micromechanical potentiometric sensors

    DOEpatents

    Thundat, Thomas G.

    2000-01-01

    A microcantilever potentiometric sensor utilized for detecting and measuring physical and chemical parameters in a sample of media is described. The microcantilevered spring element includes at least one chemical coating on a coated region, that accumulates a surface charge in response to hydrogen ions, redox potential, or ion concentrations in a sample of the media being monitored. The accumulation of surface charge on one surface of the microcantilever, with a differing surface charge on an opposing surface, creates a mechanical stress and a deflection of the spring element. One of a multitude of deflection detection methods may include the use of a laser light source focused on the microcantilever, with a photo-sensitive detector receiving reflected laser impulses. The microcantilevered spring element is approximately 1 to 100 .mu.m long, approximately 1 to 50 .mu.m wide, and approximately 0.3 to 3.0 .mu.m thick. An accuracy of detection of deflections of the cantilever is provided in the range of 0.01 nanometers of deflection. The microcantilever apparatus and a method of detection of parameters require only microliters of a sample to be placed on, or near the spring element surface. The method is extremely sensitive to the detection of the parameters to be measured.

  3. Septonex-tetraphenylborate screen-printed ion selective electrode for the potentiometric determination of Septonex in pharmaceutical preparations.

    PubMed

    Mohamed, Gehad G; El-Shahat, M F; Al-Sabagh, A M; Migahed, M A; Ali, Tamer Awad

    2011-04-01

    A screen-printed electrode (SPE) was fabricated for the determination of 1-(ethoxycarbonyl)pentadecyltrimethylammonium bromide (Septonex) based on the use of Septonex-tetraphenylborate as the electroactive substance, and o-nitrophenyloctylether (o-NPOE) as the plasticizing agent. The electrode passes a near-Nernstian cationic slope of 59.33 ± 0.85 mV from activity between pH values of 2 to 9 with a lower detection limit of 9×10(-7) M and response time of about 5 s and exhibits an adequate shelf-life of 6 months. The method was applied for the determination of Septonex in pharmaceutical preparations. A percentage recovery of 99.88% was obtained with RSD=1.24%. The electrode was successfully applied in the determination of Septonex in laboratory-prepared samples by direct potentiometric, calibration curve and standard addition methods. Potentiometric titration of Septonex with sodium tetraphenylborate and phosphotungstic acid as a titrant was monitored with the modified screen-printed electrode as an end-point indicator electrode. Selectivity coefficients for Septonex relative to a number of potential interfering substances were determined. The sensor was highly selective for Septonex over a large number of compounds. Selectivity coefficient data for some common ions show negligible interference; however, cetyltrimethylammonium bromide and iodide ions interfere significantly. The analytical usefulness of the proposed electrode was evaluated by its application in the determination of Septonex in laboratory-prepared pharmaceutical samples with satisfactory results. The results obtained with the fabricated sensor are comparable with those obtained by the British Pharmacopeia method.

  4. Coulometric calcium pump for thin layer sample titrations.

    PubMed

    Ghahraman Afshar, Majid; Crespo, Gastón A; Bakker, Eric

    2015-10-01

    A selective electrochemical calcium pump based on a fast diffusive calcium ionophore-based membrane is reported. An initially nonpolarized ionophore-based membrane allows one to establish a net calcium flux by applying a potential step function (i.e., 250 mV for 30 s). The resulting calcium flux is released into a microliter scale thin layer reservoir, and the resulting ion perturbation is monitored by either a potentiometric or a coulometric readout. This chemical perturbation in the thin layer thus acts as a titration agent that is precisely controlled by coulometry. A linear correlation between released and detected calcium is confirmed by the two different readout modes. Having demonstrated the efficiency of the calcium pump in background electrolyte solutions, a complexometric titration with known concentrations of EDTA in the thin layer sample was performed. With the potentiometric readout, titrations in the range of 0.25-0.75 mM gave a precision of 3%, whereas the coulometric readout gave a range of 0.02-0.12 mM and a precision of 2%. Improved precision is expected by better control of the thin layer geometry by microfabrication. The significance of this work is that the coupling of a selective calcium pump with a thin layer element can give rise to rapid and complete sample concentration changes and result in a promising platform for titrations either on the laboratory bench or for in situ measurements in environmental or diagnostic settings.

  5. Effects of metal cations and fulvic acid on the adsorption of ciprofloxacin onto goethite.

    PubMed

    Tan, Yinyue; Guo, Yong; Gu, Xueyuan; Gu, Cheng

    2015-01-01

    Ciprofloxacin (CIP) can be strongly adsorbed by ferric oxides, but some influencing factors, such as multivalent cations and soil organic matter, have not been evaluated extensively. In this study, the interaction between CIP and four divalent metals (Ca, Cd, Cu, and Pb) was investigated using potentiometric titration and the results indicated that CIP can bind to the divalent metals in the following affinity order: Cu(II) > Pb(II) > Cd(II) > Ca(II). The effects of metals and fulvic acid (FA) on the adsorption behavior of CIP onto goethite surfaces were also examined using batch experiments. It was found that metal cations enhanced the CIP retention on goethite surfaces in the same order as the affinity order with CIP, indicating that metals likely increased CIP retention through cation bridging. FA was found to promote CIP sorption rather than compete with it, and the coexistence of FA and Cu(II) in the system exhibited an addictive effect with CIP sorption, indicating that they might influence the sorption separately under the studied loading condition. Taken together, our results suggested that the coexistence of divalent cations or soil organic matter will enhance CIP sorption on goethite surfaces, hence reducing its mobility and bioavailability in the environment.

  6. Acid-base equilibria in ethylene glycol--III: selection of titration conditions in ethylene glycol medium, protolysis constants of alkaloids in ethylene glycol and its mixtures.

    PubMed

    Zikolov, P; Zikolova, T; Budevsky, O

    1976-08-01

    Theoretical titration curves are used for the selection of appropriate conditions for the acid-base volumetric determination of weak bases in ethylene glycol medium. The theoretical curves for titration of some alkaloids are deduced graphically on the basis of the logarithmic concentration diagram. The acid-base constants used for the construction of the theoretical titration curves were determined by potentiometric titration in a cell without liquid junction, equipped with a glass and a silver-silver chloride electrode. It is shown that the alkaloids investigated can be determined accurately by visual or potentiometric titration. The same approach for the selection of titration conditions seems to be applicable to other non-aqueous amphiprotic solvents.

  7. Acid-base titrations in nonaqueous solvents Analysis of dimethyl sulphate.

    PubMed

    Banick, W M; Francis, E C

    1966-07-01

    A nonaqueous titrimetric procedure was developed for the determination of the dimethyl sulphate, methyl hydrogen sulphate and sulphuric acid content of dimethyl sulphate samples. Methyl hydrogen sulphate and sulphuric acid are determined by a differentiating potentiometric titration in pyridine with tributylethylammonium hydroxide. Pyridine converts the dimethyl sulphate into the weakly acidic methylpyridinium methyl sulphate which does not interfere in the titration. Dimethyl sulphate is determined by reacting it with an excess of 2-dimethylaminoethanol and titrating the excess with perchloric acid. Precision and recovery data for commercial samples of dimethyl sulphate are presented.

  8. Using spectrophotometric titrations to characterize humic acid reactivity at environmental concentrations.

    PubMed

    Janot, Noémie; Reiller, Pascal E; Korshin, Gregory V; Benedetti, Marc F

    2010-09-01

    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 mgDOC/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.

  9. Tandem electrochemical desalination-potentiometric nitrate sensing for seawater analysis.

    PubMed

    Cuartero, Maria; Crespo, Gastón A; Bakker, Eric

    2015-08-18

    We report on a methodology for the direct potentiometric determination of nitrate in seawater by in-line coupling to an electrochemical desalination module. A microfluidic custom-fabricated thin layer flat cell allows one to electrochemically reduce the chloride concentration of seawater more than 100-fold, from 600 mM down to ∼2.8 mM. The desalinator operates by the exhaustive electrochemical plating of the halides from the thin layer sample onto a silver element as silver chloride, which is coupled to the transfer of the counter cations across a permselective ion-exchange membrane to an outer solution. As a consequence of suppressing the major interference of an ion-exchanger based membrane, the 80 μL desalinated sample plug is passed to a potentiometric flow cell of 13 μL volume. The potentiometric sensor is composed of an all-solid-state nitrate selective electrode based on lipophilic carbon nanotubes (f-MWCNTs) as an ion-to-electron transducer (slope of -58.9 mV dec(-1), limit of detection of 5 × 10(-7) M, and response time of 5 s in batch mode) and a miniaturized reference electrode. Nitrate is successfully determined in desalinated seawater using ion chromatography as the reference method. It is anticipated that this concept may form an attractive platform for in situ environmental analysis of a variety of ions that normally suffer from interference by the high saline level of seawater. PMID:26201537

  10. Tandem electrochemical desalination-potentiometric nitrate sensing for seawater analysis.

    PubMed

    Cuartero, Maria; Crespo, Gastón A; Bakker, Eric

    2015-08-18

    We report on a methodology for the direct potentiometric determination of nitrate in seawater by in-line coupling to an electrochemical desalination module. A microfluidic custom-fabricated thin layer flat cell allows one to electrochemically reduce the chloride concentration of seawater more than 100-fold, from 600 mM down to ∼2.8 mM. The desalinator operates by the exhaustive electrochemical plating of the halides from the thin layer sample onto a silver element as silver chloride, which is coupled to the transfer of the counter cations across a permselective ion-exchange membrane to an outer solution. As a consequence of suppressing the major interference of an ion-exchanger based membrane, the 80 μL desalinated sample plug is passed to a potentiometric flow cell of 13 μL volume. The potentiometric sensor is composed of an all-solid-state nitrate selective electrode based on lipophilic carbon nanotubes (f-MWCNTs) as an ion-to-electron transducer (slope of -58.9 mV dec(-1), limit of detection of 5 × 10(-7) M, and response time of 5 s in batch mode) and a miniaturized reference electrode. Nitrate is successfully determined in desalinated seawater using ion chromatography as the reference method. It is anticipated that this concept may form an attractive platform for in situ environmental analysis of a variety of ions that normally suffer from interference by the high saline level of seawater.

  11. A Unified Titration Formula

    NASA Astrophysics Data System (ADS)

    Glaister, P.

    1999-01-01

    In a number of standard titrations, a volume of a monoprotic base MOH at a specific concentration is added to a volume of a monoprotic acid HA at a specific concentrations. Four different types of titration are possible, depending on whether the acid and base are strong or weak. In a recent article, some of these cases are discussed in detail. However, a single unifying formula covering all four cases has been determined.

  12. A PC-based titrator for flow gradient titrations

    PubMed Central

    Fuhrmann, B.

    1993-01-01

    This paper describes a PC (personal computer) based titrator which was developed for gradient flow titrations. Concentration gradients were generated electrolytically or volumetrically in small tubes. Complete titration curves can be recorded on-line and evaluated automatically. The titrator can be used with all liquid flow detectors with low axial dispersion. The titrator was evaluated for the titration of thiosulphate with electrogenerated triiodide and for the titration of ammonia with electrogenerated hypobromite after continuous gas dialytic separation of ammonia from the sample solution. PMID:18924977

  13. Potentiometric studies at ORNL with hydrogen electrode concentration cells

    SciTech Connect

    Mesmer, R.E.; Palmer, D.A.; Wesolowski, D.J.

    1994-12-31

    The absence of suitably stable reference electrodes for and to 300 C led ORNL to develop hydrogen electrode concentration cells for studies of equilibria of interest in reactor and steam generator systems to about 300 C during the late 1960`s and seventies. During the intervening two dozen years over twenty scientists have participated in potentiometric studies at Oak Ridge and much of that work will be summarized in this paper. A description of hydrogen electrode concentration cells developed in the late sixties and currently in use at Oak Ridge is given. The method of measurement, data interpretation, and published results are reviewed for studies of acid-base ionization, metal ion hydrolysis, and metal complexation reactions using principally such cells in titration or flow modes. 41 refs.

  14. Galvanic cell without liquid junction for potentiometric determination of copper.

    PubMed

    Migdalski, Jan; Błaz, Teresa; Zrałka, Barbara; Lewenstam, Andrzej

    2007-07-01

    This paper describes potentiometric measurements in an integrated galvanic cell with both indicator and reference electrodes. Both electrodes are conducting polymer-based. The copper-sensitive indicator electrode is made by using poly(3,4-ethylenedioxythiophene) (PEDOT) doped with 2-(o-arsenophenylazo)-1,8-dihydroxynaphthalene-3,6-disulphonic sodium salt (Arsenazo-I) as the electroactive substance in the film, while the reference electrode is based on PEDOT doped by 2-morpholineoethanesulfonic acid (MES). It is shown that the galvanic cell can be used for determination of copper both in non-aqueous media (where all PVC-based membranes failed) and in the presence of chloride ions, which disturb the signal of conventional copper ion-selective electrodes with solid-state membranes. It is further shown that the titration of copper ions can be successfully monitored using the described electrochemical cell.

  15. Potentiometric sensor for the high throughput determination of tetramisole hydrochloride.

    PubMed

    Gupta, Vinod Kumar; Singh, Ashok Kumar; Gupta, Barkha

    2007-08-01

    The electrochemical response characteristics of poly(vinyl)chloride (PVC) based membrane sensors for determination of tetramisole hydrochloride (TmCl) is described. The membranes of these electrodes consist of tetramisole-tetraphenyl borate (Tm-TPB), chlorophenyl borate (Tm-ClPB), and phosphotungstate (Tm(3)-PT) ion associations dispersed in a PVC matrix with dibutylpthalate as a plasticizer. The electrodes were fully characterized in terms of composition, life span, usable pH range, and working concentration range and ionic strength. The electrodes showed Nernstian response over the concentration ranges of 7.4 x 10(-7) to 1.0 x 10(-2) M, 1.7 x 10(-6) to 1.0 x 10(-2) M, and 5.6 x 10(-6) to 1.0 x 10(-2) M TmCl, respectively, and were applied to the potentiometric determination of tetramisole ion in pure solutions and pharmaceutical preparations. The potentiometric determination was also used in the determination of tetramisole in pharmaceutical preparations in four batches of different expiration dates. The electrodes exhibited good selectivity for TmCl with respect to a large number of excipients such as inorganic cations, organic cations, amino acids, and sugars. The solubility product of the ion-pair and the formation constant of the precipitation reaction leading to the ion-pair formation were determined conductometrically. The new potentiometric method offers the advantages of high-throughput determination, simplicity, accuracy, automation feasibility, and applicability to turbid and colored sample solutions. PMID:17979641

  16. Construction and performance characterization of screen printed and carbon paste ion selective electrodes for potentiometric determination of naphazoline hydrochloride in pharmaceutical preparations.

    PubMed

    Frag, Eman Y Z; Mohamed, Gehad G; El-Dien, F A Nour; Mohamed, Marwa E

    2011-01-21

    This paper describes the development of screen-printed (SPE) and carbon paste (CPE) sensors for the rapid and sensitive quantification of naphazoline hydrochloride (NPZ) in pharmaceutical formulations. This work compares the electroactivity of conventional carbon paste and screen-printed carbon paste electrodes towards potentiometric titration of NPZ. The repeatability and accuracy of measurements performed in the analysis of these pharmaceutical matrices using new screen printed sensors were evaluated. The influence of the electrode composition, conditioning time of the electrode and pH of the test solution, on the electrode performance were investigated. The drug electrode showed Nernstain responses in the concentration range from 1 × 10(-6) to 1 × 10(-2) mol L(-1) with slopes of 57.5 ± 1.3 and 55.9 ± 1.6 mV per decade for SPE and CPE, respectively, and was found to be very precise and usable within the pH range 3-8. These sensors exhibited a fast response time (about 3 s for both SPE and CPE, respectively), a low detection limit (3.5 × 10(-6) and 1.5 × 10(-6) M for SPE and CPE, respectively), a long lifetime (3 and 2 months for SPE and CPE, respectively) and good stability. The selectivity of the electrode toward a large number of inorganic cations, sugars and amino acids was tested. It was applied to potentiometric determination of NPZ in pure state and pharmaceutical preparation under batch conditions. The percentage recovery values for the assay of NPZ in tablets (relative standard deviations ≤0.3% for n = 4) were compared well with those obtained by the official method.

  17. Universal tracer monitored titrations.

    PubMed

    DeGrandpre, Michael D; Martz, Todd R; Hart, Robert D; Elison, David M; Zhang, Alice; Bahnson, Anna G

    2011-12-15

    Titrations, while primarily known as the chemical rite of passage for fledgling science students, are still widely used for chemical analysis. With its many years of existence and improvement, the method would seem an unlikely candidate for innovation, yet it is desirable, in this age of autonomous sensing where analyzers may be sent into space or to the bottom of the ocean, to have a simplified titrimetric method that does not rely upon volumetric or gravimetric measurement of sample and titrant. In previous work on the measurement of seawater alkalinity, we found that use of a tracer in the titrant eliminates the need to measure mass or volume. Here, we show the versatility of the method for diverse types of titrations and tracers. The results suggest that tracers may be employed in all types of titrations, opening the door for greatly simplified laboratory and field-based chemical analysis.

  18. Theoretical problems associated with the use of acetic anhydride as a co-solvent for the non-aqueous titration of hydrohalides of organic bases and quaternary ammonium salts.

    PubMed

    Völgyi, Gergely; Béni, Szabolcs; Takács-Novák, Krisztina; Görög, Sándor

    2010-01-01

    A potentiometric titration study of organic base hydrohalides and quaternary ammonium salts using perchloric acid as the titrant and a mixture of acetic anhydride and acetic acid as the solvent was carried out and the titration mixture was analysed by NMR in order to clarify the chemistry of the reactions involved. It was found that in contrast to the general belief the formation of acetyl halides and titratable free acetate ion does not take place prior to the titration but NMR spectra proved the formation of acetyl halides in the course of the titration. This observation and the fact that the shape of the titration curves depends on the nature of the hydrohaloic acid bound to the base or of the anion in the quaternary ammonium salts led to the conclusion that the titrating agent is acetyl perchlorate formed in situ during the titration. Equations of the reactions involved in the titration process are shown in the paper.

  19. The Titration Project.

    ERIC Educational Resources Information Center

    Kilner, Cary

    1988-01-01

    Discusses the development of concentration and organizational skills, patience, self-discipline, attention to detail, and appreciation for error analysis through an expanded titration project. Describes the various activities in the extended project and the materials and instructional support needed. Stresses the advantage to students in their…

  20. Filtrates & Residues: Olfactory Titration.

    ERIC Educational Resources Information Center

    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)

  1. Acid-base titration curves for acids with very small ratios of successive dissociation constants.

    PubMed

    Campbell, B H; Meites, L

    1974-02-01

    The shapes of the potentiometric acid-base titration curves obtained in the neutralizations of polyfunctional acids or bases for which each successive dissociation constant is smaller than the following one are examined. In the region 0 < < 1 (where is the fraction of the equivalent volume of reagent that has been added) the slope of the titration curve decreases as the number j of acidic or basic sites increases. The difference between the pH-values at = 0.75 and = 0.25 has (1 j)log 9 as the lower limit of its maximum value.

  2. [Alkalimetric titrations of salts of organic bases in the Pharmacopoeia].

    PubMed

    Bezáková, Zelmíra; Stankovičová, Mária

    2013-12-01

    Modified methods - alkalimetry in ethanol 70% with a defined small volume of hydrochloric acid 0.01 mol/l added to the solution of the sample before the titration and alkalimetry in ethanol 70% or ethanol 96% alone with potentiometric end-point detection for the assay of halide salts of 11 organic N-bases has been investigated. The results were compared to those obtained by the method of the European Pharmacopoeia 7th Ed. (Ph. Eur. 7th Ed.). The Ph. Eur. 7th Ed. use for 8 investigated substances alkalimetry in alcohol 96 % with a defined small volume of hydrochloric acid 0.01 mol/l (5 ml) with potentiometric end-point detection: Cinchocaine hydrochloride, Codeine hydrochloride dihydrate, Ethylmorphine hydrochloride, Lidocaine hydrochloride, Papaverine hydrochloride, Pilocarpine hydrochloride, Quinine hydrochloride, Tetracaine hydrochloride. Our results revealed that the Ph. Eur. 7th Ed. method did not work for 5 drugs from this group: Cinchocaine hydrochloride, Ethylmorphine hydrochloride, Papaverine hydrochloride, Pilocarpine hydrochloride and Tetracaine hydrochloride. In the group of investigated substances we included also drugs with the character of weak organic bases for which Ph. Eur. 7th Ed. prescribed different methods for their assay: Thiamine hydrochloride and Pyridoxine hydrochloride - acidimetric titration in non-aqueous solvents with perchloric acid and Procaine hydrochloride - determination of primary aromatic amino-nitrogen (Ph. Eur. 7th Ed., chapter 2.5.8).

  3. Surfactant titration of nanoparticle-protein corona.

    PubMed

    Maiolo, Daniele; Bergese, Paolo; Mahon, Eugene; Dawson, Kenneth A; Monopoli, Marco P

    2014-12-16

    Nanoparticles (NP), when exposed to biological fluids, are coated by specific proteins that form the so-called protein corona. While some adsorbing proteins exchange with the surroundings on a short time scale, described as a "dynamic" corona, others with higher affinity and long-lived interaction with the NP surface form a "hard" corona (HC), which is believed to mediate NP interaction with cellular machineries. In-depth NP protein corona characterization is therefore a necessary step in understanding the relationship between surface layer structure and biological outcomes. In the present work, we evaluate the protein composition and stability over time and we systematically challenge the formed complexes with surfactants. Each challenge is characterized through different physicochemical measurements (dynamic light scattering, ζ-potential, and differential centrifugal sedimentation) alongside proteomic evaluation in titration type experiments (surfactant titration). 100 nm silicon oxide (Si) and 100 nm carboxylated polystyrene (PS-COOH) NPs cloaked by human plasma HC were titrated with 3-[(3-Cholamidopropyl) dimethylammonio]-1-propanesulfonate (CHAPS, zwitterionic), Triton X-100 (nonionic), sodium dodecyl sulfate (SDS, anionic), and dodecyltrimethylammonium bromide (DTAB, cationic) surfactants. Composition and density of HC together with size and ζ-potential of NP-HC complexes were tracked at each step after surfactant titration. Results on Si NP-HC complexes showed that SDS removes most of the HC, while DTAB induces NP agglomeration. Analogous results were obtained for PS NP-HC complexes. Interestingly, CHAPS and Triton X-100, thanks to similar surface binding preferences, enable selective extraction of apolipoprotein AI (ApoAI) from Si NP hard coronas, leaving unaltered the dispersion physicochemical properties. These findings indicate that surfactant titration can enable the study of NP-HC stability through surfactant variation and also selective separation

  4. Titration Curves: Fact and Fiction.

    ERIC Educational Resources Information Center

    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…

  5. Anion-exchange nanospheres as titration reagents for anionic analytes.

    PubMed

    Zhai, Jingying; Xie, Xiaojiang; Bakker, Eric

    2015-08-18

    We present here anion-exchange nanospheres as novel titration reagents for anions. The nanospheres contain a lipophilic cation for which the counterion is initially Cl(-). Ion exchange takes place between Cl(-) in the nanospheres and a more lipophilic anion in the sample, such as ClO4(-) and NO3(-). Consecutive titration in the same sample solution for ClO4(-) and NO3(-) were demonstrated. As an application, the concentration of NO3(-) in spinach was successfully determined using this method.

  6. Radiometric acid-base titrations.

    PubMed

    Erdey, L; Gimesi, O; Szabadváry, F

    1969-03-01

    Acid-base titrations can be performed with radiometric end-point detection by use of labelled metal salts (e.g., ZnCl(2), HgCl(2)). Owing to the formation or dissolution of the corresponding hydroxide after the equivalence point, the activity of the titrated solution linearly increases or decreases as excess of standard solution is added. The end-point of the titration is determined graphically.

  7. 3-methyl-2-oxazolidone as a solvent for acid-base titrations.

    PubMed

    Taphorn, J E; Davies, G M; Caruso, J A

    1975-07-01

    3-Methyl-2-oxazolidone has been evaluated as a solvent for the titration of various weak carboxylic acids and phenols. Its high dielectric constant and wide liquid range contribute to its outstanding solvent properties. Tetrabutylammonium hydroxide was the titrant. End-points were determined potentiometrically with a glass-calomel electrode system. FORTRAN computer programs were used to evaluate the results, and relative acid strengths were determined and related to the aqueous acidity. The accuracies obtained are comparable to those for other solvent media. An 800-mV potential span is available in this solvent, which may allow differentiating titrations to be performed. No titrations of acid mixtures were attempted, but it was found possible to distinguish both neutralization steps for salicylic acid and o-phthalic acid.

  8. Titration behaviour of three strains of tobacco mosaic virus.

    PubMed

    Hendry, D A; Durham, A C

    1980-01-15

    Hydrogen ion titration curves of the virions and proteins of three strains of tobacco mosaic virus (Y-TAMV, U2, and cowpea) were measured in the absence and the presence of Ca2+, Mg2+, or Mn2+ ions, and compared with the analogous curves for the type strain (vulgare). Extinction coefficients were also measured for all four strains' virions and proteins. Y-TAMV is very like vulgare in its cation affinities: the virion has probably three groups per protein subunit that titrate near neutral pH and significantly bind metal ions; the RNA-free protein has very little affinity for Ca2+, although moderate Ca2+ concentrations favour the existence of larger polymers. U2 and cowpea strain virions bind cations significantly more strongly than do Y-TAMV or vulgare virions: their polymerized proteins, too, have significant affinities for Ca2+ ions, which make their titration and sedimentation behaviours relatively sensitive to added calcium. These cation-binding differences correspond well with the differences between the strains' protein sequences. The features common to all four strains are that the virions are apparently structurally invariant and have at least one site per subunit with Ca2+ affinity in the region of 10(-5)M, while the RNA-free proteins lack the high-affinity sites but have weaker Ca2+ affinities in the region of 10(-3)M. Some of the cation-binding sites probably lie near the central holes of the virions.

  9. Actinide cation-cation complexes

    SciTech Connect

    Stoyer, N.J.; Seaborg, G.T.

    1994-12-01

    The +5 oxidation state of U, Np, Pu, and Am is a linear dioxo cation (AnO{sub 2}{sup +}) with a formal charge of +1. These cations form complexes with a variety of other cations, including actinide cations. Other oxidation states of actinides do not form these cation-cation complexes with any cation other than AnO{sub 2}{sup +}; therefore, cation-cation complexes indicate something unique about AnO{sub 2}{sup +} cations compared to actinide cations in general. The first cation-cation complex, NpO{sub 2}{sup +}{center_dot}UO{sub 2}{sup 2+}, was reported by Sullivan, Hindman, and Zielen in 1961. Of the four actinides that form AnO{sub 2}{sup +} species, the cation-cation complexes of NpO{sub 2}{sup +} have been studied most extensively while the other actinides have not. The only PuO{sub 2}{sup +} cation-cation complexes that have been studied are with Fe{sup 3+} and Cr{sup 3+} and neither one has had its equilibrium constant measured. Actinides have small molar absorptivities and cation-cation complexes have small equilibrium constants; therefore, to overcome these obstacles a sensitive technique is required. Spectroscopic techniques are used most often to study cation-cation complexes. Laser-Induced Photacoustic Spectroscopy equilibrium constants for the complexes NpO{sub 2}{sup +}{center_dot}UO{sub 2}{sup 2+}, NpO{sub 2}{sup +}{center_dot}Th{sup 4+}, PuO{sub 2}{sup +}{center_dot}UO{sub 2}{sup 2+}, and PuO{sub 2}{sup +}{center_dot}Th{sup 4+} at an ionic strength of 6 M using LIPAS are 2.4 {plus_minus} 0.2, 1.8 {plus_minus} 0.9, 2.2 {plus_minus} 1.5, and {approx}0.8 M{sup {minus}1}.

  10. Schiff's Bases and Crown Ethers as Supramolecular Sensing Materials in the Construction of Potentiometric Membrane Sensors

    PubMed Central

    Faridbod, Farnoush; Ganjali, Mohammad Reza; Dinarvand, Rassoul; Norouzi, Parviz; Riahi, Siavash

    2008-01-01

    Ionophore incorporated PVC membrane sensors are well-established analytical tools routinely used for the selective and direct measurement of a wide variety of different ions in complex biological and environmental samples. Potentiometric sensors have some outstanding advantages including simple design and operation, wide linear dynamic range, relatively fast response and rational selectivity. The vital component of such plasticized PVC members is the ionophore involved, defining the selectivity of the electrodes' complex formation. Molecular recognition causes the formation of many different supramolecules. Different types of supramolecules, like calixarenes, cyclodextrins and podands, have been used as a sensing material in the construction of ion selective sensors. Schiff's bases and crown ethers, which feature prominently in supramolecular chemistry, can be used as sensing materials in the construction of potentiometric ion selective electrodes. Up to now, more than 200 potentiometric membrane sensors for cations and anions based on Schiff's bases and crown ethers have been reported. In this review cation binding and anion complexes will be described. Liquid membrane sensors based on Schiff's bases and crown ethers will then be discussed.

  11. Effect of the presence of cationic polyacrylamide on the surface properties of aqueous alumina suspension-stability mechanism

    NASA Astrophysics Data System (ADS)

    Wiśniewska, Małgorzata; Chibowski, Stanisław; Urban, Teresa

    2014-11-01

    The effects of solution pH and the content of cationic groups in polyacrylamide (PAM) macromolecules on the stability mechanism of aqueous alumina suspension were investigated. The following experimental techniques were applied: spectrophotometry, potentiometric titration, microelectrophoresis, viscosimetry and turbidimetry. They enable determination of polymer adsorbed amount, surface charge density and zeta potential of solid particles in the presence and absence of PAM, as well as thickness of polymer adsorption layer, size of macromolecules in the solution and stability of the Al2O3-polymer systems, respectively. The obtained results indicate that adsorption of PAM increases with the increasing pH, whereas the thickness of polymeric adsorption layer decreases. Additionally, the greater the number of cationic groups in the PAM chains is, the higher adsorption was found. The polymer presence influences on the alumina suspension stability. At pH 3 and 6 the slight deterioration of stability conditions of solid particle covered with polyacrylamide was observed. At pH 9 the systems containing polymer are unstable, similarly to the suspension without PAM, but the mechanism of their destabilization is different.

  12. Rapid hydrolysis of model phosphate diesters by alkaline-earth cations in aqueous DMSO: speciation and kinetics.

    PubMed

    Taran, Olga; Medrano, Felipe; Yatsimirsky, Anatoly K

    2008-12-14

    Kinetics of the cleavage of two phosphate diesters, bis(4-nitrophenyl) phosphate and 2-hydroxypropyl 4-nitrophenyl phosphate and a triester, 4-nitrophenyl diphenyl phosphate, in the presence of Mg(II), Ca(II) and Sr(II) were studied in 90% vol. DMSO at 37 degrees C. The alkaline hydrolysis of the triester was inhibited by all cations, but with both phosphodiesters strong catalytic effects were observed. Potentiometric titrations of metal perchlorates by Bu4N(OH) revealed formation of M2(OH)3+, M(OH)+, M(OH)2 and M2(OH)5- species. Rate constants for phosphodiester cleavage by individual species were obtained from analysis of rate-concentration profiles. Observed first-order rate constants in the presence of 1-2 mM Mg(II) or Ca(II) in neutral and weakly basic solutions were 10(8)-10(11) times higher than those for background hydrolysis at the same pH while in water additions of up to 50 mM metal produced <100-fold accelerations. Possible structures of DMSO solvated catalyst-substrate complexes were modeled by DFT calculations with Mg(II). The increased catalytic activity in 90% DMSO is attributed to stronger association of hydroxide ions and anionic phosphodiesters with metal ions and to preferable solvation of cations by DMSO, which creates favorable for reaction anhydrous microenvironment in the coordination sphere of the catalyst.

  13. Tracer-monitored flow titrations.

    PubMed

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

    2016-01-01

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

  14. Tracer-monitored flow titrations.

    PubMed

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

    2016-01-01

    The feasibility of implementing tracer-monitored titrations in a flow system is demonstrated. A dye tracer is used to estimate the instant sample and titrant volumetric fractions without the need for volume, mass or peak width measurements. The approach was applied to spectrophotometric flow titrations involving variations of sample and titrant flow-rates (i.e. triangle programmed technique) or concentration gradients established along the sample zone (i.e. flow injection system). Both strategies required simultaneous monitoring of two absorbing species, namely the titration indicator and the dye tracer. Mixing conditions were improved by placing a chamber with mechanical stirring in the analytical path aiming at to minimize diffusional effects. Unlike most of flow-based titrations, the innovation is considered as a true titration, as it does not require a calibration curve thus complying with IUPAC definition. As an application, acidity evaluation in vinegars involving titration with sodium hydroxide was selected. Phenolphthalein and brilliant blue FCF were used as indicator and dye tracer, respectively. Effects of sample volume, titrand/titrant concentrations and flow rates were investigated aiming at improved accuracy and precision. Results were reliable and in agreement with those obtained by a reference titration procedure. PMID:26703261

  15. Iodine losses during Winkler titrations

    NASA Astrophysics Data System (ADS)

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

    1991-01-01

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

  16. Interaction of Sodium Hyaluronate with a Biocompatible Cationic Surfactant from Lysine: A Binding Study.

    PubMed

    Bračič, Matej; Hansson, Per; Pérez, Lourdes; Zemljič, Lidija F; Kogej, Ksenija

    2015-11-10

    Mixtures of natural and biodegradable surfactants and ionic polysaccharides have attracted considerable research interest in recent years because they prosper as antimicrobial materials for medical applications. In the present work, interactions between the lysine-derived biocompatible cationic surfactant N(ε)-myristoyl-lysine methyl ester, abbreviated as MKM, and the sodium salt of hyaluronic acid (NaHA) are investigated in aqueous media by potentiometric titrations using the surfactant-sensitive electrode and pyrene-based fluorescence spectroscopy. The critical micelle concentration in pure surfactant solutions and the critical association concentration in the presence of NaHA are determined based on their dependence on the added electrolyte (NaCl) concentration. The equilibrium between the protonated (charged) and deprotonated (neutral) forms of MKM is proposed to explain the anomalous binding isotherms observed in the presence of the polyelectrolyte. The explanation is supported by theoretical model calculations of the mixed-micelle equilibrium and the competitive binding of the two MKM forms to the surface of the electrode membrane. It is suggested that the presence of even small amounts of the deprotonated form can strongly influence the measured electrode response. Such ionic-nonionic surfactant mixtures are a special case of mixed surfactant systems where the amount of the nonionic component cannot be varied independently as was the case for some of the earlier studies.

  17. Simple Potentiometric Determination of Reducing Sugars

    ERIC Educational Resources Information Center

    Moresco, Henry; Sanson, Pedro; Seoane, Gustavo

    2008-01-01

    In this article a potentiometric method for reducing sugar quantification is described. Copper(II) ion reacts with the reducing sugar (glucose, fructose, and others), and the excess is quantified using a copper wire indicator electrode. In order to accelerate the kinetics of the reaction, working conditions such as pH and temperature must be…

  18. Amperometric, Bipotentiometric, and Coulometric Titration.

    ERIC Educational Resources Information Center

    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)

  19. Potentiometric determination of pK(A) of organic bases in acetone by the application of coulometry.

    PubMed

    Vajgand, V J; Mihajlović, R P; Dzudović, R M

    1989-11-01

    A coulometric-potentiometric method for the determination of pK(A) values of organic bases in anhydrous acetone is described. The bases were titrated with protons obtained by anodic oxidation of hydrogen dissolved in palladium, in the presence of sodium perchlorate as the supporting electrolyte. A pair of glass electrodes was used for measuring directly the difference between the half-neutralization potentials of the standard and the base being studied. The pK(A) values obtained were close to those reported in the literature. The effect of the supporting electrolyte concentration on the pK(A) values of some of the bases was also studied.

  20. Surface Complexation of Neodymium at the Rutile-Water Interface: A Potentiometric and Modeling Study in NaCl Media to 250°C

    SciTech Connect

    Ridley, Mora K.; Machesky, Michael L.; Wesolowski, David J; Palmer, Donald

    2005-01-01

    The adsorption of Nd{sup 3+} onto rutile surfaces was examined by potentiometric titration from 25 to 250 C, in 0.03 and 0.30m NaCl background electrolyte. Experimental results show that Nd{sup 3+} sorbs strongly, even at low temperature, with adsorption commencing below the pHznpc of rutile. In addition, there is a systematic increase in Nd{sup 3+} adsorption with increasing temperature. The experimental results were rationalized and described using surface oxygen proton affinities computed from the MUlti SIte Complexation or MUSIC model, coupled with a Stern-based three-layer description of the oxide/water interface. Moreover, molecular-scale information was incorporated successfully into the surface complexation model, providing a unique geometry for the adsorption of Nd{sup 3+} on rutile. The primary mode of Nd{sup 3+} adsorption was assumed to be the tetradentate configuration found for Y{sup 3+} adsorption on the rutile (110) surface from previously described in situ X-ray standing wave experiments, wherein the sorbing cations bond directly with two adjacent ''terminal'' and two adjacent ''bridging'' surface oxygen atoms. Similarly, the adsorption of Na{sup +} counterions was also assumed to be tetradentate, as supported by MD simulations of Na{sup +} interactions with the rutile (110) surface, and by analogous X-ray standing wave results for Rb{sup +} adsorption on rutile. Fitting parameters for Nd{sup 3+} adsorption included binding constants for the tetradentate adsorption complex and capacitance values for the inner-sphere binding plane. In addition, hydrolysis of the tetradentate adsorption complex was permitted and resulted in significantly improved model fits at higher temperature and pH values. The modeling results indicate that the Stern-based MUSIC surface-complexation model adequately accommodates molecular-scale information to uniquely rationalize and describe multivalent ion adsorption systematically into the hydrothermal regime.

  1. Surface complexation of neodymium at the rutile-water interface: A potentiometric and modeling study in NaCl media to 250°C

    NASA Astrophysics Data System (ADS)

    Ridley, Moira K.; Machesky, Michael L.; Wesolowski, David J.; Palmer, Donald A.

    2005-01-01

    The adsorption of Nd 3+ onto rutile surfaces was examined by potentiometric titration from 25 to 250°C, in 0.03 and 0.30 m NaCl background electrolyte. Experimental results show that Nd 3+ sorbs strongly, even at low temperature, with adsorption commencing below the pH znpc of rutile. In addition, there is a systematic increase in Nd 3+ adsorption with increasing temperature. The experimental results were rationalized and described using surface oxygen proton affinities computed from the MUlti SIte Complexation or MUSIC model, coupled with a Stern-based three-layer description of the oxide/water interface. Moreover, molecular-scale information was incorporated successfully into the surface complexation model, providing a unique geometry for the adsorption of Nd 3+ on rutile. The primary mode of Nd 3+ adsorption was assumed to be the tetradentate configuration found for Y 3+ adsorption on the rutile (110) surface from previously described in situ X-ray standing wave experiments, wherein the sorbing cations bond directly with two adjacent "terminal" and two adjacent "bridging" surface oxygen atoms. Similarly, the adsorption of Na + counterions was also assumed to be tetradentate, as supported by MD simulations of Na + interactions with the rutile (110) surface, and by analogous X-ray standing wave results for Rb + adsorption on rutile. Fitting parameters for Nd 3+ adsorption included binding constants for the tetradentate adsorption complex and capacitance values for the inner-sphere binding plane. In addition, hydrolysis of the tetradentate adsorption complex was permitted and resulted in significantly improved model fits at higher temperature and pH values. The modeling results indicate that the Stern-based MUSIC surface-complexation model adequately accommodates molecular-scale information to uniquely rationalize and describe multivalent ion adsorption systematically into the hydrothermal regime.

  2. Design and construction of new potentiometric sensors for determination of Al3+ ion based on (Z)-2-(2-methyl benzylidene)-1-(2,4-dinitrophenyl) hydrazine.

    PubMed

    Mizani, F; Salmanzadeh Ardabili, S; Ganjaliab, M R; Faridbod, F; Payehghadr, M; Azmoodeh, M

    2015-04-01

    (Z)-2-(2-methyl benzylidene)-1-(2,4-dinitrophenyl) hydrazine (L) was used as an active component of PVC membrane electrode (PME), coated graphite electrode (CGE) and coated silver wire electrode (CWE) for sensing Al(3+) ion. The electrodes exhibited linear Nernstian responses to Al(3+) ion in the concentration range of 1.0×10(-6) to 1.0×10(-1)M (for PME, LOD=8.8×10(-7)M), 5.5×10(-7) to 2.0×10(-1)M (for CWE, LOD=3.3×10(-7)M) and 1.5×10(-7) to 1.0×10(-1)M (for CGE, LOD=9.2×10(-8)M). The best performances were observed with the membranes having the composition of L:PVC:NPOE:NaTPB in the ratio of 5:35:57:3 (w/w; mg). The electrodes have a response time of 6s and an applicable pH range of 3.5-9.1. The sensors have a lifetime of about 15weeks and exhibited excellent selectivity over a number of mono-, bi-, and tri-valent cations including alkali, alkaline earth metal, heavy and transition metal ions. Analytical utility of the proposed sensor has been further tested by using it as an indicator electrode in the potentiometric titration of Al(3+) with EDTA. The electrode was also successfully applied for the determination of Al(3+) ion in real and pharmaceutical samples.

  3. Potentiometric determination of free acidity in presence of hydrolysable ions and a sequential determination of hydrazine.

    PubMed

    Ganesh, S; Khan, Fahmida; Ahmed, M K; Pandey, S K

    2011-08-15

    A simple potentiometric method for the determination of free acidity in presence of hydrolysable ions and sequential determination of hydrazine is developed and described. Both free acid and hydrazine are estimated from the same aliquot. In this method, free acid is titrated with standard sodium carbonate solution after the metal ions in solutions are masked with EDTA. Once the end point for the free acid is determined at pH 3.0, an aliquot of formaldehyde is added to liberate the acid equivalent to hydrazine which is then titrated with the same standard sodium carbonate solution using an automatic titration system. The described method is simple, accurate and reproducible. This method is especially applicable to all ranges of nitric acid and heavy metal ion concentration relevant to Purex process used for nuclear fuel reprocessing. The overall recovery of nitric acid is 98.9% with 1.2% relative standard deviation. Hydrazine content has also been determined in the same aliquot with a recovery of nitric acid is 99% with 2% relative standard deviation. The major advantage of the method is that generation of corrosive analytical wastes containing oxalate or sulphate is avoided. Valuable metals like uranium and plutonium can easily be recovered from analytical waste before final disposal. PMID:21726724

  4. Beer classification by means of a potentiometric electronic tongue.

    PubMed

    Cetó, Xavier; Gutiérrez-Capitán, Manuel; Calvo, Daniel; del Valle, Manel

    2013-12-01

    In this work, an electronic tongue (ET) system based on an array of potentiometric ion-selective electrodes (ISEs) for the discrimination of different commercial beer types is presented. The array was formed by 21 ISEs combining both cationic and anionic sensors with others with generic response. For this purpose beer samples were analyzed with the ET without any pretreatment rather than the smooth agitation of the samples with a magnetic stirrer in order to reduce the foaming of samples, which could interfere into the measurements. Then, the obtained responses were evaluated using two different pattern recognition methods, principal component analysis (PCA), which allowed identifying some initial patterns, and linear discriminant analysis (LDA) in order to achieve the correct recognition of sample varieties (81.9% accuracy). In the case of LDA, a stepwise inclusion method for variable selection based on Mahalanobis distance criteria was used to select the most discriminating variables. In this respect, the results showed that the use of supervised pattern recognition methods such as LDA is a good alternative for the resolution of complex identification situations. In addition, in order to show an ET quantitative application, beer alcohol content was predicted from the array data employing an artificial neural network model (root mean square error for testing subset was 0.131 abv).

  5. Protonation and Complexation of Isosaccharinic Acid with U(VI) and Fe(III) in Acidic Solutions: Potentiometric and Calorimetric Studies

    SciTech Connect

    Rao, Linfeng; Garnov, A Y.; Rai, Dhanpat; Xia, Yuanxian; Moore, R C.

    2004-12-01

    Protonation and complexation of {alpha}-isosaccharinic acid with U(VI) and Fe(III) have been studied in acidic solutions at t=25 C and I=1.0 mol dm{sup -3} NaClO{sub 4}. From the potentiometric titrations, the protonation constant of the carboxylate group is calculated to be 3.65 {+-} 0.05 and the data are consistent with the presence of three and four successive mononuclear complexes for U(VI) and Fe(III), respectively. The formation constants of the complexes, log {beta}{sub j}for the reactions of M+L=ML{sub j} where j=1-3 for U(VI), j=1-4 for Fe(III) and L stands for isosaccharinate, are determined to be 2.91 {+-} 0.15 (UO{sub 2}L), 5.37 {+-} 0.07 (UO{sub 2}L{sub 2}), 7.25 {+-} 0.18 (UO{sub 2}L{sub 3}), 5.06 {+-} 0.17 (FeL), 8.51 {+-} 0.15 (FeL{sub 2}), 11.00 {+-} 0.16 (FeL{sub 3}), and 12.99 {+-} 0.17 (FeL{sub 4}). From the calorimetric titrations, the enthalpy of protonation of the carboxylate group is determined to be -(7.94 {+-} 0.03)kJ mol{sup -1}, similar to that of other ?-hydroxycarboxylates. The enthalpies of complexation between U(VI) and isosaccharinate are quite small: {Delta} H{sub 1} = -(1.0 {+-} 1.0)kJ mol{sup -1}, {Delta} H{sub 2}=1.4 {+-} 1.8 kJ mol{sup -1} and {Delta} H{sub 3}=-(6.2 {+-} 3.0)kJ mol{sup -1}, typical of the interactions between carboxylates and hard-acid cations. The complexation between U(VI) and isosaccharinate is mainly entropy-driven. In comparison, the enthalpies of complexation for FeL{sub 3} and FeL{sub 4} are large and exothermic, contributing significantly to the stability of the complexes.

  6. Potentiometric determination of saccharin in dietary products using mercurous nitrate as titrant.

    PubMed

    Fo, O F; Moraes, A J; Dos Santos, G

    1993-05-01

    A rapid, precise and low cost method for saccharin determination in dietary products is proposed. Saccharin in several samples is potentiometrically titrated with mercurous nitrate solution using a silver wire coated with a metallic mercury film as the working electrode, and the end point was found using a Gran's plot. The detection limit of sodium saccharin was 0.5 mg/ml and the best pH range was from 2.0 to 3.5. Sucrose, glucose, aspartame, sodium cyclamate, sorbitol, fructose, benzoic acid, salicylic acid and lactose do not interfere even in significant amounts. The interference due to the presence of chloride and/or phosphate ions can be eliminated by previous solvent extraction of this sweetener. Recovery of saccharin from various dietary products gave from 95.2 to 103.2% of the label claim.

  7. Amperometric, Bipotentiometric, and Coulometric Titration.

    ERIC Educational Resources Information Center

    Stock, John T.

    1984-01-01

    Reviews literature on amperometric, bipotentiometric, and coulometric titration methods examining: apparatus and methodology; acid-base reactions; precipitation and complexing reactions (considering methods involving silver, mercury, EDTA or analogous reagents, and other organic compounds); and oxidation-reduction reactions (considering methods…

  8. Spectrophotometric, potentiometric, and gravimetric determination of lanthanides with peri-dihydroxynaphthindenone

    SciTech Connect

    Hassan, S.S.M.; Mahmoud, W.H.

    1982-02-01

    Sensitive and reasonably selective methods are described for the spectrophotometric, potentiometric, and gravimetric determination of lanthanides using peri-dihydroxynaphthindenone as a novel chromogenic and precipitating reagent. The reagent forms a stable 1:2 (metal:reagent) type of complex with light lanthanides at pH 2-7 in 1:1 ethanol-water mixture. Low metal concentrations (<10 ..mu..g/mL) develop colored species (lambda/sub max/ 580 to 590 nm, epsilon/sub max/ (4-6) x 10/sup 4/ L mol/sup -1/ cm/sup -1/) which obey Beer's law. Quantitative precipitation of the complexes from metal solutions of concentrations > 100 ..mu..g/mL permits both gravimetric quantitation by igniting the precipitates to the metal oxides and potentiometric titration of the excess reagent. Results with an average recovery of 98% (standard deviation 0.7%) are obtainable for 0.1 ..mu..g to 200 mg of all light lanthanides. Many foreign ions naturally occurring or frequently associated with lanthanides do not interfere or can be tolerated.

  9. Potentiometric Zinc Ion Sensor Based on Honeycomb-Like NiO Nanostructures

    PubMed Central

    Abbasi, Mazhar Ali; Ibupoto, Zafar Hussain; Hussain, Mushtaque; Khan, Yaqoob; Khan, Azam; Nur, Omer; Willander, Magnus

    2012-01-01

    In this study honeycomb-like NiO nanostructures were grown on nickel foam by a simple hydrothermal growth method. The NiO nanostructures were characterized by field emission electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM) and X-ray diffraction (XRD) techniques. The characterized NiO nanostructures were uniform, dense and polycrystalline in the crystal phase. In addition to this, the NiO nanostructures were used in the development of a zinc ion sensor electrode by functionalization with the highly selective zinc ion ionophore 12-crown-4. The developed zinc ion sensor electrode has shown a good linear potentiometric response for a wide range of zinc ion concentrations, ranging from 0.001 mM to 100 mM, with sensitivity of 36 mV/decade. The detection limit of the present zinc ion sensor was found to be 0.0005 mM and it also displays a fast response time of less than 10 s. The proposed zinc ion sensor electrode has also shown good reproducibility, repeatability, storage stability and selectivity. The zinc ion sensor based on the functionalized NiO nanostructures was also used as indicator electrode in potentiometric titrations and it has demonstrated an acceptable stoichiometric relationship for the determination of zinc ion in unknown samples. The NiO nanostructures-based zinc ion sensor has potential for analysing zinc ion in various industrial, clinical and other real samples. PMID:23202217

  10. Potentiometric determination of the total acidity of humic acids by constant-current coulometry.

    PubMed

    Palladino, Giuseppe; Ferri, Diego; Manfredi, Carla; Vasca, Ermanno

    2007-01-16

    A straightforward method for both the quantitative and the equilibrium analysis of humic acids in solution, based on the combination of potentiometry with coulometry, is presented. The method is based on potentiometric titrations of alkaline solutions containing, besides the humic acid sample, also NaClO(4) 1M; by means of constant current coulometry the analytical acidity in the solutions is increased with a high precision, until the formation of a solid phase occurs. Hence, the total acid content of the macromolecules may be determined from the e.m.f. data by using modified Gran plots or least-squares sum minimization programs as well. It is proposed to use the pK(w) value in the ionic medium as a check of the correctness of each experiment; this datum may be readily obtained as a side-result in each titration. Modelling acid-base equilibria of the HA samples analysed was also performed, on the basis of the buffer capacity variations occurring during each titration. The experimental data fit, having the least standard deviation, was obtained assuming a mixture of three monoprotic acids (HX, HY, HZ) having about the same analytical concentration, whose acid dissociation constants in NaClO(4) 1M at 25 degrees C were pK(HX)=3.9+/-0.2, pK(HY)=7.5+/-0.3, pK(HZ)=9.5+/-0.2, respectively. With the proposed method the handling of alkaline HA solutions, the titration with very dilute NaOH or HCl solutions and the need for the availability of very small volumes of titrant to be added by microburettes may be avoided.

  11. Determination of the phenolic-group capacities of humic substances by non-aqueous titration technique.

    PubMed

    Kirishima, Akira; Ohnishi, Takashi; Sato, Nobuaki; Tochiyama, Osamu

    2009-07-15

    The phenolic-group capacities of five humic substances, such as, the Aldrich humic acid, the humic and fulvic acids extracted from a soil, the humic and fulvic acids extracted from a peat have been precisely determined by the non-aqueous potentiometric titration technique. The titration by KOH in the mixed solvent of DMSO:2-propanol:water=80:19.3:0.7 at [K(+)]=0.02 M enabled to measure the potential change in a wide range of pOH (=-log[OH(-)]), and thus to determine the capacities of phenolic groups which could not be precisely determined in the aqueous titration. The results of the titration revealed that the mean protonation constants of the phenolic groups were nearly the same for all humic substances and close to that of phenol in the same medium, indicating that each phenolic-group in the humic substances is rather isolated and is not electronically affected by other affecting groups in the humic macromolecule.

  12. Light-scattering study of polyelectrolyte complex formation between anionic and cationic nanogels in an aqueous salt-free system.

    PubMed

    Miyake, Masafumi; Ogawa, Kazuyoshi; Kokufuta, Etsuo

    2006-08-15

    We studied complex formation in an aqueous salt-free system (pH approximately 3 and at 25 degrees C) between nanogel particles having opposite charges. Anionic gel (AG) and cationic gel (CG) particles consist of lightly cross-linked N-isopropylacrylamide (NIPA) copolymers with 2-acrylamido-2-methylpropane sulfonic acid and with 1-vinylimidazole, respectively. The number of charges per particle was -4490 for AG and +20 300 for CG, as estimated from their molar masses (3.33 MD for AG and 11.7 MD for CG) by static light scattering (SLS) and their charge densities (1.35 mmol/g for AG and 1.74 mmol/g for CG) by potentiometric titration. The complexes were formed through the addition of AG to CG and vice versa using a turbidimetric titration technique. At the endpoint of the titration, the aggregate formed was a complex based upon stoichiometric charge neutralization: CG(n)()(+) + xAG(m)()(-) --> CG(n)()(+) (AG(m)()(-))(x)() where x = (n)()/(m)(). At different stages of the titration before the endpoint, the resulting complexes were examined in detail using dynamic light scattering, SLS, and electrophoretic light scattering (ELS). The main results are summarized as follows: (i) When AG with a hydrodynamic radius (R(h)) of 119 nm is added to CG (R(h) approximately 156 nm), the (R(h)) of the complex size decreases from 156 to 80 nm. (ii) In contrast to this (R(h)) change, the molar mass increases from 11.7 MD to 24 MD with increasing amounts of added AG. (iii) Upon addition of CG to AG, the complex formed has the same size ((R(h)) approximately 80 nm) and the same molar mass (55 +/- 2.5 MD) until 55 +/- 5% of AG has been consumed in the complexation. To understand these results, we used the following two models: the random model (RM), in which the added AG particles uniformly bind to all of the CG particles in the system via a strong electrostatic attraction, and the all-or-none model (AONM), in which part of the AG particles in the system preferably bind to the added CG

  13. Colorblindness and Titrations with Visual Indicators.

    ERIC Educational Resources Information Center

    Diehl, Harvey; And Others

    1985-01-01

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

  14. Titration of gold nanoparticles in phase extraction.

    PubMed

    Cheng, Han-Wen; Schadt, Mark J; Zhong, Chuan-Jian

    2015-12-01

    In the organic-aqueous phase transfer process of gold nanoparticles, there are two types of distinctive interfaces involving hydrophilic and hydrophobic ligands, the understanding of which is important for the design of functional nanomaterials for analytical/bioanalytical applications and the control over the nanoparticles' nanoactivity and nanotoxicity in different phases. This report describes new findings of an investigation of the quantitative aspect of ligand ion pairing at the capping monolayer structure that drives the phase extraction of gold nanoparticles. Alkanethiolate-capped gold nanoparticles of 8 nm diameter with high size monodispersity (RSD ∼ 5%) were first derivatized by a ligand place exchange reaction with 11-mercaptoundecanoic acid to form a mixed monolayer shell consisting of both hydrophobic (-CH3) and hydrophilic (-COOH) groups. It was followed by quantitative titration of the resulting nanoparticles with a cationic species (-NR4(+)) in a toluene phase, yielding ion pairing of -NR4(+) and -COO(-) on part of the capping monolayer. Analysis of the phase extraction allowed a quantitative determination of the percentage of ion pairing and structural changes in the capping monolayer on the nanoparticles. The results, along with morphological characterization, are discussed in terms of the interfacial structural changes and their implications on the rational design of surface-functionalized nanoparticles and fine tuning of the interfacial reactivity. PMID:26523548

  15. Titration of gold nanoparticles in phase extraction.

    PubMed

    Cheng, Han-Wen; Schadt, Mark J; Zhong, Chuan-Jian

    2015-12-01

    In the organic-aqueous phase transfer process of gold nanoparticles, there are two types of distinctive interfaces involving hydrophilic and hydrophobic ligands, the understanding of which is important for the design of functional nanomaterials for analytical/bioanalytical applications and the control over the nanoparticles' nanoactivity and nanotoxicity in different phases. This report describes new findings of an investigation of the quantitative aspect of ligand ion pairing at the capping monolayer structure that drives the phase extraction of gold nanoparticles. Alkanethiolate-capped gold nanoparticles of 8 nm diameter with high size monodispersity (RSD ∼ 5%) were first derivatized by a ligand place exchange reaction with 11-mercaptoundecanoic acid to form a mixed monolayer shell consisting of both hydrophobic (-CH3) and hydrophilic (-COOH) groups. It was followed by quantitative titration of the resulting nanoparticles with a cationic species (-NR4(+)) in a toluene phase, yielding ion pairing of -NR4(+) and -COO(-) on part of the capping monolayer. Analysis of the phase extraction allowed a quantitative determination of the percentage of ion pairing and structural changes in the capping monolayer on the nanoparticles. The results, along with morphological characterization, are discussed in terms of the interfacial structural changes and their implications on the rational design of surface-functionalized nanoparticles and fine tuning of the interfacial reactivity.

  16. Potentiometric and ³¹P NMR studies on inositol phosphates and their interaction with iron(III) ions.

    PubMed

    Sala, Martin; Makuc, Damjan; Kolar, Jana; Plavec, Janez; Pihlar, Boris

    2011-03-01

    Potentiometric, conductometric and ³¹P NMR titrations have been applied to study interactions between myo-inositol hexakisphosphate (phytic acid), (±)-myo-inositol 1,2,3,5-tetrakisphosphate and (±)-myo-inositol 1,2,3-trisphosphate with iron(III) ions. Potentiometric and conductometric titrations of myo-inositol phosphates show that addition of iron increases acidity and consumption of hydroxide titrant. By increasing the Fe(III)/InsP(6) ratio (from 0.5 to 4) 3 mol of protons are released per 2 mol of iron(III). At first, phytates coordinate iron octahedrally between P2 and P1,3. The second coordination site represents P5 and neighbouring P4,6 phosphate groups. Complexation is accompanied with the deprotonation of P1,3 and P4,6 phosphate oxygens. At higher concentration of iron(III) intermolecular P-O-Fe-O-P bonds trigger formation of a polymeric network and precipitation of the amorphous Fe(III)-InsP(6) aggregates. (31)P NMR titration data complement the above results and display the largest chemical shift changes at pD values between 5 and 10 in agreement with strong interactions between iron and myo-inositol phosphates. The differences in T(1) relaxation times of phosphorous atoms have shown that phosphate groups at positions 1, 2 and 3 are complexated with iron(III). The interactions between iron(III) ions and inositol phosphates depend significantly on the metal to ligand ratio and an attempt to coordinate more than two irons per InsP(6) molecule results in an unstable heterogeneous system.

  17. Fibrous polymer grafted magnetic chitosan beads with strong poly(cation-exchange) groups for single step purification of lysozyme.

    PubMed

    Bayramoglu, Gulay; Tekinay, Turgay; Ozalp, V Cengiz; Arica, M Yakup

    2015-05-15

    Lysozyme is an important polypetide used in medical and food applications. We report a novel magnetic strong cation exchange beads for efficient purification of lysozyme from chicken egg white. Magnetic chitosan (MCHT) beads were synthesized via phase inversion method, and then grafted with poly(glycidyl methacrylate) (p(GMA)) via the surface-initiated atom transfer radical polymerization (SI-ATRP). Epoxy groups of the grafted polymer, were modified into strong cation-exchange groups (i.e., sulfonate groups) in the presence of sodium sulfite. The MCTH and MCTH-g-p(GMA)-SO3H beads were characterized by ATR-FTIR, SEM, and VSM. The sulphonate groups content of the modified MCTH-g-p(GMA)-4 beads was found to be 0.53mmolg(-1) of beads by the potentiometric titration method. The MCTH-g-p(GMA)-SO3H beads were first used as an ion-exchange support for adsorption of lysozyme from aqueous solution. The influence of different experimental parameters such as pH, contact time, and temperature on the adsorption process was evaluated. The maximum adsorption capacity was found to be 208.7mgg(-1) beads. Adsorption of lysozyme on the MCTH-g-p(GMA)-SO3H beads fitted to Langmuir isotherm model and followed the pseudo second-order kinetic. More than 93% of the adsorbed lysozyme was desorbed using Na2CO3 solution (pH 11.0). The purity of the lysozyme was checked by HPLC and SDS gel electrophoresis. In addition, the MCTH-g-p(GMA)-SO3H beads prepared in this work showed promising potential for separation of various anionic molecules. PMID:25864009

  18. Potentiometric map of the Cockfield Aquifer in Mississippi, fall, 1980

    USGS Publications Warehouse

    Wasson, B.E.

    1981-01-01

    This potentiometric map of the Cockfield aquifer is the eleventh in a series of maps, prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources , Bureau of Land and Water Resources, delineating the potentiometric surfaces of the major aquifers in Mississippi. In the outcrop area of the Cockfield quifer the potentiometric surface is strongly affected by recharge from precipitation, by topography, and by drainage of the aquifer by streams. The potentiometric surface slopes downward generally to the west away from the area of outcrop and is strongly affected by large ground-water withdrawals in the Jackson and Greenville areas. Historically, water levels in or near the outcrop of the Cockfield aquifer have shown little or no long-term changes, but in much of the confined part of the aquifer during the past 20 years, water levels have declined from 1 to 2 feet per year. (USGS)

  19. Potentiometric Urea Biosensor Based on an Immobilised Fullerene-Urease Bio-Conjugate

    PubMed Central

    Saeedfar, Kasra; Heng, Lee Yook; Ling, Tan Ling; Rezayi, Majid

    2013-01-01

    A novel method for the rapid modification of fullerene for subsequent enzyme attachment to create a potentiometric biosensor is presented. Urease was immobilized onto the modified fullerene nanomaterial. The modified fullerene-immobilized urease (C60-urease) bioconjugate has been confirmed to catalyze the hydrolysis of urea in solution. The biomaterial was then deposited on a screen-printed electrode containing a non-plasticized poly(n-butyl acrylate) (PnBA) membrane entrapped with a hydrogen ionophore. This pH-selective membrane is intended to function as a potentiometric urea biosensor with the deposition of C60-urease on the PnBA membrane. Various parameters for fullerene modification and urease immobilization were investigated. The optimal pH and concentration of the phosphate buffer for the urea biosensor were 7.0 and 0.5 mM, respectively. The linear response range of the biosensor was from 2.31 × 10−3 M to 8.28 × 10−5 M. The biosensor's sensitivity was 59.67 ± 0.91 mV/decade, which is close to the theoretical value. Common cations such as Na+, K+, Ca2+, Mg2+ and NH4+ showed no obvious interference with the urea biosensor's response. The use of a fullerene-urease bio-conjugate and an acrylic membrane with good adhesion prevented the leaching of urease enzyme and thus increased the stability of the urea biosensor for up to 140 days. PMID:24322561

  20. Potentiometric responses of polymeric liquid membranes based on hydrophobic chelating agents to metal ions.

    PubMed

    Itoh, Y; Ueda, Y; Hirano, A; Sugawara, M; Tohda, K; Akaiwa, H; Umezawa, Y

    2001-05-01

    The effect of hydrophobicity of acidic chelating agents as sensing materials on the potentiometric responses of polymeric liquid membranes was investigated. The chelating agents tested were 8-quinolinol (HOx), dithizone (HDz), 1-(2-pyridylazo)-2-naphthol (PAN) and their alkylated analogues, 5-octyloxymethyl-8-quinolinol (HO8Q), di(phexylphenyl)thiocarbazone (C6HDz), 7-pentadecyloxy-1-(2-pyridylazo)-2-naphthol (C15PAN) and a series of N-alkylcarbonyl-N-phenylhydroxylamines (CnPHA, n = 3, 6, 9, 12). The distribution coefficients between membrane solvent and water were determined to evaluate the hydrophobicity of the agents. The potential-pH profiles of the membranes containing hydrophobic chelating agents demonstrated the generation of potentiometric responses, while less hydrophobic agents gave no response. A possible model for the generation of membrane potential is proposed. The charge separation is attained by the permselective uptake of metal cations by the chelating agent anion at membrane/solution interface, where the high hydrophobicity of the agent enables the anionic or deprotonated form of the agents to remain at the membrane/solution interface.

  1. Potentiometric electronic tongue-flow injection analysis system for the monitoring of heavy metal biosorption processes.

    PubMed

    Wilson, D; del Valle, M; Alegret, S; Valderrama, C; Florido, A

    2012-05-15

    An automated flow injection potentiometric (FIP) system with electronic tongue detection (ET) is used for the monitoring of biosorption processes of heavy metals on vegetable wastes. Grape stalk wastes are used as biosorbent to remove Cu(2+) ions in a fixed-bed column configuration. The ET is formed by a 5-sensor array with Cu(2+) and Ca(2+)-selective electrodes and electrodes with generic response to heavy-metals, plus an artificial neural network response model of the sensor's cross-response. The real-time monitoring of both the Cu(2+) and the cation exchanged and released (Ca(2+)) in the effluent solution is performed by using flow-injection potentiometric electronic tongue system. The coupling of the electronic tongue with automation features of the flow-injection system allows us to accurately characterize the Cu(2+) ion-biosorption process, through obtaining its breakthrough curves, and the profile of the Ca(2+) ion release. In parallel, fractions of the extract solution are analysed by spectroscopic techniques in order to validate the results obtained with the reported methodology. The sorption performance of grape stalks is also evaluated by means of well-established sorption models.

  2. Flow injection potentiometric determination of saccharin in dietary products with relocation of filtration unit.

    PubMed

    Fatibello-Filho, O; Nóbrega, J A; Moraes Guaritá-Santos, A J

    1994-05-01

    A flow injection potentiometric procedure for saccharin determination in dietary products is proposed. Saccharin is precipitated as mercurous saccharinate and the excess of the mercurous cation is potentiometrically measured using a silver wire coated with a mercury film as the working electrode. A filter unit is used to avoid contact between the precipitate and the electrode surface. With relocation in the flow manifold, the accumulated precipitate is removed on-line. Sucrose, glucose, aspartame, sodium cyclamate and sodium benzoate do not interfere when present in amounts similar to those observed in commercial products. Results are comparable with those obtained by UV-spectrophotometry and the correlation coefficient between methods is equal to 0.9930. A linear relationship between DeltaE (mV) and the logarithm of saccharin concentration was obtained in the saccharin concentration range 2 x 10(-3) - 1 x 10(-2)M. The sampling frequency is 60/hour and only 0.76 mg of Hg(2+)(2) is consumed in each determination.

  3. Simple PVC-PPy electrode for pH measurement and titrations.

    PubMed

    Masalles, C; Borrós, S; Viñas, C; Teixidor, F

    2002-02-01

    Cobaltabis(dicarbollide) [3,3'-Co(1,2-C2B9H11)](-)-doped polypyrrole (PPy) films have been prepared galvanostatically on glassy carbon electrodes in acetonitrile solution. The potential response behavior of the film of this new material has been investigated in some common pH buffers and in acid-base titrations. The potentiometric characteristics of the resulting films are indicative of a quasi-Nernstian response (approximately 50 mV/pH unit), a linearity range from pH 12 to 3 and correlation coefficients (r2) of approximately 0.98. The electrode is suitable for pH measurements and for monoprotic titrations of strong alkalis with strong acids, and weak bases with strong acids, but the long response time hinders the use of this electrode for multiprotic titrations. The time response has been dramatically improved by reducing the film thickness by using the template effect of a non-conducting polymer (PVC) cast over the graphite surface before PPy deposition. PPy polymerization occurs in the free channels of PVC leading to the formation of PPy wires. The morphological change of PPy does not affect the slope or linearity range. The response of the PVC-PPy electrochemical sensor is rapid and the sensor is easy to prepare, at low cost, and its performance is comparable with that of commercial glass electrodes. PMID:11939624

  4. Simple PVC-PPy electrode for pH measurement and titrations.

    PubMed

    Masalles, C; Borrós, S; Viñas, C; Teixidor, F

    2002-02-01

    Cobaltabis(dicarbollide) [3,3'-Co(1,2-C2B9H11)](-)-doped polypyrrole (PPy) films have been prepared galvanostatically on glassy carbon electrodes in acetonitrile solution. The potential response behavior of the film of this new material has been investigated in some common pH buffers and in acid-base titrations. The potentiometric characteristics of the resulting films are indicative of a quasi-Nernstian response (approximately 50 mV/pH unit), a linearity range from pH 12 to 3 and correlation coefficients (r2) of approximately 0.98. The electrode is suitable for pH measurements and for monoprotic titrations of strong alkalis with strong acids, and weak bases with strong acids, but the long response time hinders the use of this electrode for multiprotic titrations. The time response has been dramatically improved by reducing the film thickness by using the template effect of a non-conducting polymer (PVC) cast over the graphite surface before PPy deposition. PPy polymerization occurs in the free channels of PVC leading to the formation of PPy wires. The morphological change of PPy does not affect the slope or linearity range. The response of the PVC-PPy electrochemical sensor is rapid and the sensor is easy to prepare, at low cost, and its performance is comparable with that of commercial glass electrodes.

  5. pH-metric solubility. 3. Dissolution titration template method for solubility determination.

    PubMed

    Avdeef, A; Berger, C M

    2001-12-01

    The main objective of this study was to develop an effective potentiometric saturation titration protocol for determining the aqueous intrinsic solubility and the solubility-pH profile of ionizable molecules, with the specific aim of overcoming incomplete dissolution conditions, while attempting to shorten the data collection time. A modern theory of dissolution kinetics (an extension of the Noyes-Whitney approach) was applied to acid-base titration experiments. A thermodynamic method was developed, based on a three-component model, to calculate interfacial, diffusion-layer, and bulk-water reactant concentrations in saturated solutions of ionizable compounds perturbed by additions of acid/base titrant, leading to partial dissolution of the solid material. Ten commercial drugs (cimetidine, diltiazem hydrochloride, enalapril maleate, metoprolol tartrate, nadolol, propoxyphene hydrochloride, quinine hydrochloride, terfenadine, trovafloxacin mesylate, and benzoic acid) were chosen to illustrate the new titration methodology. It was shown that the new method is about 10 times faster in determining equilibrium solubility constants, compared to the traditional saturation shake-flask methods.

  6. Spectroscopic study on variations in illite surface properties after acid-base titration.

    PubMed

    Liu, Wen-xin; Coveney, R M; Tang, Hong-xiao

    2003-07-01

    FT-IR, Raman microscopy, XRD, 29Si and 27Al MAS NMR, were used to investigate changes in surface properties of a natural illite sample after acid-base potentiometric titration. The characteristic XRD lines indicated the presence of surface Al-Si complexes, preferable to Al(OH)3 precipitates. In the microscopic Raman spectra, the vibration peaks of Si-O and Al-O bonds diminished as a result of treatment with acid, then increased after hydroxide back titration. The varied ratio of signal intensity between (IV)Al and (VI)Al species in 27Al MAS NMR spectra, together with the stable BET surface area after acidimetric titration, suggested that edge faces and basal planes in the layer structure of illite participated in dissolution of structural components. The combined spectroscopic evidence demonstrated that the reactions between illite surfaces and acid-leaching silicic acid and aluminum ions should be considered in the model description of surface acid-base properties of the aqueous illite.

  7. Effects of alkyl chain length and solvents on thermodynamic dissociation constants of the ionic liquids with one carboxyl group in the alkyl chain of imidazolium cations.

    PubMed

    Chen, Yuehua; Wang, Huiyong; Wang, Jianji

    2014-05-01

    Thermodynamic dissociation constants of the Brønsted acidic ionic liquids (ILs) are important for their catalytic and separation applications. In this work, a series of imidazolium bromides with one carboxylic acid substitute group in their alkyl chain ([{(CH2)nCOOH}mim]Br, n = 1,3,5,7) have been synthesized, and their dissociation constants (pKa) at different ionic strengths have been determined in aqueous and aqueous organic solvents at 0.1 mole fraction (x) of ethanol, glycol, iso-propanol, and dimethyl sulfoxide by potentiometric titrations at 298.2 K. The standard thermodynamic dissociation constants (pKa(T)) of the ILs in these solvents were calculated from the extended Debye-Hückel equation. It was found that the pKa values increased with the increase of ionic strength of the media and of the addition of organic solvent in water. The pKa(T) values also increased with the increase of the alkyl chain length of cations of the ILs. In addition, the effect of solvent nature on pKa(T) values is interpreted from solvation of the dissociation components and their Gibbs energy of transfer from water to aqueous organic solutions. PMID:24720707

  8. Effects of alkyl chain length and solvents on thermodynamic dissociation constants of the ionic liquids with one carboxyl group in the alkyl chain of imidazolium cations.

    PubMed

    Chen, Yuehua; Wang, Huiyong; Wang, Jianji

    2014-05-01

    Thermodynamic dissociation constants of the Brønsted acidic ionic liquids (ILs) are important for their catalytic and separation applications. In this work, a series of imidazolium bromides with one carboxylic acid substitute group in their alkyl chain ([{(CH2)nCOOH}mim]Br, n = 1,3,5,7) have been synthesized, and their dissociation constants (pKa) at different ionic strengths have been determined in aqueous and aqueous organic solvents at 0.1 mole fraction (x) of ethanol, glycol, iso-propanol, and dimethyl sulfoxide by potentiometric titrations at 298.2 K. The standard thermodynamic dissociation constants (pKa(T)) of the ILs in these solvents were calculated from the extended Debye-Hückel equation. It was found that the pKa values increased with the increase of ionic strength of the media and of the addition of organic solvent in water. The pKa(T) values also increased with the increase of the alkyl chain length of cations of the ILs. In addition, the effect of solvent nature on pKa(T) values is interpreted from solvation of the dissociation components and their Gibbs energy of transfer from water to aqueous organic solutions.

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

    USGS Publications Warehouse

    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.

  10. Risks and Benefits of Rapid Clozapine Titration.

    PubMed

    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.

  11. Determination of the acid dissociation constant of the biosurfactant monorhamnolipid in aqueous solution by potentiometric and spectroscopic methods.

    PubMed

    Lebrón-Paler, Ariel; Pemberton, Jeanne E; Becker, Bridget A; Otto, William H; Larive, Cynthia K; Maier, Raina M

    2006-11-15

    The acid dissociation constant in water for a monorhamnolipid mixture extracted from Pseudomonas aeruginosa ATCC 9027 has been determined using potentiometry and two spectroscopic approaches at concentrations below and above the critical micelle concentration (cmc). Potentiometric titrations resulted in pKa values ranging from 4.28 +/- 0.16 to 5.50 +/- 0.06 depending on concentration. 1H NMR spectrochemical titrations at concentrations below the cmc revealed a pKa value of 4.39 +/- 0.06. ATR-FT-IR spectrochemical titrations on solutions well above the cmc gave a pKa value of 4.84 +/- 0.05. The value of 4.28 for the free rhamnolipid molecule for concentrations below the cmc differs markedly from that reported previously. However, the pKa of 5.50 for surface-adsorbed and solution aggregates correlates closely to that previously reported. Differences in these pKa values are rationalized in terms of the pH- and concentration-dependent aggregation behavior of rhamnolipids in aqueous solution.

  12. Logarithmic diagrams in acid-base titrations and estimation of titration errors.

    PubMed

    Wänninen, E

    1980-01-01

    The use of a logarithmic diagram for the estimation of the pH-value at the equivalence point and the titration error when a solution containing one or two acids is titrated with standard alkali is described.

  13. Prediction of aluminum, uranium, and co-contaminants precipitation and adsorption during titration of acidic sediments.

    PubMed

    Tang, Guoping; Luo, Wensui; Watson, David B; Brooks, Scott C; Gu, Baohua

    2013-06-01

    Batch and column recirculation titration tests were performed with contaminated acidic sediments. A generic geochemical model was developed combining precipitation, cation exchange, and surface complexation reactions to describe the observed pH and metal ion concentrations in experiments with or without the presence of CO2. Experimental results showed a slow pH increase due to strong buffering by Al hydrolysis and precipitation and CO2 uptake. The cation concentrations generally decreased at higher pH than those observed in previous tests without CO2. Using amorphous Al(OH)3 and basaluminite precipitation reactions and a cation exchange selectivity coefficient K(Na\\Al) of 0.3, the model approximately described the observed (1) pH titration curve, (2) Ca, Mg, and Mn concentration by cation exchange, and (3) U concentrations by surface complexation with Fe hydroxides at pH < 5 and with liebigite (Ca2UO2(CO3)3·10H2O) precipitation at pH > 5. The model indicated that the formation of aqueous carbonate complexes and competition with carbonate for surface sites could inhibit U and Ni adsorption and precipitation. Our results suggested that the uncertainty in basaluminite solubility is an important source of prediction uncertainty and ignoring labile solid phase Al underestimates the base requirement in titration of acidic sediments.

  14. Prediction of aluminum, uranium, and co-contaminants precipitation and adsorption during titration of acidic sediments.

    PubMed

    Tang, Guoping; Luo, Wensui; Watson, David B; Brooks, Scott C; Gu, Baohua

    2013-06-01

    Batch and column recirculation titration tests were performed with contaminated acidic sediments. A generic geochemical model was developed combining precipitation, cation exchange, and surface complexation reactions to describe the observed pH and metal ion concentrations in experiments with or without the presence of CO2. Experimental results showed a slow pH increase due to strong buffering by Al hydrolysis and precipitation and CO2 uptake. The cation concentrations generally decreased at higher pH than those observed in previous tests without CO2. Using amorphous Al(OH)3 and basaluminite precipitation reactions and a cation exchange selectivity coefficient K(Na\\Al) of 0.3, the model approximately described the observed (1) pH titration curve, (2) Ca, Mg, and Mn concentration by cation exchange, and (3) U concentrations by surface complexation with Fe hydroxides at pH < 5 and with liebigite (Ca2UO2(CO3)3·10H2O) precipitation at pH > 5. The model indicated that the formation of aqueous carbonate complexes and competition with carbonate for surface sites could inhibit U and Ni adsorption and precipitation. Our results suggested that the uncertainty in basaluminite solubility is an important source of prediction uncertainty and ignoring labile solid phase Al underestimates the base requirement in titration of acidic sediments. PMID:23641798

  15. Potentiometric membrane sensor for the selective determination of pethidine in pharmaceutical preparations and biological fluids.

    PubMed

    Shalaby, Abdalla; El-Tohamy, Maha; El-Maamly, Magda; Aboul-Enein, Hassan Y

    2007-10-01

    The construction and general performance characteristics of a novel potentiometric PVC membrane sensor based on pethidine-phosphomolybdate as electroactive material for the determination of pethidine are described. This sensor exhibits fast, stable and near-Nernstain response 55.24 +/- 0.1, over the concentration range 1.10(-2)-1.10(-5)M for pethidine-phosphomolybdate over pH 2-7. No interferences are caused by many organic, inorganic cations, alkaloids and amino acids. The sensor proved useful for determining pethidine in pure forms, pharmaceutical injections and monitoring the content uniformity assay of ampoules. The designed sensor also show good accuracy for the determination of pethidine in biological fluids.

  16. Isothermal titration calorimetry of RNA.

    PubMed

    Salim, Nilshad N; Feig, Andrew L

    2009-03-01

    Isothermal titration calorimetry (ITC) is a fast and robust method to study the physical basis of molecular interactions. A single well-designed experiment can provide complete thermodynamic characterization of a binding reaction, including K(a), DeltaG, DeltaH, DeltaS and reaction stoichiometry (n). Repeating the experiment at different temperatures allows determination of the heat capacity change (DeltaC(P)) of the interaction. Modern calorimeters are sensitive enough to probe even weak biological interactions making ITC a very popular method among biochemists. Although ITC has been applied to protein studies for many years, it is becoming widely applicable in RNA biochemistry as well, especially in studies which involve RNA folding and RNA interactions with small molecules, proteins and with other RNAs. This review focuses on best practices for planning, designing and executing effective ITC experiments when one or more of the reactants is an RNA. PMID:18835447

  17. Potentiometric sensors enabling fast screening of the benign prostatic hyperplasia drug alfuzosin in pharmaceuticals, urine and serum.

    PubMed

    Gupta, Vinod K; Singh, Ashok K; Gupta, Barkha

    2007-08-01

    The construction and characterization of potentiometric membrane electrodes are described for the quantification of alfuzosin, a drug used in a mono- and combined therapy of benign prostatic hyperplasia (BPH). The membranes of these electrodes consist of alfuzosin hydrochloride-tetraphenyl borate, (Az-TPB), chlorophenyl borate (Az-ClPB), and phosphotungstate (Az(3)-PT) ion associations as molecular recognition reagent dispersed in PVC matrix with dioctylpthalate as plasticizer. The performance characteristics of these electrodes, which were evaluated according to IUPAC recommendations, revealed a fast, stable and liner response for alfuzosin over the concentration ranges of 8.3 x 10(-6) to 1.0 x 10(-2) M, 3.8 x 10(-6) to 1.0 x 10(-2) M, 7.5 x 10(-7) to 1.0 x 10(-2) M AzCl with cationic slopes of 57.0, 56.0 and 58.5 mV/decade, respectively. The solubility product of the ion-pair and the formation constant of the precipitation reaction leading to the ion-pair formation were determined conductometrically. The electrodes, fully characterized in terms of composition, life span and usable pH range, were applied to the potentiometric determination of alfuzosin hydrochloride ion in different pharmaceutical preparations and biological fluids without any interference from excipients or diluents commonly used in drug formulations. The potentiometric method was also used in the determination of alfuzosin hydrochloride in pharmaceutical preparations in four batches with different expiration dates. Validation of the method showed suitability of the proposed electrodes for use in the quality control assessment of alfuzosin hydrochloride. This potentiometric method offers the advantages of high-throughput determination, simplicity, accuracy, automation feasibility, and applicability to turbid and colored sample solutions. PMID:17979639

  18. A Tabular Approach to Titration Calculations

    ERIC Educational Resources Information Center

    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…

  19. The Ca(2+)-EDTA chelation as standard reaction to validate Isothermal Titration Calorimeter measurements (ITC).

    PubMed

    Ràfols, Clara; Bosch, Elisabeth; Barbas, Rafael; Prohens, Rafel

    2016-07-01

    A study about the suitability of the chelation reaction of Ca(2+)with ethylenediaminetetraacetic acid (EDTA) as a validation standard for Isothermal Titration Calorimeter measurements has been performed exploring the common experimental variables (buffer, pH, ionic strength and temperature). Results obtained in a variety of experimental conditions have been amended according to the side reactions involved in the main process and to the experimental ionic strength and, finally, validated by contrast with the potentiometric reference values. It is demonstrated that the chelation reaction performed in acetate buffer 0.1M and 25°C shows accurate and precise results and it is robust enough to be adopted as a standard calibration process. PMID:27154686

  20. The Ca(2+)-EDTA chelation as standard reaction to validate Isothermal Titration Calorimeter measurements (ITC).

    PubMed

    Ràfols, Clara; Bosch, Elisabeth; Barbas, Rafael; Prohens, Rafel

    2016-07-01

    A study about the suitability of the chelation reaction of Ca(2+)with ethylenediaminetetraacetic acid (EDTA) as a validation standard for Isothermal Titration Calorimeter measurements has been performed exploring the common experimental variables (buffer, pH, ionic strength and temperature). Results obtained in a variety of experimental conditions have been amended according to the side reactions involved in the main process and to the experimental ionic strength and, finally, validated by contrast with the potentiometric reference values. It is demonstrated that the chelation reaction performed in acetate buffer 0.1M and 25°C shows accurate and precise results and it is robust enough to be adopted as a standard calibration process.

  1. Determination of Poly(Diallyldimethylammonium Chloride) via Spectrophotometric Titration with Coomassie Brilliant Blue G Dye.

    PubMed

    Shyichuk, Alexander; Ziółkowska, Dorota; Lamkiewicz, Jan

    2016-02-01

    Poly(diallyldimethylammonium chloride) (PDDA) is used as organic coagulant in water purification and auxiliary agent in paper production. Determination of PDDA in aqueous solutions is carried out usually by means of polyelectrolyte titration using streaming current detector or o-Toluidine Blue dye for endpoint recognition. The proposed method of PDDA assay takes advantage of Coomassie Brilliant Blue G dye having strong affinity to cationic macromolecules. Titration of PDDA solution with the dye is carried out measuring absorbance at 585 nm. Inflection points of the obtained zigzag photometric curves have good repeatability provided that titration rate is low enough to attain endpoint for 1 hour or more. The method assures rectilinear calibration (R² = 0.999 5) in the broad range of PDDA concentrations from 0.3 to 9.6 mg · dm⁻³.

  2. Potentiometric Biosensor for Studying Hydroquinone Cytotoxicity in vitro

    PubMed Central

    Wang, Yanyan; Chen, Qiang; Zeng, Xiangqun

    2009-01-01

    Many processes in living cells have electrochemical characteristics that are suitable for measurement by potentiometric biosensors. Potentiometric biosensors allow non invasive, real-time monitoring of the extracellular environment changes by measuring the potential at cell/sensor interface. This can be used as an indicator for overall cell cytotoxicity. The present work employs a potentiometric sensor array to investigate the cytotoxicity of hydroquinone to cultured mammalian V79 cells. Various electrode substrates (Au, PPy-HQ and PPy-PS) used for cell growth were designed and characterized. The controllable release of hydroquinone from PPy substrates was studied. Our results showed that hydroquinone exposure affected cell proliferation and delayed cell growth and attachment in a dose-dependent manner. Additionally, we have shown that exposure of V79 cells to hydroquinone at low doses (i.e 5μM) for more than 15 hours allows V79 cells to gain enhanced adaptability to survive exposure to high toxic HQ doses afterwards. Compared with traditional methods, the potentiometric biosensor not only provides non-invasive and real time monitoring of the cellular reactions but also is more sensitive for in vitro cytotoxicity study. By real time and non-invasive monitoring of the extracellular potential in vitro, the potentiometric sensor system represents a promising biosensor system for drug discovery. PMID:19926470

  3. High affinity of water-soluble cryptophanes for cesium cations.

    PubMed

    Brotin, Thierry; Montserret, Roland; Bouchet, Aude; Cavagnat, Dominique; Linares, Mathieu; Buffeteau, Thierry

    2012-01-20

    Exceptionally high affinity for cesium cations was achieved in aqueous solution using two enantiopure cryptophanes. Complexation of cesium was evidenced by (133)Cs NMR spectroscopy and by electronic circular dichroism (ECD). Binding constants as high as 6 × 10(9) M(-1) have been measured by isothermal titration calorimetry (ITC). Very strong complexation of rubidium cations (K ~10(6) M(-1)) has also been measured. Chiral hosts allowed the detection of the two cations at low concentrations (μM) using ECD.

  4. Direct potentiometric determination of diastase activity in honey.

    PubMed

    Sak-Bosnar, Milan; Sakač, Nikola

    2012-11-15

    A novel method for the determination of diastase activity is reported. The method is based on a direct potentiometric measurement of triiodide ion that is released when a starch-triiodide complex is hydrolysed by honey diastase. The increase of free triiodide ion concentration in a sample is found to be directly proportional to the diastase activity of the sample. A response mechanism of the platinum redox electrode is proposed, allowing a calculation of the diastase activity factor (F). The sensor and analyte parameters, including F, were obtained by least squares fitting of potentiometric data using the optimisation function of the Solver add-in of Microsoft Excel. The values of F obtained by the new direct potentiometric method were compared with those obtained using the standard Phadebas method (DN values), and the two values were found to agree within experimental error. Finally, the diastase activity of nine varieties of honey was determined using the novel method developed here.

  5. Conceptual Models of the Potentiometric Surface at Yucca Mountain, NV

    NASA Astrophysics Data System (ADS)

    Hill, M.; Winterle, J.; Farrell, D.; Sims, D.; Bertetti, P.

    2002-05-01

    The U.S. Department of Energy (DOE) is evaluating Yucca Mountain (YM) Nevada, as the potential site for geologic disposal of high-level nuclear waste (HLW). If approved, the repository would be located approximately 244 to 305 m (800-1,000 ft) above the present water table. Total-system performance assessments that consider both engineered and geologic barrier systems are one method used to evaluate whether the potential repository can meet regulatory requirements. Flow paths interpreted from the potentiometric surface in the saturated zone beneath YM are incorporated into the performance assessment codes. Therefore, it is important that our understanding of the potentiometric surface is sufficient to assess potential repository performance. The addition of new water-level data from the Nye County Early Warning Drilling Program (EWDP) has helped constrain the conceptual model of the site-scale potentiometric surface at YM, specifically in the southern portion of the site along U.S. Highway 95. The EWDP was initiated in 1998, with the purpose of identifying the flow paths for contaminants should they egress from the proposed repository into the groundwater system. A revised site-scale potentiometric surface map for YM utilizing the new water-level data obtained from the EWDP is presented. The revised site-scale potentiometric surface map and other existing site-scale potentiometric surface maps interpreted from water-level data, are compared to structural, geophysical, and chemical data to evaluate whether consensus exists among the different data types concerning groundwater flow at YM. This abstract documents work performed in part by the Center for Nuclear Waste Regulatory Analyses under contract No. NRC-02-97-009. The report is an independent product and does not reflect the regulatory position of the NRC.

  6. Micro coulometric titration in a liquid drop.

    PubMed

    Kanyanee, Tinakorn; Fuekhad, Pongwasin; Grudpan, Kate

    2013-10-15

    Miniaturized coulometric titration in a liquid drop has been investigated. Assays of ascorbic acid and thiosulfate with iodine titration were chosen as models. Constant volumes of falling liquid drops containing sample or reagent are manipulated via gravimetrical force to move along a slope hydrophobic path and directed to stop or to move out from an electrode. Such manipulation is useful for delivery of sample and reagents, in a way of flow without tubing. Electrochemical generation of titrant, in this case, iodine, is started at the electrode and micro coulometric titration can be performed in a drop by applying constant current. Timing in the titration can be made via naked eye with a stopwatch or via recording with a webcam camera connecting to a computer to detect the change due to the blue color complex of the excess iodine and starch.

  7. Micro coulometric titration in a liquid drop.

    PubMed

    Kanyanee, Tinakorn; Fuekhad, Pongwasin; Grudpan, Kate

    2013-10-15

    Miniaturized coulometric titration in a liquid drop has been investigated. Assays of ascorbic acid and thiosulfate with iodine titration were chosen as models. Constant volumes of falling liquid drops containing sample or reagent are manipulated via gravimetrical force to move along a slope hydrophobic path and directed to stop or to move out from an electrode. Such manipulation is useful for delivery of sample and reagents, in a way of flow without tubing. Electrochemical generation of titrant, in this case, iodine, is started at the electrode and micro coulometric titration can be performed in a drop by applying constant current. Timing in the titration can be made via naked eye with a stopwatch or via recording with a webcam camera connecting to a computer to detect the change due to the blue color complex of the excess iodine and starch. PMID:24054589

  8. Data acquisition system for ion-selective potentiometric sensors

    NASA Astrophysics Data System (ADS)

    Filipkowski, Andrzej; Ogrodzki, Jan; Opalski, Leszek J.; Rybaniec, Radoslaw; Wieczorek, Piotr Z.

    2009-06-01

    The paper presents an idea and directives on construction of a measurement system for estimation of ions' concentration in water. System presented in paper has been fully designed and manufactured in Warsaw University of Technology in Institute of Electronic Systems. The measurement system works with cheap ion-selective potentiometric sensors. System allows for potentiometric, transient response and voltamperometric measurements. Data fusion method has been implemented in the system to increase the estimation's accuracy. Presented solution contains of many modern electronic elements like 32bit ARM microcontroller, precise operational amplifiers and some hydraulics subsystems essential for chemical measurements.

  9. Gasometric titration for dimethylaluminum chloride analysis.

    PubMed

    Wang, Lin; Maligres, Peter; Eckenroad, Kyle; Simmons, Bryon

    2016-06-01

    A gasometric titration method was developed to quantitate active alkylaluminum content in dimethylaluminum chloride solution to perform the stoichiometry calculation for the reaction charge. The procedure was reproducible with good precision, and the results showed good correlation with ICP-MS method. The gasometric titration is a simple, inexpensive alternative to analysis via ICP-MS which provides more selective analysis of methylaluminum species without the need for inertion.

  10. Novel potentiometric sensor for monitoring beryllium based on naphto-9-crown-3.

    PubMed

    Ganjali, Mohammad Reza; Daftari, Azadeh; Faal-Rastegar, Majid; Moghimi, Abolghasem

    2003-03-01

    A novel poly(vinyl chloride) (PVC) membrane electrode based on naphto-9-crown-3 was prepared and tested for the selective detection of beryllium ions. A suitable lipophilicity of the carrier and appropriate coordination ability were found to be essential for designing an electrode with good response characteristics. A PVC membrane with 9% naphtho-9-crown-3 carrier, 58% o-NPOE plasticizer, 3% tetraphenylborate anionic excluder and 30% poly(vinyl chloride) satisfied these requirements. The proposed sensor displayed a linear response to beryllium over a wide concentration range of 1.0 x 10(-1)-8.0 x 10(-6) M with a Nernstian slope of 29.5 mV per decade. The electrode showed very short response time (<15 s) and could be used in the pH range 3.5-9.0. The selectivity coefficient for alkali, alkaline earth, transition and heavy metal ions was smaller than 4.0 x 10(-4). The sensor was successfully used as an indicator electrode in the potentiometric titration of Be2+ with EDTA. The proposed Be(II) sensor was also used for the determination of Be2+ ions in binary mixtures.

  11. Potentiometric sensors for the determination of trifluoperazine hydrochloride in pharmaceutical preparations.

    PubMed

    Hassan, Ahmed K; Ameen, Suhaam T; Saad, Bahruddin; Al-Aragi, Suad M

    2009-11-01

    Trifluoperazine is widely used in the treatment of psychotic patients for its neuroleptic and antidepressive action. In this study, the construction, evaluation and application of new potentiometric sensors for trifluoperazine hydrochloride (TFPH) are described. The sensing membranes incorporated either ion-pair complexes of the trifluoperazine cation and phosphotungstic acid (PTA) or phosphomolybdic acid (PMA) or sodium tetraphenyl borate (NaTPB) as electroactive materials in poly(vinyl chloride) matrix membrane. The plasticizers used were di-n-butyl phthalate (DBPH) and tri-n-butyl phosphate (TBP). After a series of experiments, the best electrodes were based on PTA or PMA as electroactive materials and DBPH as plasticizer. A linear concentration range between 1 x 10(-5)-1 x 10(-2) M with a near Nernstian slope of 28.43 and 32.11 mV decade(-1), respectively, was obtained. The electrodes were characterized in terms of the composition, usable pH range, life span and response time. The selectivity coefficient values were calculated for different inorganic cations and sugars. Validation of the method shows the suitability of the electrodes for the determination of TFPH in pharmaceutical formulations.

  12. Potentiometric titration for determining the composition and stability of metal(II) alginates and pectinates in aqueous solutions

    NASA Astrophysics Data System (ADS)

    Kaisheva, N. Sh.; Kaishev, A. Sh.

    2015-07-01

    The compositions and stabilities of Cu2+, Mn2+, Pb2+, Ca2+, Zn2+, Cd2+, Co2+, and Ni2+ alginates and pectinates are determined in aqueous solutions via titrimetry and potentiometry with calculations performed using Bjerrum's method, the curve intersection technique, and the equilibrium shift method. It is found that the interaction between Cu2+ and polyuronides is a stepwise process and, depending on the ligand concentration and the method of determination, Cu2+ alginate can be characterized by its ML, ML2, and ML3 compositions (where M is the metal ion and L is the structural unit of polyuronide) and stability constants logβ = 2.65, 5.00-5.70, and 7.18-7.80, respectively. The compositions of Cu2+ pectinates are ML and ML2 with logβ = 3.00 and 7.64-7.94, respectively. It is concluded that Pb2+, Ca2+, Mn2+, Zn2+, Cd2+, Co2+, and Ni2+ ions form only alginates and pectinates of ML2 composition with logβ values of 3.45 (Pb2+ alginate), 2.20 (Ca2+ alginate), 1.06 (Mn2+ alginate), 3.51 (Pb2+ pectinate), 2.35 (Ca2+ pectinate), and 1.24 (Mn2+ pectinate). The pectinates are shown to be more stable than the alginates, the most stable compounds being those formed by polyuronides and Cu2+. The least stable are those with Mn2+.

  13. Convergence-optimized procedure for applying the NICA-Donnan model to potentiometric titrations of humic substances.

    PubMed

    Lenoir, Thomas; Matynia, Anthony; Manceau, Alain

    2010-08-15

    Despite the high success of the NICA-Donnan (N-D) model to describe the interaction of protons and metal ions with natural organic matter, the large number of fit parameters is a major hindrance to its capacity to provide unique numerical solutions. This well-known difficulty is reflected in the unusually low value of the generic proton binding constant for carboxylic-type groups of fulvic acid (pK(H1) = 2.34), and to some extent of humic acid (2.93), and by the considerable covariance of the other generic N-D parameters. In some studies, the number of parameters obtained by regression is reduced by estimating some values independently with other techniques. Alternatively, the applicability of the model can be improved by devising a rigorous simulation procedure, which constrains the model-fit to converge toward chemically and physically realistic values. A procedure based on three successive iterations is proposed, and the solution is shown to be stable and invariant with the initial set of parameter values. The new generic parameters, in particular pK(H1)(FA) = 3.54 and pK(H1)(HA) = 3.87, derived from the same data set as the previous generic parameters, are in better agreement with literature data.

  14. Polyelectrolyte assisted charge titration spectrometry: Applications to latex and oxide nanoparticles.

    PubMed

    Mousseau, F; Vitorazi, L; Herrmann, L; Mornet, S; Berret, J-F

    2016-08-01

    The electrostatic charge density of particles is of paramount importance for the control of the dispersion stability. Conventional methods use potentiometric, conductometric or turbidity titration but require large amount of samples. Here we report a simple and cost-effective method called polyelectrolyte assisted charge titration spectrometry or PACTS. The technique takes advantage of the propensity of oppositely charged polymers and particles to assemble upon mixing, leading to aggregation or phase separation. The mixed dispersions exhibit a maximum in light scattering as a function of the volumetric ratio X, and the peak position XMax is linked to the particle charge density according to σ∼D0XMax where D0 is the particle diameter. The PACTS is successfully applied to organic latex, aluminum and silicon oxide particles of positive or negative charge using poly(diallyldimethylammonium chloride) and poly(sodium 4-styrenesulfonate). The protocol is also optimized with respect to important parameters such as pH and concentration, and to the polyelectrolyte molecular weight. The advantages of the PACTS technique are that it requires minute amounts of sample and that it is suitable to a broad variety of charged nano-objects. PMID:27153216

  15. A new method for determining the acid number of biodiesel based on coulometric titration.

    PubMed

    Barbieri Gonzaga, Fabiano; Pereira Sobral, Sidney

    2012-08-15

    A new method is proposed for determining the acid number (AN) of biodiesel using coulometric titration with potentiometric detection, basically employing a potentiostat/galvanostat and an electrochemical cell containing a platinum electrode, a silver electrode, and a combination pH electrode. The method involves a sequential application of a constant current between the platinum (cathode) and silver (anode) electrodes, followed by measuring the potential of the combination pH electrode, using an isopropanol/water mixture as solvent and LiCl as the supporting electrolyte. A preliminary evaluation of the new method, using acetic acid for doping a biodiesel sample, showed an average recovery of 100.1%. Compared to a volumetric titration-based method for determining the AN of several biodiesel samples (ranging from about 0.18 to 0.95 mg g(-1)), the new method produced statistically similar results with better repeatability. Compared to other works reported in the literature, the new method presented an average repeatability up to 3.2 times better and employed a sample size up to 20 times smaller.

  16. Polyelectrolyte assisted charge titration spectrometry: Applications to latex and oxide nanoparticles.

    PubMed

    Mousseau, F; Vitorazi, L; Herrmann, L; Mornet, S; Berret, J-F

    2016-08-01

    The electrostatic charge density of particles is of paramount importance for the control of the dispersion stability. Conventional methods use potentiometric, conductometric or turbidity titration but require large amount of samples. Here we report a simple and cost-effective method called polyelectrolyte assisted charge titration spectrometry or PACTS. The technique takes advantage of the propensity of oppositely charged polymers and particles to assemble upon mixing, leading to aggregation or phase separation. The mixed dispersions exhibit a maximum in light scattering as a function of the volumetric ratio X, and the peak position XMax is linked to the particle charge density according to σ∼D0XMax where D0 is the particle diameter. The PACTS is successfully applied to organic latex, aluminum and silicon oxide particles of positive or negative charge using poly(diallyldimethylammonium chloride) and poly(sodium 4-styrenesulfonate). The protocol is also optimized with respect to important parameters such as pH and concentration, and to the polyelectrolyte molecular weight. The advantages of the PACTS technique are that it requires minute amounts of sample and that it is suitable to a broad variety of charged nano-objects.

  17. A digital image-based method for determining of total acidity in red wines using acid-base titration without indicator.

    PubMed

    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.

  18. Potentiometric sensors based on fluorous membranes doped with highly selective ionophores for carbonate.

    PubMed

    Chen, Li D; Mandal, Debaprasad; Pozzi, Gianluca; Gladysz, John A; Bühlmann, Philippe

    2011-12-28

    Manganese(III) complexes of three fluorophilic salen derivatives were used to prepare ion-selective electrodes (ISEs) with ionophore-doped fluorous sensing membranes. Because of their extremely low polarity and polarizability, fluorous media are not only chemically very inert but also solvate potentially interfering ions poorly, resulting in a much improved discrimination of such ions. Indeed, the new ISEs exhibited selectivities for CO(3)(2-) that exceed those of previously reported ISEs based on nonfluorous membranes by several orders of magnitude. In particular, the interference from chloride and salicylate was reduced by 2 and 6 orders of magnitude, respectively. To achieve this, the selectivities of these ISEs were fine-tuned by addition of noncoordinating hydrophobic ions (i.e., ionic sites) into the sensing membranes. Stability constants of the anion-ionophore complexes were determined from the dependence of the potentiometric selectivities on the charge sign of the ionic sites and the molar ratio of ionic sites and the ionophore. For this purpose, a previously introduced fluorophilic tetraphenylborate and a novel fluorophilic cation with a bis(triphenylphosphoranylidene)ammonium group, (R(f6)(CH(2))(3))(3)PN(+)P(R(f6)(CH(2))(3))(3), were utilized (where R(f6) is C(6)F(13)). The optimum CO(3)(2-) selectivities were found for sensing membranes composed of anionic sites and ionophore in a 1:4 molar ratio, which results in the formation of 2:1 complexes with CO(3)(2-) with stability constants up to 4.1 × 10(15). As predicted by established theory, the site-to-ionophore ratios that provide optimum potentiometric selectivity depend on the stoichiometries of the complexes of both the primary and the interfering ions. However, the ionophores used in this study give examples of charges and stoichiometries previously neither explicitly predicted by theory nor shown by experiment. The exceptional selectivity of fluorous membranes doped with these carbonate ionophores

  19. Potentiometric and electrokinetic signatures of iron(II) interactions with (a,y)-Fe2O3

    SciTech Connect

    Toczydlowska, Diana; Kedra-Krolik, Karolina; Nejbert, Krzysztof; Preocanin, Tajana; Rosso, Kevin M.; Zarzycki, Piotr P.

    2015-05-29

    The role of surface electrostatics on the reductive dissolution of iron (III) oxides is poorly understood, despite its importance in controlling the amount of mobilized iron. We report the potentiometric titration of the a; y -Fe2O3 oxides exposed to reductants and complexing ligands (Fe(II), ascorbate, oxalate, malonate). We monitored in situ surface and potentials, the ratio of mobilized ferric to ferrous ions, and periodically analyzed nanoparticle crystal structure using X-ray diffraction. We found that addition of Fe2+ ions produces a response consistent with the iron solubilityactivity curve, whereas the presence of ascorbate significantly decreases the amount of mobilized Fe(III) due to reduction to Fe(II). In addition, XRD analysis proved that y-Fe2O3 particles remain structurally unchanged along the titration pathway despite iron cycling between aqueous and solid reservoirs. Our studies, suggest that the surface redoxactivity of iron oxides is primarily governed by the balance between Fe(III) and Fe(II) ions in aqueous phase, which may be easily altered by complexing and reducing agents.

  20. Integrated acquisition of analytical and biopharmaceutical screening data for beta-adrenergic-drugs employing diversified macrocycle supported potentiometric detection in HPLC systems.

    PubMed

    Bazylak, Grzegorz; Nagels, Luc J

    2002-08-01

    Potentiometric detection with poly(vinyl chloride) (PVC) based liquid membrane electrode coatings is presented for a series of eighteen beta-adrenoceptor binding drugs (five agonists and thirteen antagonists) in cation exchange-HPLC and RP-HPLC systems. Incorporation of lipophilic cation-exchanger tetrakis(p-chlorophenyl)borate (TCPB) alone or in combination with trioctylated alpha-cyclodextrin into the polymeric liquid membrane gives very sensitive responses for racemic forms of bufuralol, propranolol, carazolol, clenbuterol, mabuterol, cimaterol, bisoprolol, oxprenolol, alprenolol, tertatolol, and bevantolol, especially in the cation-exchange HPLC system applying acetonitrile -- 40 mM phosphoric acid (15: 85, v/v, pH* = 2.35) as the mobile phase. In both applied orthogonal HPLC modes we observed that use of TCPB containing electrodes (no addition of neutral macrocyclic ionophores) gives more than five fold improvement in limit of detection down to 10(-7) M for mabuterol, bufuralol, alprenolol and tertatolol in comparison with UV detection. These results suggest that potentiometric detection, especially in RP-HPLC employing hybrid polymer-silica packings, can be considered as the promising alternative in the high-throughput drug abuse or doping control procedures of investigated beta-adrenergic agonists and beta-adrenolytics in humans and animals. The quantitative structure - potentiometric response relationships were developed for a set of eighteen beta-adrenenergic drugs and a set of PVC based electrodes using TCPB alone or in admixture with trioctylated alpha-cyclodextrin, dibenzo-18-crown-6 or calix[6]arene hexaethylacetate ester. A multiple linear regression model based on computationally derived set of molecular descriptors was used to predict detection limits of beta-blocking agents and beta-adrenergic agonists from their molecular structure in the developed potentiometric detectors. Principal components analysis (PCA) of data considering determined

  1. Textile-based sampling for potentiometric determination of ions.

    PubMed

    Lisak, Grzegorz; Arnebrant, Thomas; Ruzgas, Tautgirdas; Bobacka, Johan

    2015-06-01

    Potentiometric sensing utilizing textile-based micro-volume sampling was applied and evaluated for the determination of clinically (Na(+), K(+), Cl(-)) and environmentally (Cd(2+), Pb(2+) and pH) relevant analytes. In this technological design, calibration solutions and samples were absorbed into textiles while the potentiometric cells (ion-selective electrodes and reference electrode) were pressed against the textile. Once the liquid, by wicking action, reached the place where the potentiometric cell was pressed onto the textile, hence closing the electric circuit, the potentiometric response was obtained. Cotton, polyamide, polyester and their blends with elastane were applied for micro-volume sampling. The textiles were found to influence the determination of pH in environmental samples with pH close to neutral and Pb(2+) at low analyte concentrations. On the other hand, textile-based micro-volume sampling was successfully applied in measurements of Na(+) using solid-contact sodium-selective electrodes utilizing all the investigated textiles for sampling. It was found that in order to extend the application of textile-based sampling toward environmental analysis of ions it will be necessary to tailor the physio-chemical properties of the textile materials. In general, textile-based sampling opens new possibilities for direct chemical analysis of small-volume samples and provide a simple and low-cost method to screen various textiles for their effects on samples to identify which textiles are the most suitable for on-body sensing.

  2. Fluorescent cationic probes of mitochondria. Metrics and mechanism of interaction.

    PubMed

    Bunting, J R; Phan, T V; Kamali, E; Dowben, R M

    1989-11-01

    Mitochondria strongly accumulate amphiphilic cations. We report here a study of the association of respiring rat liver mitochondria with several fluorescent cationic dyes from differing structural classes. Using gravimetric and fluorometric analysis of dye partition, we find that dyes and mitochondria interact in three ways: (a) uptake with fluorescence quenching, (b) uptake without change in fluorescence intensity, and (c) lack of uptake. For dyes that quench upon uptake, the extent of quenching correlates with the degree of aggregation of the dye to dimers, as predicted by theory (Tomov, T.C. 1986. J. Biochem. Biophys. Methods. 13:29-38). Also predicted is the relationship observed between quenching and the mitochondria concentration when constant dye is titrated with mitochondria. Not predicted is the relationship observed between quenching and dye concentration when constant mitochondria are titrated with dye. Because a limit to dye uptake exists, in this case, the degree of quenching decreases as dye is added. A Langmuir isotherm analysis gives phenomenological parameters that predict quenching when it is observed as a function of dye concentration. By allowing for a decrease in membrane potential, caused by incorporation of cationic dye into the lipid bilayer, a modification of the Tomov theory predicts the dye titration data. We present a model of cationic dye-mitochondria interaction and discuss the use of these as probes of mitochondrial membrane potential.

  3. Determination of metal speciation by reverse titrations.

    PubMed

    Nuester, Jochen; van den Berg, Constant M G

    2005-01-01

    A new method is proposed to determine metal speciation by varying the concentration of a competing ligand at a constant metal concentration, with detection by cathodic stripping voltammetry. The free metal ion concentration is gradually lowered from its natural level while the method probes progressively deeper into the already complexed metal fraction: it is therefore a reverse titration rather than the forward titration which is used for conventional complexing ligand titrations. The sensitivity is greatest at the lowest free metal ion concentration, where it matters most, and the method can be carried out in a single sample aliquot in the voltammetric cell. The method is applied here to copper speciation, but in principle, it can also be used for other metals. Modeling shows that this method has good sensitivity at ligand concentrations near the metal concentration (lower as well as greater). Comparative measurements of copper speciation using reverse and forward titrations of representative water samples of oceanic and coastal origin show good agreement. The data showed that these samples did not contain low levels of strong ligands in addition to the ligands detected by the forward titrations.

  4. Association quotients of aluminum sulphate complexes in NaCl media from 50 to 125 C: Results of a potentiometric and solubility study

    SciTech Connect

    Ridley, M.K.; Kettler, R.M.; Wesolowski, D.J.; Palmer, D.A.

    1999-02-01

    The speciation and molal formation quotients for the complexation of aluminum with sulphate were measured based on potentiometric and solubility experiments. Potentiometric titrations, utilizing a hydrogen-electrode concentration cell, were performed from 50 to 125 C at ionic strengths of 0.1, 0.3 and 1.0 molal in aqueous NaCl media. Two aluminum-sulphate species, AlSO{sub 4}{sup +} and Al(SO{sub 4}){sub 2}{sup {minus}}, were identified from the titration data and the formation quotients for these species were modeled by empirical equations to describe their temperature and ionic strength dependencies. Thermodynamic parameters for the complexation reactions were obtained by differentiating the empirical equations with respect to temperature. The thermodynamic quantities obtained for the formation of AlSO{sub 4}{sup +} at 50 C and infinite dilution are: logK{sub 1} = 3.7 {+-} 0.4, {Delta}H{sub 1}{degree} = {minus}10 {+-} 30 kJ/mol, {Delta}S{sub 1}{degree} = 40 {+-} 100 J/K{center_dot}mol and {Delta}C{sub p 1}{degree} = 1900 {+-} 800 J/K{center_dot}mol; whereas the values for Al(SO{sub 4}){sub 2}{sup {minus}} are: logK{sub 2} = 5.6 {+-} 0.7, {Delta}H{sub 2}{degree} = 10 {+-} 50 kJ/mol, {Delta}S{sub 2}{degree} = 100 {+-} 100 J/K{center_dot}mol and {Delta}C{sub p 2}{degree} = 2800 {+-} 800 J/K{center_dot}mol. A solubility study, which was undertaken to verify the 50 C potentiometric data, was performed by reacting powdered gibbsite (Al(OH){sub 3}) with sulphate solutions at 10{sup {minus}3.5} and 10{sup {minus}4} molal H{sup +}, total sulphate concentrations from 0.005 to 0.080 molal, and 0.1 and 1.0 molal ionic strength in aqueous NaCl media. The results of the solubility study are in good agreement with the potentiometric data and establish that Al-sulphate complexation substantially enhances the equilibrium solubility of gibbsite.

  5. Determination of copper, zinc, selenium, lead and cadmium in potatoes (Solanum tuberosum L.) using potentiometric stripping methods.

    PubMed

    Dugo, G; La Pera, L; Lo Turco, V; Giuffrida, D; Restuccia, S

    2004-07-01

    Potentiometric stripping analysis was used to determine simultaneously the content of zinc(II), cadmium(II), lead(II) and copper(II) in potatoes, whereas the concentration of selenium was determined by cathodic stripping potentiometric analysis. Metal cations were extracted from potatoes by hydrogen peroxide/hydrochloric acid treatments. The relative standard deviation of the methods ranged from 2.3 to 4.1% and the detection limits were lower than 2.5 microg kg(-1). The results obtained with the proposed methods were compared with those obtained with graphite furnace atomic absorption spectroscopy, a common method for determining metals. The results of the two methods agreed to within 6.1%. Twelve samples of yellow flesh potatoes from different cultivars were analysed. Of all the metals determined, Cu and Zn were the most abundant with concentrations between 0.5 and 4.6 mg kg(-1). Selenium was only found in three samples in very low amounts (<0.1 mg kg(-1)), whilst Pb and Cd concentrations were in the range 0.01-0.27 mg kg(-1).

  6. Protein Detection with Potentiometric Aptasensors: A Comparative Study between Polyaniline and Single-Walled Carbon Nanotubes Transducers

    PubMed Central

    Imran, Hassan; Levon, Kalle; Rius, F. Xavier

    2013-01-01

    A comparison study on the performance characteristics and surface characterization of two different solid-contact selective potentiometric thrombin aptasensors, one exploiting a network of single-walled carbon nanotubes (SWCNTs) and the other the polyaniline (PANI), both acting as a transducing element, is described in this work. The molecular properties of both SWCNT and PANI surfaces have been modified by covalently linking thrombin binding aptamers as biorecognition elements. The two aptasensors are compared and characterized through potentiometry and electrochemical impedance spectroscopy (EIS) based on the voltammetric response of multiply charged transition metal cations (such as hexaammineruthenium, [Ru(NH3)6]3+) bound electrostatically to the DNA probes. The surface densities of aptamers were accurately determined by the integration of the peak for the reduction of [Ru(NH3)6]3+ to [Ru(NH3)6]2+. The differences and the similarities, as well as the transduction mechanism, are also discussed. The sensitivity is calculated as 2.97 mV/decade and 8.03 mV/decade for the PANI and SWCNTs aptasensors, respectively. These results are in accordance with the higher surface density of the aptamers in the SWCNT potentiometric sensor. PMID:23533345

  7. Titration of the bacteriorhodopsin Schiff base involves titration of an additional protein residue.

    PubMed

    Zadok, Uri; Asato, Alfred E; Sheves, Mordechai

    2005-06-14

    The retinal protein protonated Schiff base linkage plays a key role in the function of bacteriorhodopsin (bR) as a light-driven proton pump. In the unphotolyzed pigment, the Schiff base (SB) is titrated with a pK(a) of approximately 13, but following light absorption, it experiences a decrease in the pK(a) and undergoes several alterations, including a deprotonation process. We have studied the SB titration using retinal analogues which have intrinsically lower pK(a)'s which allow for SB titrations over a much lower pH range. We found that above pH 9 the channel for the SB titration is perturbed, and the titration rate is considerably reduced. On the basis of studies with several mutants, it is suggested that the protonation state of residue Glu204 is responsible for the channel perturbation. We suggest that above pH 12 a channel for the SB titration is restored probably due to titration of an additional protein residue. The observations may imply that during the bR photocycle and M photointermediate formation the rate of Schiff base protonation from the bulk is decreased. This rate decrease may be due to the deprotonation process of the "proton-releasing complex" which includes Glu204. In contrast, during the lifetime of the O intermediate, the protonated SB is exposed to the bulk. Possible implications for the switch mechanism, and the directionality of the proton movement, are discussed.

  8. Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, May 2009

    USGS Publications Warehouse

    Kinnaman, Sandra L.; Dixon, Joann F.

    2009-01-01

    This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2009. Potentiometric contours are based on water-level measurements collected at 625 wells during the period May 14 - May 29, near the end of the dry season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to groundwater withdrawals and spring flow. Potentiometric-surface highs generally correspond to topographic highs where the aquifer is recharged. Springs and areas of diffuse upward leakage naturally discharge water from the aquifer and are most prevalent along the St. Johns River. Areas of discharge are reflected by depressions in the potentiometric surface. Groundwater withdrawals locally have lowered the potentiometric surface. Groundwater in the Upper Floridan aquifer generally flows from potentiometric highs to potentiometric lows in a direction perpendicular to the contours.

  9. Colorimetric Titration Experiment for the Undergraduate Laboratory.

    ERIC Educational Resources Information Center

    Lopez, Edwin; Vassos, Basil H.

    1984-01-01

    Describes a colorimetric titration instrument usable in the undergraduate laboratory that fulfills the objectives of ruggedness, freedom from ambient light interference, and low cost. Although accessories can be added (raising the price), the basic instrument is low priced and can be used manually with a simple voltmeter. (JN)

  10. Acid Rain Analysis by Standard Addition Titration.

    ERIC Educational Resources Information Center

    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)

  11. Isothermal Titration Calorimetry in the Student Laboratory

    ERIC Educational Resources Information Center

    Wadso, Lars; Li, Yujing; Li, Xi

    2011-01-01

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

  12. Titration Calculations with Computer Algebra Software

    ERIC Educational Resources Information Center

    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,…

  13. Problems in the interpretation of nonaqueous titrations.

    PubMed

    Buvári-Barcza, A; Barcza, L

    2005-04-01

    Most phenomena (like promoting and leveling as well as differentiating effects) of common nonaqueous titrations can be explained by the Brönsted's concept combined with the hydrogen bond theory but some open problems are shown in connection with the use of formic acid and/or acetic anhydride.

  14. Rapid titration of viruses by flow cytometry.

    PubMed

    Drayman, Nir; Oppenheim, Ariella

    2011-06-01

    Traditionally, the most common methods used to titrate virus stocks are the plaque assay and the hemagglutination assay. The protocol presented here is based on the detection of viral-expressed proteins in infected cells by flow cytometry. It is simpler and more rapid than the traditional plaque-forming assay and it enables high-throughput analyses.

  15. Direct potentiometric determination of starch using a platinum redox sensor.

    PubMed

    Sakač, Nikola; Sak-Bosnar, Milan; Horvat, Marija

    2013-05-01

    Here, we describe the development of a platinum redox sensor for the direct potentiometric quantification of starch in solution. The sensor measures the decrease in free triiodide ion after it complexes with starch to form a starch-triiodide complex. This decrease was, therefore, correlated with starch concentration, and the composition and stability of the potassium triiodide solution were optimised. The starch-triiodide complex was characterized potentiometrically at variable starch and triiodide concentrations. We also propose a response mechanism for the platinum redox sensor towards starch and an appropriate theoretical model. The optimised method exhibited satisfactory accuracy and precision and was in good agreement with a standard spectrophotometric method. The sensor was tested over a range of 0.4-9 mg starch, with recoveries ranging from 97.8% to 103.4% and a detection limit of 0.01 mg starch.

  16. Tracer monitored titrations: measurement of total alkalinity.

    PubMed

    Martz, Todd R; Dickson, Andrew G; DeGrandpre, Michael D

    2006-03-15

    We introduce a new titration methodology, tracer monitored titration (TMT), in which analyses are free of volumetric and gravimetric measurements and insensitive to pump precision and reproducibility. Spectrophotometric monitoring of titrant dilution, rather than volume increment, lays the burden of analytical performance solely on the spectrophotometer. In the method described here, the titrant is a standardized mixture of acid-base indicator and strong acid. Dilution of a pulse of titrant in a titration vessel is tracked using the total indicator concentration measured spectrophotometrically. The concentrations of reacted and unreacted indicator species, derived from Beer's law, are used to calculate the relative proportions of titrant and sample in addition to the equilibrium position (pH) of the titration mixture. Because the method does not require volumetric or gravimetric additions of titrant, simple low-precision pumps can be used. Here, we demonstrate application of TMT for analysis of total alkalinity (A(T)). High-precision, high-accuracy seawater A(T) measurements are crucial for understanding, for example, the marine CaCO3 budget and saturation state, anthropogenic CO2 penetration into the oceans, calcareous phytoplankton blooms, and coral reef dynamics. We present data from 286 titrations on three types of total alkalinity standards: Na2CO3 in 0.7 mol kg x soln(-1) NaCl, NaOH in 0.7 mol kg x soln(-1) NaCl, and a seawater Certified Reference Material (CRM). Based on Na2CO3 standards, the accuracy and precision are +/-0.2 and +/-0.1% (4 and 2 micromol kg x soln(-1) for A(T) approximately 2100-2500 micromol kg x soln(-1), n = 242), using low-precision solenoid pumps to introduce sample and titrant. Similar accuracy and precision were found for analyses run 42 days after the initial experiments. Excellent performance is achieved by optimizing the spectrophotometric detection system and relying upon basic chemical thermodynamics for calculating the

  17. Porous silicon as a substrate material for potentiometric biosensors

    NASA Astrophysics Data System (ADS)

    Thust, Marion; Schöning, M. J.; Frohnhoff, S.; Arens-Fischer, R.; Kordos, P.; Lüth, H.

    1996-01-01

    For the first time porous silicon has been investigated for the purpose of application as a substrate material for potentiometric biosensors operating in aqueous solutions. Porous silicon was prepared from differently doped silicon substrates by a standard anodic etching process. After oxidation, penicillinase, an enzyme sensitive to penicillin, was bound to the porous structure by physical adsorption. To characterize the electrochemical properties of the so build up penicillin biosensor, capacitance - voltage (C - V) measurements were performed on these field-effect structures.

  18. Potentiometric map of the Cockfield Aquifer in Mississippi, fall 1984

    USGS Publications Warehouse

    Darden, Daphne

    1986-01-01

    This map, the second in a series for the Cockfield aquifer in Mississippi, follows a map that delineated the 1980 potentiometric surface of the aquifer. This water level map is based on water level measurements made in about 80 wells in the Cockfield aquifer in the fall of 1984. The contours show altitudes at which water levels would have stood in tightly cased unpumped wells in fall 1984. (Lantz-PTT)

  19. Automated potentiometric electrolyte analysis system. [for use in weightlessness

    NASA Technical Reports Server (NTRS)

    1973-01-01

    The feasibility is demonstrated of utilizing chemical sensing electrode technology as the basis for an automatically-controlled system for blood gas and electrolyte analyses under weightlessness conditions. The specific measurements required were pH, pCO2, sodium, chloride, potassium ions, and ionized calcium. The general electrode theory, and ion activity measurements are described along with the fluid transport package, electronics unit, and controller for the automated potentiometric analysis system.

  20. Potentiometric Surface of the Ozark Aquifer in Northern Arkansas, 2007

    USGS Publications Warehouse

    Pugh, Aaron L.

    2008-01-01

    The Ozark aquifer in northern Arkansas is composed of dolomite, limestone, sandstone, and shale of Late Cambrian to Middle Devonian age, and ranges in thickness from approximately 1,100 feet to more than 4,000 feet. Hydrologically, the aquifer is complex, characterized by discrete and discontinuous flow components with large variations in permeability. The potentiometric-surface map, based on 58 well and 5 spring water-level measurements collected in 2007 in Arkansas and Missouri, has a maximum water-level altitude measurement of 1,169 feet in Carroll County and a minimum water-level altitude measurement of 118 feet in Randolph County. Regionally, the flow within the aquifer is to the south and southeast in the eastern and central part of the study area and to the west, northwest, and north in the western part of the study area. Comparing the 2007 potentiometric-surface map with a predevelopment potentiometric-surface map indicates general agreement between the two surfaces except in the northwestern part of the study area. Potentiometric-surface differences can be attributed to withdrawals related to increasing population, changes in public-supply sources, processes or water withdrawals outside the study area, or differences in data-collection or map-construction methods. The rapidly increasing population within the study area appears to have some effect on ground-water levels. Although, the effect appears to have been minimized by the development and use of surface-water distribution infrastructure, suggesting most of the incoming populations are fulfilling their water needs from surface-water sources. The conversion of some users from ground water to surface water may be allowing water levels in wells to recover (rise) or decline at a slower rate, such as in Benton, Carroll, and Washington Counties.

  1. Fabrication of a potentiometric/amperometric bifunctional enzyme microbiosensor.

    PubMed

    Reddy, K Ravi Charan; Turcu, Florin; Schulte, Albert; Kayastha, Arvind M; Schuhmann, Wolfgang

    2005-08-01

    We report the fabrication and functional characterization of a needle-type bifunctional enzyme microbiosensor that has, as technical novelty, simultaneously integrated a potentiometric and amperometric detection of an enzyme-catalyzed reaction at the tip of a pulled glass micropipet. The construction involved immobilizing an enzyme onto the platinized outer tip surface using the precipitation of electrodeposition paint with direct entrapment of the biocomponent in the slowly growing polymer film. Products of enzyme-substrate reaction could then be targeted in a dual-detection mode on one hand with the covered Pt layer at the tip region as amperometric detector and on the other hand with a proton-selective liquid membrane-based potentiometric sensor inside the open pipet tip. Completing and testing bifunctional glucose microsensors demonstrated the functionality of the proposed strategy. Synchronized amperometric and potentiometric detection of the addition of a glucose standard to a buffer solution became evident by observing stepwise increases in the amperometric H2O2 oxidation current and corresponding increases in the potential of the pH-selective sensor, which translates to a local pH decrease around the tip due to hydrolysis of enzymatically formed gluconic acid. PMID:16053323

  2. Potentiometric surface of the Ozark Aquifer in northern Arkansas, 1995

    USGS Publications Warehouse

    Pugh, Aaron L.

    1998-01-01

    The Ozark aquifer in northern Arkansas is comprised of dolostones, limestones, sandstones, and shales of Late Cambrian to Middle Devonian age, and ranges in thickness from approximately 1,100 feet to more than 4,000 feet. Hydrologically, the aquifer is complex, characterized by discrete and diffuse flow components with large spatial variations in porosity and permeability. Regionally, the flow within the aquifer is to the south and southeast in the eastern and central part of the study area and to the northwest and north in the western part of the study area. Within Arkansas, the potentiometric-surface map based on October- December 1995 data indicates maximum water-level altitudes of greater than 1,300 feet in Boone, Carroll, and Madison Counties and minimum water-level altitudes of less than 400 feet in Independence, Izard, Lawrence, Randolph, Sharp, and Stone Counties. Comparing the 1995 potentiometric-surface map with a predevelopment potentiometric- surface map (Imes, 199), indicates general agreement between the two surfaces except in parts of Benton and Sharp Counties. Water-level differences could be attributed to differences in the time of year in which the water-level data were collected, differences in pumping conditions just prior to water-level measurement, differences in interpretation resulting (in part) from greater number of water-level measurements used for this report than for Imes (1990), or erroneous water-level data.

  3. Preliminary potentiometric map and flow dynamic characteristics for the upper-basalt confined aquifer system

    SciTech Connect

    Spane, F.A. Jr.; Raymond, R.G.

    1993-09-01

    This report presents the first comprehensive Hanford Site-wide potentiometric map for the upper-basalt confined aquifer system (i.e., the upper Saddle Mountains Basalt). In constructing the potentiometric map, over forty on-site and off-site monitoring wells and boreholes were used. The potentiometric map developed for the upper-basalt confined aquifer is consistent with the areal head pattern indicated for the Mabton interbed, which is a deeper and more areally extensive confined aquifer underlying the Hanford Site. Salient features for the upper-basalt confined aquifer system potentiometric map are described.

  4. An Olfactory Indicator for Acid-Base Titrations.

    ERIC Educational Resources Information Center

    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)

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

    PubMed

    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.

  6. Redox potential of shallow groundwater by 1-month continuous in situ potentiometric measurements

    NASA Astrophysics Data System (ADS)

    Ioka, Seiichiro; Muraoka, Hirofumi; Suzuki, Yota

    2016-06-01

    One-month continuous in situ potentiometric measurements of redox potential (Eh) were used to investigate the dominant redox processes in the shallow groundwater (i.e., <10 m) of a Holocene aquifer, Aomori City, northern Japan. The Eh values, which were determined using a platinum electrode, were -163, -169 and -173 mV, respectively, for three monitoring campaigns. The temperatures and pH values of shallow groundwater during all three periods were approximately 12 °C and 6.6, respectively. Dissolved oxygen and sulfide ion concentrations were not detected. Chemical analyses showed that the shallow groundwater is Na-Fe-HCO3 type, and contains over 40 mg/L of Fe (the dominant cation) and over 200 mg/L of HCO3 - (the dominant anion). A good fit was found between measured Eh values and Eh values calculated using thermodynamic data of fine-grained goethite. This suggests that Fe redox system is related to the Eh values of shallow groundwater in the Aomori City aquifer.

  7. Manganese(III) porphyrin-based potentiometric sensors for diclofenac assay in pharmaceutical preparations.

    PubMed

    Vlascici, Dana; Pruneanu, Stela; Olenic, Liliana; Pogacean, Florina; Ostafe, Vasile; Chiriac, Vlad; Pica, Elena Maria; Bolundut, Liviu Calin; Nica, Luminita; Fagadar-Cosma, Eugenia

    2010-01-01

    Two manganese(III) porphyrins: manganese(III) tetraphenylporphyrin chloride and manganese(III)-tetrakis(3-hydroxyphenyl)porphyrin chloride were tested as ionophores for the construction of new diclofenac-selective electrodes. The electroactive material was incorporated either in PVC or a sol-gel matrix. The effect of different plasticizers and additives (anionic and cationic) on the potentiometric response was studied. The best results were obtained for the PVC membrane plasticized with dioctylphtalate and having sodium tetraphenylborate as a lipophilic anionic additive incorporated. The sensor response was linear in the concentration range 3 × 10(-6) - 1 × 10(-2) M with a slope of -59.7 mV/dec diclofenac, a detection limit of 1.5 × 10(-6) M and very good selectivity coefficients. It was used for the determination of diclofenac in pharmaceutical preparations, by direct potentiometry. The results were compared with those obtained by the HPLC reference method and a good agreement was found between the two methods.

  8. Determination of carbonate carbon in geological materials by coulometric titration

    USGS Publications Warehouse

    Engleman, E.E.; Jackson, L.L.; Norton, D.R.

    1985-01-01

    A coulometric titration is used for the determination of carbonate carbon in geological materials. Carbon dioxide is evolved from the sample by the addition of 2 M perchloric acid, with heating, and is determined by automated coulometric titration. The coulometric titration showed improved speed and precision with comparable accuracy to gravimetric and gasometric techniques. ?? 1985.

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

    ERIC Educational Resources Information Center

    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…

  10. A potentiometric study of the hydrolysis of ethylenediaminetetraacetic acid to 150{degrees}C

    SciTech Connect

    Palmer, D.A.; Nguyen-Trung, Chinh

    1995-02-01

    Ethylenediaminetetraacetate anions, EDTA{sup 4-}, were titrated in a hydrogen-electrode concentration cell with an acidic titrant from 0 to 150{degrees}C at 25{degrees}C intervals. These titrations were carried out in the presence of 0. 1, 0.2, and 1.0 mol{center_dot}kg{sup -1} with the supporting electrolytes, sodium chloride, NaCl, and 1.0 mol{center_dot}kg{sup -1} tetramethylammonium trifluoromethylsulfonate, (CH{sub 3}){sub 4}N(F{sub 3}CSO{sub 3}) {l_brace}TMATFMS{r_brace} in order to assess the effect of both cation complexation by EDTA{sup 4-} and anion activity coefficient variations. The resulting hydrolysis quotients are discussed with reference to applications in boiler and heat exchanger chemical cleaning, as well as chemical and nuclear waste containment. Some recent diverse uses of this emf technique that also pertain to these applications will be mentioned briefly, e.g., surface absorption - zero-point-of-charge - measurements to high temperatures and in situ pH measurements in solubility and kinetic experiments.

  11. Digital movie-based on automatic titrations.

    PubMed

    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%.

  12. Digital movie-based on automatic titrations.

    PubMed

    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%. PMID:26592600

  13. A new sensor for thermometric titrations.

    PubMed

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

    2007-01-15

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

  14. A monosegmented-flow Karl Fischer titrator.

    PubMed

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

    2007-02-28

    A monosegmented volumetric Karl Fischer titrator is described to mechanize the determination of water content in organic solvents. The system is based on the flow-batch characteristics of the monosegmented analysis concept and employs biamperometry to monitor the progress of the titration. The system shows accuracy and precision that are highly independent of the flow rate, does not require calibration, and is carried out in a closed system capable of minimizing contact of the sample and reagents with ambient moisture. Sample volumes in the range of 40-300muL are employed, depending on the water concentration. An automatic dilution is provided to deal with concentrated samples. The consumption of Karl Fischer reagent depends on the water content of the sample but is not larger than 100muL. The system was evaluated for determination of water in ethanol and methanol in the range 0.02-0.5% (w/w). The average relative precision estimated in that range (9-3%) is comparable to that obtained with a larger volume commercial system and no significant difference was observed between the results obtained for the two systems at the 95% confidence level. A complete titration can be performed in less than 5min employing the proposed system. PMID:19071447

  15. Integrated, paper-based potentiometric electronic tongue for the analysis of beer and wine.

    PubMed

    Nery, Emilia Witkowska; Kubota, Lauro T

    2016-04-28

    The following manuscript details the stages of construction of a novel paper-based electronic tongue with an integrated Ag/AgCl reference, which can operate using a minimal amount of sample (40 μL). First, we optimized the fabrication procedure of silver electrodes, testing a set of different methodologies (electroless plating, use of silver nanoparticles and commercial silver paints). Later a novel, integrated electronic tongue system was assembled with the use of readily available materials such as paper, wax, lamination sheets, bleach etc. New system was thoroughly characterized and the ion-selective potentiometric sensors presented performance close to theoretical. An electronic tongue, composed of electrodes sensitive to sodium, calcium, ammonia and a cross-sensitive, anion-selective electrode was used to analyze 34 beer samples (12 types, 19 brands). This system was able to discriminate beers from different brands, and types, indicate presence of stabilizers and antioxidants, dyes or even unmalted cereals and carbohydrates added to the fermentation wort. Samples could be classified by type of fermentation (low, high) and system was able to predict pH and in part also alcohol content of tested beers. In the next step sample volume was minimalized by the use of paper sample pads and measurement in flow conditions. In order to test the impact of this advancement a four electrode system, with cross-sensitive (anion-selective, cation-selective, Ca(2+)/Mg(2+), K(+)/Na(+)) electrodes was applied for the analysis of 11 types of wine (4 types of grapes, red/white, 3 countries). Proposed matrix was able to group wines produced from different varieties of grapes (Chardonnay, Americanas, Malbec, Merlot) using only 40 μL of sample. Apart from that, storage stability studies were performed using a multimeter, therefore showing that not only fabrication but also detection can be accomplished by means of off-the-shelf components. This manuscript not only describes new

  16. Potentiometric surface of the Lloyd aquifer on Long Island, New York, in January 1975

    USGS Publications Warehouse

    Rich, Charles A.; Prince, Keith R.; Spinello, Anthony G.

    1975-01-01

    A map showing the potentiometric surface of the Lloyd aquifer was drawn from water-level measurements made in January 1975. Altitude of the potentiometric surface ranged from more than 20 feet below mean sea level in Queens County to more than 40 feet above mean sea level in Suffolk County.

  17. Kinetic detection of the end-point in titrations involving slow reactions Direct titration of polyhydroxy-compounds with periodate.

    PubMed

    Efstathiou, C E; Hadjiioannou, T P

    1983-03-01

    A new titration technique is described in which the end-point is determined by measuring the relative reaction rate of the titration reaction. This technique is adequate for rather slow reactions where conventional direct titrations are not applicable. The titrations are done automatically under microcomputer control. The efficiency of this technique is demonstrated with direct titrations of certain polyhydroxy-compounds with standard periodate solution. Ethylene glycol and propylene glycol (0.05-0.3 mmole), glycerol (0.06-0.17 mmole) and mannitol (0.01-0.03 mmole) were determined with average relative errors of 0.1-0.3%.

  18. Potentiometric surface of the Catahoula aquifer in central Louisiana, 2013

    USGS Publications Warehouse

    Fendick, Jr., Robert B.; Carter, Kayla

    2015-12-09

    The potentiometric surface of the Catahoula aquifer was constructed by using the altitude of water levels measured at 29 wells during the period May through September 2013. The altitude of water levels ranged from 0.02 ft above the National Geodetic Vertical Datum of 1929 (NGVD 29) in well Co-51 to 238 ft above NGVD 29 in well Na-317. Groundwater movement in the Catahoula aquifer is generally to the southeast and towards discharge areas beneath the Sabine, Red, Little, and Tensas River Valleys.

  19. Electrochemical titrations and reaction time courses monitored in situ by magnetic circular dichroism spectroscopy.

    PubMed

    Bradley, Justin M; Butt, Julea N; Cheesman, Myles R

    2011-12-15

    Magnetic circular dichroism (MCD) spectra, at ultraviolet-visible or near-infrared wavelengths (185-2000 nm), contain the same transitions observed in conventional absorbance spectroscopy, but their bisignate nature and more stringent selection rules provide greatly enhanced resolution. Thus, they have proved to be invaluable in the study of many transition metal-containing proteins. For mainly technical reasons, MCD has been limited almost exclusively to the measurement of static samples. But the ability to employ the resolving power of MCD to follow changes at transition metal sites would be a potentially significant advance. We describe here the development of a cuvette holder that allows reagent injection and sample mixing within the 50-mm-diameter ambient temperature bore of an energized superconducting solenoid. This has allowed us, for the first time, to monitor time-resolved MCD resulting from in situ chemical manipulation of a metalloprotein sample. Furthermore, we report the parallel development of an electrochemical cell using a three-electrode configuration with physically separated working and counter electrodes, allowing true potentiometric titration to be performed within the bore of the MCD solenoid.

  20. Aqueous complexation of trivalent lanthanide and actinide cations by N,N,N'{sub 2},N'-tetrakis(2-pyridylmethyl)ethylenediamine.

    SciTech Connect

    Beitz, J. V.; Ensor, D. D.; Jensen, M. P.; Morss, L. R.

    1999-06-16

    The aqueous complexation reactions of trivalent lanthanide and actinide cations with the hexadentate ligand N,N,N{prime},N{prime}-tetrakis(2-pyridylmethyl)ethylenediamine (TPEN), have been characterized using potentiometric and spectroscopic techniques in 0.1 M NaClO{sub 4} At 25 C, the stability constant of Am(TPEN){sup 3+} is two orders of magnitude larger than that of Sm(TPEN){sup 3+}, reflecting the stronger interactions of the trivalent actinide cations with softer ligands as compared to lanthanide cations.

  1. Direct spectrophotometric detection of the endpoint in metachromatic titration of polydiallyldimethylammonium chloride in water

    NASA Astrophysics Data System (ADS)

    Gumbi, B.; Ngila, J. C.; Ndungu, P. G.

    Polydiallyldimethylammonium chloride (poly-DADMAC) is a water soluble polymer that easily ionizes when dissolved in water. This cationic polyelectrolyte is mainly used as a flocculant within the water treatment industry, but little is known of its toxicological properties or its fate in the environment. It is often assumed that the polyelectrolyte sorbs onto solid surfaces in the water treatment stream and may be removed with the sludge or by a sand bed filter; which may not always be the case. In any event, reliable analytical techniques are needed for the determination of poly-DADMAC in matrices of environmental relevance. Metachromatic polyelectrolyte titration was used to quantify poly-DADMAC in model and tap water samples. We compared a routine visual titration method with a direct spectrophotometric technique that uses a dip probe, spectrometer, and computer. The direct spectrophotometric technique allowed for the determination of titration curves at 634 nm and 510 nm, whereby the later value has never been successfully utilised in the literature. The method simplifies the data analysis, and our recovery and matrix interference experiments demonstrate that the method is accurate, precise, and robust. The detection limit for this method was 0.1 mg L-1 in model water and 0.5 mg L-1 in tap water. The limit of quantification for both water matrices was 0.5 mg L-1.

  2. Potentiometric Sensor for Real-Time Remote Surveillance of Actinides in Molten Salts

    SciTech Connect

    Natalie J. Gese; Jan-Fong Jue; Brenda E. Serrano; Guy L. Fredrickson

    2012-07-01

    A potentiometric sensor is being developed at the Idaho National Laboratory for real-time remote surveillance of actinides during electrorefining of spent nuclear fuel. During electrorefining, fuel in metallic form is oxidized at the anode while refined uranium metal is reduced at the cathode in a high temperature electrochemical cell containing LiCl-KCl-UCl3 electrolyte. Actinides present in the fuel chemically react with UCl3 and form stable metal chlorides that accumulate in the electrolyte. This sensor will be used for process control and safeguarding of activities in the electrorefiner by monitoring the concentrations of actinides in the electrolyte. The work presented focuses on developing a solid-state cation conducting ceramic sensor for detecting varying concentrations of trivalent actinide metal cations in eutectic LiCl-KCl molten salt. To understand the basic mechanisms for actinide sensor applications in molten salts, gadolinium was used as a surrogate for actinides. The ß?-Al2O3 was selected as the solid-state electrolyte for sensor fabrication based on cationic conductivity and other factors. In the present work Gd3+-ß?-Al2O3 was prepared by ion exchange reactions between trivalent Gd3+ from GdCl3 and K+-, Na+-, and Sr2+-ß?-Al2O3 precursors. Scanning electron microscopy (SEM) was used for characterization of Gd3+-ß?-Al2O3 samples. Microfocus X-ray Diffraction (µ-XRD) was used in conjunction with SEM energy dispersive X-ray spectroscopy (EDS) to identify phase content and elemental composition. The Gd3+-ß?-Al2O3 materials were tested for mechanical and chemical stability by exposing them to molten LiCl-KCl based salts. The effect of annealing on the exchanged material was studied to determine improvements in material integrity post ion exchange. The stability of the ß?-Al2O3 phase after annealing was verified by µ-XRD. Preliminary sensor tests with different assembly designs will also be presented.

  3. CONDUCTIVITY TITRATION OF GELATIN SOLUTIONS WITH ACIDS.

    PubMed

    Hitchcock, D I

    1923-11-20

    Titrations have been made, by the conductivity method, of gelatin solutions with hydrochloric and sulphuric acids. The results indicate an end-point at about 8.6 cc. of N/10 acid per gm. of gelatin, or a combining weight of about 1,160. These results are in fair agreement with those previously obtained by the hydrogen electrode method. Better agreement between the two methods was found in the case of deaminized gelatin. The data are in accord with a purely chemical conception of the combination between protein and acid.

  4. Tracer monitored titrations: measurement of dissolved oxygen.

    PubMed

    Martz, Todd; Takeshita, Yuichiro; Rolph, Rebecca; Bresnahan, Philip

    2012-01-01

    The tracer monitored titration (TMT) technique is evaluated for measurement of dissolved oxygen. The TMT developed in this work uses a simple apparatus consisting of a low-precision pump for titrant delivery and an optical detector based on a white LED and two photodiodes with interference filters. It is shown that the classic Winkler method can be made free of routine volumetric and gravimetric measurements by application of TMT theory, which allows tracking the amounts of titrant and sample using a chemical tracer. The measurement precision of the prototype setup was 0.3% RSD.

  5. Modeling complexometric titrations of natural water samples.

    PubMed

    Hudson, Robert J M; Rue, Eden L; Bruland, Kenneth W

    2003-04-15

    Complexometric titrations are the primary source of metal speciation data for aquatic systems, yet their interpretation in waters containing humic and fulvic acids remains problematic. In particular, the accuracy of inferred ambient free metal ion concentrations and parameters quantifying metal complexation by natural ligands has been challenged because of the difficulties inherent in calibrating common analytical methods and in modeling the diverse array of ligands present. This work tests and applies a new method of modeling titration data that combines calibration of analytical sensitivity (S) and estimation of concentrations and stability constants for discrete natural ligand classes ([Li]T and Ki) into a single step using nonlinear regression and a new analytical solution to the one-metal/two-ligand equilibrium problem. When applied to jointly model data from multiple titrations conducted at different analytical windows, it yields accurate estimates of S, [Li]T, Ki, and [Cu2+] plus Monte Carlo-based estimates of the uncertainty in [Cu2+]. Jointly modeling titration data at low-and high-analytical windows leads to an efficient adaptation of the recently proposed "overload" approach to calibrating ACSV/CLE measurements. Application of the method to published data sets yields model results with greater accuracy and precision than originally obtained. The discrete ligand-class model is also re-parametrized, using humic and fulvic acids, L1 class (K1 = 10(13) M(-1)), and strong ligands (L(S)) with K(S) > K1 as "natural components". This approach suggests that Cu complexation in NW Mediterranean Sea water can be well represented as 0.8 +/- 0.3/0.2 mg humic equiv/L, 13 +/- 1 nM L1, and 2.5 +/- 0.1 nM L(S) with [CU]T = 3 nM. In coastal seawater from Narragansett Bay, RI, Cu speciation can be modeled as 0.6 +/- 0.1 mg humic equiv/L and 22 +/- 1 nM L1 or approximately 12 nM L1 and approximately 9 nM L(S), with [CU]T = 13 nM. In both waters, the large excess

  6. Determination of lanthanum by flame photometric titration.

    PubMed

    Svehla, G; Slevin, P J

    1968-09-01

    The flame emission of lanthanum at 560 mmu decreases linearly with phosphate concentration until a 1:1 molar ratio is reached, and then remains practically constant. Lanthanum can be titrated with phosphate, the equivalence point being detected from the change in emission intensity. Errors due to consumption of solution by the atomizer can be kept low by using short spraying times and low galvanometer damping. The average error is about -1% for 0.1M solutions and less than -5% for 0.01M. The method gives good results in the presence of titanium(III), zirconium, thorium and aluminium but cerium(III) and yttrium seriously interfere. PMID:18960392

  7. Improving the limits of detection in potentiometric sensors

    NASA Astrophysics Data System (ADS)

    van der Bent, J. F.; Puik, E. C. N.; Tong, H. D.; van Rijn, C. J. M.

    2015-12-01

    Potentiometric sensors will generally suffer from unwanted responses as a result to changing temperatures by generating an electromotive force. Typically, this voltage drift has a non-linear character and therefore it is difficult to compensate using linear algorithms implemented in the analogue domain. A solution is proposed to improve the sensor characteristics by combining the digitized output of two CO2 rubidium silver iodide sensors with a specially designed digital algorithm to improve the limits of detection (LOD). Experiments show that this method has the capability to improve the LOD of the sensor with a factor 4.5x during temperature variations of 22 °C over a measurement period of 22 h. It enables potentiometric sensors to be used in low power wireless sensor networks for long term air quality control. Furthermore, the influence of depletion of the rubidium silver iodide electrolyte layer can be effectively compensated by determining the decay of the active layer according to the Nernst equation. Knowing the function of depletion over time helps to correct the sensor output and thereby improves the accuracy of the sensor.

  8. Determination of urine ionic composition with potentiometric multisensor system.

    PubMed

    Yaroshenko, Irina; Kirsanov, Dmitry; Kartsova, Lyudmila; Sidorova, Alla; Borisova, Irina; Legin, Andrey

    2015-01-01

    The ionic composition of urine is a good indicator of patient's general condition and allows for diagnostics of certain medical problems such as e.g., urolithiasis. Due to environmental factors and malnutrition the number of registered urinary tract cases continuously increases. Most of the methods currently used for urine analysis are expensive, quite laborious and require skilled personnel. The present work deals with feasibility study of potentiometric multisensor system of 18 ion-selective and cross-sensitive sensors as an analytical tool for determination of urine ionic composition. In total 136 samples from patients of Urolithiasis Laboratory and healthy people were analyzed by the multisensor system as well as by capillary electrophoresis as a reference method. Various chemometric approaches were implemented to relate the data from electrochemical measurements with the reference data. Logistic regression (LR) was applied for classification of samples into healthy and unhealthy producing reasonable misclassification rates. Projection on Latent Structures (PLS) regression was applied for quantitative analysis of ionic composition from potentiometric data. Mean relative errors of simultaneous prediction of sodium, potassium, ammonium, calcium, magnesium, chloride, sulfate, phosphate, urate and creatinine from multisensor system response were in the range 3-13% for independent test sets. This shows a good promise for development of a fast and inexpensive alternative method for urine analysis. PMID:25281140

  9. High throughput continuous titration based on a flow ratiometry controlled with feedback-based variable triangular waves and subsequent fixed triangular waves.

    PubMed

    Tanaka, Hideji; Baba, Tsutomu

    2005-10-15

    We propose a new approach for high-throughput continuous titration based on a flow ratiometry. The method was applied to potentiometric titrations of acids and bases. A base solution, the flow rate F(B) of which was varied in response to controller output voltage V(c), was merged with an acid solution under constant total (acid+base) flow rate. Downstream, the pH of the mixed solution was measured with a flow-through glass electrode. Initially, V(c), and thus F(B) was increased linearly. At the instant the equivalence point (EP) was sensed, the ramp direction of V(c) was reversed from upward to downward. The direction was reversed to upward when EP was sensed again. Such the feedback-based operation gives a triangular waveform of V(c), because there is a delay corresponding mainly to the transit time of merged solutions to reach the sensor. The value of V(c) that gives EP composition, V(E), was estimated by averaging the most recent maximum and minimum values of V(c). Next, fixed triangular waves of V(c) was used to control F(B). The amplitude and the scan rate of the waves were fixed narrower and faster, respectively, than those in the feedback-based operation in order to improve the throughput rate. The EP can be located as long as the scan range covers V(E). These automated processes limited the titration to just the narrow range around EP, and thus realized extremely high throughput rate of maximally 17.6 titrations per minute (=3.4s per titration) at R.S.D.=0.35%. PMID:18970249

  10. Bivoltametric titrations using electrodes with innovative geometry.

    PubMed

    Surmann, P; Peter, B; Stark, C

    1996-09-01

    Electrodes with different surface areas were investigated for the determination of reversible, quasireversible, irreversible or electroinactive substrates. Two kinds of electrodes were constructed, a helical electrode with a given asymmetry and a platinum array electrode with a variable area. These electrodes were applied for the cerimetry of ammonium iron(II) sulfate and for the bromatometry of various organic substances. The theoretically derived effects on the shape of the voltametric titration curve are verified experimentally. It is possible to sharpen one side of the peak and to broaden the other side, depending on the system and the side of the peak one is interested in. It is possible to improve the bivoltametric determination of hydroquinone, benzocaine and sulfaguanidine by bromatometry by the directed employment of electrodes of different areas. For the bromatometric determination of electrochemically irreversible substrates the use of the electrode geometries proposed is a way to obtain a sharp bend and a steep decrease of titration curves with low values of the constant current which is a basic requirement for the accuracy.

  11. Biochemical titration of glycogen in vitro.

    PubMed

    Pelletier, Joffrey; Bellot, Grégory; Pouysségur, Jacques; Mazure, Nathalie M

    2013-01-01

    Glycogen is the main energetic polymer of glucose in vertebrate animals and plays a crucial role in whole body metabolism as well as in cellular metabolism. Many methods to detect glycogen already exist but only a few are quantitative. We describe here a method using the Abcam Glycogen assay kit, which is based on specific degradation of glycogen to glucose by glucoamylase. Glucose is then specifically oxidized to a product that reacts with the OxiRed probe to produce fluorescence. Titration is accurate, sensitive and can be achieved on cell extracts or tissue sections. However, in contrast to other techniques, it does not give information about the distribution of glycogen in the cell. As an example of this technique, we describe here the titration of glycogen in two cell lines, Chinese hamster lung fibroblast CCL39 and human colon carcinoma LS174, incubated in normoxia (21% O2) versus hypoxia (1% O2). We hypothesized that hypoxia is a signal that prepares cells to synthesize and store glycogen in order to survive(1).

  12. Biochemical Titration of Glycogen In vitro

    PubMed Central

    Pelletier, Joffrey; Bellot, Grégory; Pouysségur, Jacques; Mazure, Nathalie M.

    2013-01-01

    Glycogen is the main energetic polymer of glucose in vertebrate animals and plays a crucial role in whole body metabolism as well as in cellular metabolism. Many methods to detect glycogen already exist but only a few are quantitative. We describe here a method using the Abcam Glycogen assay kit, which is based on specific degradation of glycogen to glucose by glucoamylase. Glucose is then specifically oxidized to a product that reacts with the OxiRed probe to produce fluorescence. Titration is accurate, sensitive and can be achieved on cell extracts or tissue sections. However, in contrast to other techniques, it does not give information about the distribution of glycogen in the cell. As an example of this technique, we describe here the titration of glycogen in two cell lines, Chinese hamster lung fibroblast CCL39 and human colon carcinoma LS174, incubated in normoxia (21% O2) versus hypoxia (1% O2). We hypothesized that hypoxia is a signal that prepares cells to synthesize and store glycogen in order to survive1. PMID:24300406

  13. Retention of Cationic Starch onto Cellulose Fibres

    NASA Astrophysics Data System (ADS)

    Missaoui, Mohamed; Mauret, Evelyne; Belgacem, Mohamed Naceur

    2008-08-01

    Three methods of cationic starch titration were used to quantify its retention on cellulose fibres, namely: (i) the complexation of CS with iodine and measurement of the absorbency of the ensuing blue solution by UV-vis spectroscopy; (ii) hydrolysis of the starch macromolecules followed by the conversion of the resulting sugars to furan-based molecules and quantifying the ensuing mixture by measuring their absorbance at a Ι of 490 nm, using the same technique as previous one and; finally (iii) hydrolysis of starch macromolecules by trifluoro-acetic acid and quantification of the sugars in the resulting hydrolysates by high performance liquid chromatography. The three methods were found to give similar results within the range of CS addition from 0 to 50 mg per g of cellulose fibres.

  14. The hydrolysis and precipitation of Pd(II) in 0.6 mol kg-1 NaCl: A potentiometric, spectrophotometric, and EXAFS study

    SciTech Connect

    Boily, Jean F.; Seward, Terry M.; Charnock, John M.

    2007-10-15

    The hydrolysis of palladium was investigated in 0.6 mol•kg-1 NaCl at 298.2 K. Potentiometric titrations of solutions at various total concentrations of palladium(II) revealed that dilute (millimolar) conditions can be used to monitor the proton release due to hydrolysis reactions up to 2 protons per palladium(II) as long as the equilibration time is kept small. Spectrophotometric titrations were used to corroborate the homogeneous changes in speciation for the PdCl3OH2- species and to extract its correlative molar absorption coefficients in the 210-320 nm range. The molar absorption coefficients are similar to those of PdCl42- but exhibit a broader distribution of excitation energies resulting from the blue shift of the dominant charge transfer bands due to the presence of OH-. The longer-term potentiometric titrations systematically yielded, on the other hand, precipitates which matured over a period of 6 weeks and resulted in a more extensive release of protons to the solution. Precipitation experiments at six different total palladium(II) concentrations in the 3-11 pH range showed the dominant precipitating phase as Pd(OH)1.72Cl0.28. The coordination environment of Pd in this solid was investigated by extended X-ray absorption fine structure spectroscopy (EXAFS) and yielded an average 1.75 O and 0.25 Cl per Pd atoms with a Pd-O distance of 2.0 Å and Pd-Cl of 2.1 Å. Finally, the precipitation experiments showed the final products to be of larger solubility than a literature Pd(OH)2 solubility study in which the KCl media induced a solid phase transformation to Pd(OH)1.72Cl0.28. Polynuclear complexes Pdq(OH)r2q-r with q=r=[3,9] explain the combined precipitation and hydrolysis data and may represent subsets of [Pd(OH)2]n and/or [Pd(OH)1.72Cl0.28]n chains coiled into nanometer-sized spheroids previously described in the literature.

  15. Automated titration method for use on blended asphalts

    DOEpatents

    Pauli, Adam T.; Robertson, Raymond E.; Branthaver, Jan F.; Schabron, John F.

    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.

  16. Rapid Clozapine Titration in Patients with Treatment Refractory Schizophrenia.

    PubMed

    Poyraz, Cana Aksoy; Özdemir, Armağan; Sağlam, Nazife Gamze Usta; Turan, Şenol; Poyraz, Burç Çağrı; Tomruk, Nesrin; Duran, Alaattin

    2016-06-01

    The aim of this study is to evaluate the safety and effectiveness of rapid clozapine titration in patients with schizophrenia in hospital settings. We conducted a retrospective two-center cohort study to compare the safety and effectiveness of clozapine with different titration rates in treatment-refractory patients with schizophrenia. In the first center, clozapine was started at 25-50 mg followed by 50-100 mg as needed every 6 h on day 1, followed by increases of 50-100 mg/day. In the second center, titration was slower; clozapine initiated with 12.5-50 mg on day 1 followed by increases of 25-50 mg/day. The number of days between starting of clozapine until discharge was shorter in the rapid titration group (22.4 ± 8.72 vs 27.0 ± 10.5, p = 0.1). Number of days of total hospital stay were significantly shorter in the rapid titration group (29.6 ± 10.6 vs 41.2 ± 14.8, p = 0.002). Hypotension was more common in the rapid titration group and one patient had suspected myocarditis. Rapid clozapine titration appeared safe and effective. The length of stay following initiation of clozapine was shorter in the rapid-titration group, although this was not statistically significant. However starting clozapine earlier together with rapid titration has significantly shortened the length of hospital stay in patients with treatment refractory schizophrenia.

  17. Thermodynamics of the lysozyme--salt interaction from calorimetric titrations.

    PubMed

    Boncina, Matjaz; Lah, Jurij; Rescic, Jurij; Vlachy, Vojko

    2010-04-01

    It is well-known that the addition of salts influences the properties of proteins in solution. The essential nature of this phenomenon is far from being fully understood, partly due to the absence of the relevant thermodynamic information. To help fill this gap, in this work isothermal titration calorimetry (ITC) was employed to study the ion-lysozyme association in aqueous buffer solutions at pH = 4.0. ITC curves measured for NaCl, NaBr, NaI, NaNO3, NaSCN, KCl, CaCl2, and BaCl2 salts at three different temperatures were described by a model assuming two sets of independent binding sites on the lysozyme. The resulting thermodynamic parameters of binding of anions (counterions) to the first class of sites (N approximately 7) indicate that the binding constant (K approximately 102 M-1) increases in the order Cl- < Br- < I- < NO3- < SCN-. The anion-lysozyme association is entropy driven, accompanied by a small favorable enthalpy contribution and a positive change in heat capacity. It seems that the entropy and heat capacity increase is due to the water released upon binding, while the net exothermic effect originates from the anion-NH3+ pair formation. Moreover, the results reveal that the nature of the cation has little effect on the thermodynamics of the anion-lysozyme association under the given experimental conditions. Taken together, it seems that the observed thermodynamics of association is a result of a combination of both electrostatic and short-range interactions. The anion ordering reflects the strength of water mediated interactions between anions and lysozyme.

  18. Modified screen-printed ion selective electrodes for potentiometric determination of sodium dodecylsulfate in different samples.

    PubMed

    Ali, Tamer Awad; Mohamed, Gehad G

    2015-01-01

    Fabrication and general performance characteristics of novel screen-printed sensors for potentiometric determination of sodium dodecylsulfate (SDS) are described. The sensors are based on the use of ion-association complexes of SDS with cetylpyridinium chloride (electrode I) and cetyltrimethylammonium bromide (electrode II) as exchange sites in a screen-printed electrode matrix. Electrodes (I) and (II) show fast, stable, and near-Nernstian response for the mono-charge anion of SDS over the concentration range of 1×10(-2) - 5.8×10(-7) and 1×10(-2)-6.3×10(-7) mol/L at 25°C and the pH range of 2.0-9.0 and 2.0-8.0 with anionic slope of 57.32±0.81 and 56.58±0.65 mV/decade, respectively. Electrodes (I) and (II) have lower LODs of 5.8×10(-7) and 6.3×10(-7) mol/L and response times of about 8 and 13 s, respectively. Shelf life of 5 months for both electrodes is adequate. Selectivity coefficients of SDS related to a number of interfering cations, and some inorganic compounds were investigated. There were negligible interferences caused by most of the investigated species. The direct determination of 0.10-13.50 mg of SDS by electrodes (I) and (II) shows average recoveries of 99.96 and 99.85%, and mean RSDs of 0.83 and 1.04%, respectively. In the present investigation, both electrodes were used successfully as end point indicators for determination of SDS in pure pharmaceutical preparations and real spiked water samples. The results obtained using the proposed sensors to determine SDS in solution compared favorably with those obtained by the standard addition method.

  19. Potentiometric surface of the lower Patapsco Aquifer in southern Maryland, September 1991

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, D.C.; Mack, Frederick K.

    1993-01-01

    A map showing the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1991 was prepared from water levels measured in 53 wells. The potentiometric surface was at least 125 feet above sea level near the northwestern boundary and outcrop area of the aquifer in a topographically high area of Prince Georges County, and at least 87 ft above sea level in a similar setting in Anne Arundel County. From these high areas, the potentiometric surface declined to the south and southeast toward large well fields at Severndale, Annapolis, Waldorf, La Plata, Indian Head, and Morgantown.

  20. Potentiometric surface of the upper Patapsco Aquifer in southern Maryland, September 1991

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, D.C.; Mack, Frederick K.

    1993-01-01

    A map showing the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1991 was prepared from water levels measured in wells. The potentiometric surface was at least 70 feet above sea level near the northwestern boundary and outcrop area of the aquifer in a topographically high area of Anne Arundel County, and at least 56 feet above sea level in a similar setting in Prince Georges County. From these high areas, the potentiometric surface declined to the south and southeast toward large well fields in the Annapolis and Waldorf areas and at the Chalk Point powerplant.

  1. Map showing the potentiometric surface of the Aquia Aquifer, May 19-23, 1980

    USGS Publications Warehouse

    Chapelle, Frank; Drummond, Dave; Curley, Tracey

    1981-01-01

    The map is based on water level measurements made May 19-23, 1980. The well network used included 83 wells which have been screened in the Aquia aquifer (Aquia Formation of Paleocene Age). Highest levels of the potentiometric surface, 20 to 35 feet above sea level, were measured near the outcrop or subcrop of the aquifer in the topographically high areas of Anne Arundel and Prince Georges Counties. The potentiometric surface slopes to the southeast. Four separate and extensive cones of depression have developed in the potentiometric surface in the vicinities of Lexington Park, Leonardtown, Prince Frederick, and Chesapeake Beach. The cones of Leonardtown and Lexington Park seem to be merging. (USGS)

  2. Potentiometric surface of the Floridan Aquifer, Southwest Florida Water Management District, September 1980

    USGS Publications Warehouse

    Yobbi, D.K.; Woodham, W.M.; Schiner, George R.

    1980-01-01

    A September 1980 potentiometric-surface map of the Southwest Florida Water Management District depicts the annual high water-level period. Potentiometric levels rose 1 to 31 feet between May 1980 and September 1980 in the citrus and farming sections of southern Hillsborough, northern Hardee, southwestern Polk, northwestern DeSoto, and Manatee Counties. Water levels in these areas are widely affected by reduced pumping for irrigation and have the greatest range in fluctuations. Generally, potentiometric levels were lower than previous September levels except in Citrus, eastern Levy, and western Marion Counties where levels were 0 to 8 feet higher. (USGS)

  3. Potentiometric surface of the Floridan Aquifer, Southwest Florida Water Management District, September 1979

    USGS Publications Warehouse

    Yobbi, D.K.; Woodham, W.M.; Laughlin, Charles P.

    1979-01-01

    A September 1979 potentiometric-surface map of the Southwest Florida Water Management District depicts the annual high water-level period. Potentiometric levels increased 1 to 20 feet between May 1979 and September 1979, in the citrus and farming sections of southern Hillsborough, northern Hardee, southwestern Polk, northwestern DeSoto, and Manatee Counties. Water levels in these areas are widely affected by pumping for irrigation and have the greatest range in fluctuations. Water-level increases ranged from 0 to 7 feet in coastal, northern, and southern areas of the Water Management District. Generally, potentiometric levels were higher than previous September levels due to heavy rains in August and September. (USGS)

  4. The acid-base titration of montmorillonite

    NASA Astrophysics Data System (ADS)

    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

  5. Automated analysis of calorimetric demicellization titrations.

    PubMed

    Textor, Martin; Keller, Sandro

    2015-09-15

    Determination of the critical micellar concentration of surfactants and of the heat of demicellization by means of isothermal titration calorimetry usually involves either calculation of the first derivative of the heat of demicellization with respect to surfactant concentration or application of a generic sigmoidal fit to the demicellization isotherm. Here, we show that a combination of both approaches provides an unbiased and reproducible data analysis strategy without the need for user input other than the calorimetric data proper. The approach is explained and exemplified using demicellization isotherms of the fluorinated surfactant F6OPC (3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluoro-n-octylphosphocholine) and the zwitterionic detergent CHAPSO (3-([3-cholamidopropyl]dimethylammonio)-2-hydroxy-1-propanesulfonate).

  6. Production and titration of lentiviral vectors.

    PubMed

    Salmon, Patrick; Trono, Didier

    2006-11-01

    Lentiviral vectors have emerged over the last decade as powerful, reliable and safe tools for stable gene transfer in a wide variety of mammalian cells. Unlike other vectors derived from oncoretroviruses, they allow for stable gene delivery into most nondividing primary cells, including neurons. This is why LVs are becoming the most useful and promising tools in the field of neuroscience, not only for research, but also for future gene and cell therapy approaches. Lentivectors (LVs) derived from HIV-1 have gradually evolved to display many desirable features aimed at increasing both their safety and their versatility. These latest designs are reviewed in this unit. This unit also describes protocols for production and titration of LVs that can be implemented in a research laboratory setting, with an emphasis on standardization to improve transposability of results between laboratories.

  7. Killed poliovirus antigen titration in humans.

    PubMed

    Salk, J; Cohen, H; Fillastre, C; Stoeckel, P; Rey, J L; Schlumberger, M; Nicolas, A; van Steenis, G; van Wezel, A L; Triau, R; Saliou, P; Barry, L F; Moreau, J P; Mérieux, C

    1978-01-01

    To establish the antigen content of a killed poliovirus vaccine sufficiently potent to induce immunity with one or two doses and to establish a reference standard vaccine which has been tested under field conditions, a titration was carried out in infants to determine the amount of each of the three antigenic types of poliovirus vaccine required to induce seroconversion with a single dose. It has been observed that over a critical range of antigen concentration there is an essentially linear relationship between antibody response and quantity of antigen administered. More than 90 percent of the groups studied had detectable antibody after receiving single injections of 80, 8 and 64 D-antigen units of Types I, II and III, respectively. Four-fold less antigen for each of the three types was less effective. The implications of these findings for an efficient immunization procedure are discussed.

  8. Rapid method for SV40 titration.

    PubMed

    Drayman, Nir; Kler, Slava; Ben-nun-Shaul, Orly; Oppenheim, Ariella

    2010-03-01

    SV40 titer is determined traditionally by the conventional plaque assay. Plaques appear after several rounds of infection and the assay takes around two weeks, which may delay research. A simpler assay was developed, based on detection of T-antigen in the infected cells by flow cytometry. Cells grown in 6-well plates are infected with serial dilutions of the viral stock, harvested 48h post-infection, stained and analyzed for T-antigen using a flow cytometer. The viral titer is calculated based on the percentage of T-antigen positive cells. The procedure is accomplished in 2 days. Unexpectedly we found that titers on different permissive African Green Monkey kidney cell lines were consistently different, suggesting variable susceptibility to SV40 infection. The method described, optimized for SV40 titration, may be adapted readily to other viruses.

  9. Isothermal Titration Calorimetry to Characterize Enzymatic Reactions.

    PubMed

    Mazzei, Luca; Ciurli, Stefano; Zambelli, Barbara

    2016-01-01

    Isothermal titration calorimetry (ITC) is a technique that measures the heat released or absorbed during a chemical reaction as an intrinsic probe to characterize any chemical process that involves heat changes spontaneously occurring during the reaction. The general features of this method to determine the kinetic and thermodynamic parameters of enzymatic reactions (kcat, KM, ΔH) are described and discussed here together with some detailed applications to specific cases. ITC does not require any modification or labeling of the system under analysis, can be performed in solution, and needs only small amounts of enzyme. These properties make ITC an invaluable, powerful, and unique tool to extend the knowledge of enzyme kinetics to drug discovery.

  10. Isothermal Titration Calorimetry of Chiral Polymeric Nanoparticles.

    PubMed

    Werber, Liora; Preiss, Laura C; Landfester, Katharina; Muñoz-Espí, Rafael; Mastai, Yitzhak

    2015-09-01

    Chiral polymeric nanoparticles are of prime importance, mainly due to their enantioselective potential, for many applications such as catalysis and chiral separation in chromatography. In this article we report on the preparation of chiral polymeric nanoparticles by miniemulsion polymerization. In addition, we describe the use of isothermal titration calorimetry (ITC) to measure the chiral interactions and the energetics of the adsorption of enantiomers from aqueous solutions onto chiral polymeric nanoparticles. The characterization of chirality in nano-systems is a very challenging task; here, we demonstrate that ITC can be used to accurately determine the thermodynamic parameters associated with the chiral interactions of nanoparticles. The use of ITC to measure the energetics of chiral interactions and recognition at the surfaces of chiral nanoparticles can be applied to other nanoscale chiral systems and can provide further insight into the chiral discrimination processes of nanomaterials.

  11. Comparison of a potentiometric and a micromechanical triglyceride biosensor.

    PubMed

    Fernandez, Renny Edwin; Hareesh, Vemulachedu; Bhattacharya, Enakshi; Chadha, Anju

    2009-01-01

    Sensitive biosensors for detection of triglyceride concentration are important. In this paper we report on two types of silicon based triglyceride sensors: an electrolyte-insulator-semiconductor capacitor (EISCAP) which is a potentiometric device and a polysilicon microcantilever. The detection principle for both sensors is based on the enzymatic hydrolysis of triglyceride though the sensing mechanisms are different: electronic for the EISCAP and mechanical for the microcantilever. The characteristics and performances of the two sensors are critically compared. The EISCAP sensor necessitates the presence of a buffer for stable measurements which limits the sensitivity of the sensor at low concentrations of the bioanalyte to 1mM. The cantilever sensor works without a buffer which improves the lower level of sensitivity to 10 microm. Both sensors are found to give reproducible and reliable results.

  12. Revised potentiometric-surface map, Yucca Mountain and vicinity, Nevada

    USGS Publications Warehouse

    Ervin, E.M.; Luckey, R.R.; Burkhardt, D.J.

    1993-01-01

    The revised potentiometric-surface map presented in this report updates earlier maps of the Yucca Mountain area using mainly 1988 average water levels. Because of refinements in the corrections to the water-level measurements, these water levels have increased accuracy and precision over older values. The small-gradient area to the southeast of Yucca Mountain is contoured with a 0.25-meter interval and ranges in water-level altitude from 728.5 to 731.0 meters. Other areas with different water levels, to the north and west of Yucca Mountain, are illustrated with shaded patterns. The potentiometric surface can be divided into three regions: 1) A small-gradient area to the southeast of Yucca Mountain, which may be explained by flow through high-transmissivity rocks or low ground-water flux through the area; 2) A moderate-gradient area, on the western side of Yucca Mountain, where the water-level altitude ranges from 775 to 780 meters, and appears to be impeded by the Solitario Canyon Fault and a splay of that fault; and 3) A large-gradient area, to the north-northeast of Yucca Mountain, where water level altitude ranges from 738 to 1,035 meters, possibly as a result of a semi-perched groundwater system. Water levels from wells at Yucca Mountain were examined for yearly trends (1986-89) using linear least-squares regression. Data from five wells exhibited trends which were statistically significant, but some of those may be a result of slow equilibration of the water level from drilling in less permeable rocks. Adjustments for temperature and density changes in the deep wells with long fluid columns were attempted, but some of the adjusted data did not fit the surrounding data and, thus, were not used.

  13. Revised potentiometric-surface map, Yucca Mountain and vicinity, Nevada

    SciTech Connect

    Ervin, E.M.; Luckey, R.R.; Burkhardt, D.J.

    1994-12-01

    The revised potentiometric-surface map presented in this report updates earlier maps of the Yucca Mountain area using mainly 1988 average water levels. Because of refinements in the corrections to the water-level measurements, these water levels have increased accuracy and precision over older values. The small-gradient area to the southeast of Yucca Mountain is contoured with a 0.25-meter interval and ranges in water-level altitude from 728.5 to 73 1.0 meters. Other areas with different water levels, to the north and west of Yucca Mountain, are illustrated with shaded patterns. The potentiometric surface can be divided into three regions: (1) A small-gradient area to the southeast of Yucca Mountain, which may be explained by flow through high-transmissivity rocks or low ground-water flux through the area; (2) A moderate-gradient area, on the western side of Yucca Mountain, where the water-level altitude ranges from 775 to 780 meters, and appears to be impeded by the Solitario Canyon Fault and a splay of that fault; and (3) A large-gradient area, to the north-northeast of Yucca Mountain, where water level altitude ranges from 738 to 1,035 meters, possibly as a result of a semi-perched groundwater system. Water levels from wells at Yucca Mountain were examined for yearly trends using linear least-squares regression. Data from five wells exhibited trends which were statistically significant, but some of those may be a result of slow equilibration of the water level from drilling in less permeable rocks. Adjustments for temperature and density changes in the deep wells with long fluid columns were attempted, but some of the adjusted data did not fit the surrounding data and, thus, were not used.

  14. Microdroplet-Based Potentiometric Redox Measurements on Gold Nanoporous Electrodes.

    PubMed

    Freeman, Christopher J; Farghaly, Ahmed A; Choudhary, Hajira; Chavis, Amy E; Brady, Kyle T; Reiner, Joseph E; Collinson, Maryanne M

    2016-04-01

    Potentiometric redox measurements were made in subnanoliter droplets of solutions using an optically transparent nanoporous gold electrode strategically mounted on the stage of an inverted microscope. Nanoporous gold was prepared via dealloying gold leaf with concentrated nitric acid and was chemisorbed to a standard microscope coverslip with (3-mercaptopropyl)trimethoxysilane. The gold surface was further modified with 1-hexanethiol to optimize hydrophobicity of the surface to allow for redox measurements to be made in nanoscopic volumes. Time traces of the open-circuit potential (OCP) were used to construct Nernst plots to evaluate the applicability of the droplet-based potentiometric redox measurement system. Two poised one-electron transfer systems (potassium ferricyanide/ferrocyanide and ferrous/ferric ammonium sulfate) yielded Nernstian slopes of -58.5 and -60.3 mV, respectively, with regression coefficients greater than 0.99. The y-intercepts of the two agreed well to the formal potential of the two standard oxidation-reduction potential (ORP) calibrants, ZoBell's and Light's solution. The benzoquinone and hydroquinone redox couple was examined as a representative two-electron redox system; a Nernst slope of -30.8 mV was obtained. Additionally, two unpoised systems (potassium ferricyanide and ascorbic acid) were studied to evaluate the system under conditions where only one form of the redox couple is present in appreciable concentrations. Again, slopes near the Nernstian values of -59 and -29 mV, respectively, were obtained. All experiments were carried out using solution volumes between 280 and 1400 pL with injection volumes between 8 and 100 pL. The miniscule volumes allowed for extremely rapid mixing (<305 ms) as well. The small volumes and rapid mixing along with the high accuracy and sensitivity of these measurements lend support to the use of this approach in applications where time is a factor and only small volumes are available for testing. PMID

  15. Continuous on-line feedback based flow titrations. Complexometric titrations of calcium and magnesium.

    PubMed

    Jo, Kyoo Dong; Dasgupta, Purnendu K

    2003-05-28

    The methodology of continuous feedback-based flow titrations and the principle of compensating errors [Anal. Chem. 72 (2000) 4713; Anal. Chim. Acta 435 (2001) 289] were applied to the determination of calcium and magnesium ions with EDTA. The flow of the titrant, EDTA, varied linearly in response to a controller output voltage while the total flow (F(T), the sum of the metal ion sample flow and the titrant flow) was held constant. The sample was pre-doped with a metal ion indicator; the status of the indicator color in the mixed stream was monitored by an optical detector and was used for governing the controller output as well as for interpreting the results of the titrations. The titrant flow initially ramped upward linearly. As a change in the color corresponding to the equivalence point was sensed by the detector, the controller output (instantaneous value V(H)) reversed its ramp direction, thus decreasing the titrant flow linearly at the same ramp rate. When the predefined absorbance corresponding to the equivalence point was sensed again, the controller voltage (instantaneous value V(L)) was ramped in reverse once more, going upward. Because of the lag time between a change in the controller output and its effect being sensed by the detector, the controller voltage corresponding to the actual equivalence point was the average of V(H) and V(L). Continuous sensor-governed operation of the controller resulted in a triangular waveform. The mean of this waveform during any cycle gives the equivalence point controller voltage V(E). This principle allowed true titrations with good reproducibility (0.2-0.7% R.S.D.) and throughput (33-42 s per titration).

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

    PubMed

    Herrera, Isaac; Winnik, Mitchell A

    2016-03-10

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

  17. Students' integration of multiple representations in a titration experiment

    NASA Astrophysics Data System (ADS)

    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.

  18. Microscale pH Titrations Using an Automatic Pipet.

    ERIC Educational Resources Information Center

    Flint, Edward B.; Kortz, Carrie L.; Taylor, Max A.

    2002-01-01

    Presents a microscale pH titration technique that utilizes an automatic pipet. A small aliquot (1-5 mL) of the analyte solution is titrated with repeated additions of titrant, and the pH is determined after each delivery. The equivalence point is determined graphically by either the second derivative method or a Gran plot. The pipet can be…

  19. A Closer Look at Acid-Base Olfactory Titrations

    ERIC Educational Resources Information Center

    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.

  20. pH Static Titration: A Quasistatic Approach

    ERIC Educational Resources Information Center

    Michalowski, Tadeusz; Toporek, Marcin; Rymanowski, Maciej

    2007-01-01

    The pH-static titration is applicable to those systems where at least two types of reactions occur in comparable intensities. The commonalities in titrimetric procedure realized according to pH-static titration, irrespective of the kind of chemical processes occurring are discussed.

  1. Quantitative Analysis of Sulfate in Water by Indirect EDTA Titration

    ERIC Educational Resources Information Center

    Belle-Oudry, Deirdre

    2008-01-01

    The determination of sulfate concentration in water by indirect EDTA titration is an instructive experiment that is easily implemented in an analytical chemistry laboratory course. A water sample is treated with excess barium chloride to precipitate sulfate ions as BaSO[subscript 4](s). The unprecipitated barium ions are then titrated with EDTA.…

  2. A novel view of pH titration in biomolecules.

    PubMed

    Onufriev, A; Case, D A; Ullmann, G M

    2001-03-27

    When individual titratable sites in a molecule interact with each other, their pH titration can be considerably more complex than that of an independent site described by the classical Henderson-Hasselbalch equation. We propose a novel framework that decomposes any complex titration behavior into simple standard components. The approach maps the set of N interacting sites in the molecule onto a set of N independent, noninteracting quasi-sites, each characterized by a pK'(a) value. The titration curve of an individual site in the molecule is a weighted sum of Henderson-Hasselbalch curves corresponding to the quasi-sites. The total protonation curve is the unweighted sum of these Henderson-Hasselbalch curves. We show that pK'(a) values correspond to deprotonation constants available from methods that can be used to assess total proton uptake or release, and establish their connection to protonation curves of individual residues obtained by NMR or infrared spectroscopy. The new framework is tested on a small molecule diethylenetriaminepentaacetate (DTPA) exhibiting nonmonotonic titration curves, where it gives an excellent fit to experimental data. We demonstrate that the titration curve of a site in a group of interacting sites can be accurately reconstructed, if titration curves of the other sites are known. The application of the new framework to the protein rubredoxin demonstrates its usefulness in calculating and interpreting complicated titration curves.

  3. New method for titration of virus infectivity by immunostaining.

    PubMed

    Usuba, O; Schulman, J L; Deatly, A M; Bona, C A; Moran, T M

    1990-01-01

    We have developed a new method for titration of viruses utilizing automated microtiter technology. Compared to existing methods such as plaque assay or hemagglutination titration of influenza virus, the new method offers distinct advantages in terms of time and effort. In addition because multiple replicates can easily be employed accuracy can be increased.

  4. Characterization of binding interactions by isothermal titration calorimetry.

    PubMed

    Doyle

    1997-02-01

    Isothermal titration calorimetry is a high-accuracy method for measuring binding affinities. Titration calorimetry is a universal method that has broad impact throughout biotechnology. In recent years, microcalorimeters that are capable of characterizing binding interactions of biological macromolecules have become commercially available. Results from these studies are providing new insight into the molecular nature of macromolecular interactions.

  5. Spectrophotometric Titration of a Mixture of Calcium and Magnesium.

    ERIC Educational Resources Information Center

    Fulton, Robert; And Others

    1986-01-01

    Describes a spectrophotometric titration experiment which uses a manual titration spectrophotometer and manually operated buret, rather than special instrumentation. Identifies the equipment, materials, and procedures needed for the completion of the experiment. Recommends the use of this experiment in introductory quantitative analysis…

  6. Potentiometric map of the Coffee Sand Aquifer in northeastern Mississippi, October and November 1978

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    This potentiometric map of the Coffee Sand aquifer in northeastern Mississippi is the fourth in a series of maps, prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources, Bureau of Land and Water Resources, delineating the potentiometric surfaces of the major aquifers in Mississippi. In the outcrop areas the potentiometric surface is strongly affected by recharge from precipitation, topography, and drainage of the aquifer by streams. The potentiometric surface slopes generally to the west away from the area of outcrop and is mildly affected by moderate ground-water withdrawals by wells in Tippah and Union County. Historically, water levels in or near the outcrop of the Coffee Sand have shown little or no long-term changes as shown by a hydrograph of one well in Alcorn County. In the downdip part of the aquifer water-level declines of 2 feet per year are common. (USGS)

  7. Galvanostatic entrapment of penicillinase into polytyramine films and its utilization for the potentiometric determination of penicillin.

    PubMed

    Ismail, Fatma; Adeloju, Samuel B

    2010-01-01

    A sensitive and reliable potentiometric biosensor for determination of penicillin has been developed by exploiting the self-limiting growth of the non-conducting polymer, polytyramine. Optimum polytyramine-penicillinase (PTy-PNCnase) films for potentiometric detection of penicillin were accomplished with monomer solutions which contained 0.03 M tyramine, 37 U/mL penicillinase, 0.01 M KNO3, and 3 mM penicillin with an applied current density of 0.8 mA/cm2 and an electropolymerisation time of 40 seconds. The potentiometric biosensor gave a linear concentration range of 3-283 μM for penicillin and achieved a minimum detectable concentration of 0.3 μM. The biosensor was successfully utilized for the detection of Amoxycillin and gave an average percentage recovery of 102±6%. Satisfactory recoveries of penicillin G were also achieved in milk samples with the potentiometric biosensor when concentrations are ≥20 ppm.

  8. Potentiometric surface of Floridan Aquifer, Southwest Florida Water Management District and adjacent areas, May 1979

    USGS Publications Warehouse

    Wolansky, R.M.; Mills, L.R.; Woodham, W.M.; Laughlin, C.P.

    1979-01-01

    A May 1979 potentiometric-surface map depicts the annual low water-level period. Potentiometric levels declined 4 to 21 feet between September 1978 and May 1979, in the citrus and farming sections of southern Hillsborough, northern Hardee, southwestern Polk, northwestern DeSoto, and Manatee Counties. Water levels in these areas are widely affected by pumping for irrigation and have the greatest range in fluctuations. Water-level declines ranged from 0 to 6 feet in coastal, northern, and southern areas of the Water Management District. Generally potentiometric levels were higher than previous May levels due to heavy rains in April and May. In parts of Hillsborough, Pasco, and Pinellas Counties, May 1979 potentiometric levels were 18 feet higher than those of September 1978. (USGS)

  9. Investigation of the interaction between sodium dodecyl sulfate and cationic polymers.

    PubMed

    Lee, Jungno; Moroi, Yoshikiyo

    2004-05-25

    Aggregation properties of sodium dodecyl sulfate (SDS) on a cationic hydroxyethyl cellulose, Polyquaternium-10 (PQ-10), of low charge density were studied by potentiometric and pyrene fluorescence methods and compared with those of poly(diallyldimethylammomium chloride) (PDADMAC) of high charge density. The critical aggregation concentration (cac) was measured with the potentiometric method and further confirmed with the fluorescence method. The former was found to be more accurate. The value of the cac for the SDS/PQ-10 system was measured at 100, 200, and 400 ppm polymer and at 288.2,298.2, and 308.2 K. They showed almost the same cac value, 0.04 mmol dm-3. The I1/I3 value of the pyrene fluorescence spectrum in the SDS/PQ-10 system at higher SDS concentration was smaller than that in SDS/PDADMAC solution and much larger than that of water. From the binding isotherm by the potentiometric method, the free DS- concentration (Cf) and the bound DS- concentration (Cb) could be evaluated with ease over the SDS concentration range above the cac. The aggregation number of DS- aggregates for both the above polymers was evaluated from the fluorescence quenching method using the values of Cf and Cb from the potentiometric method. Because Cf in the SDS/PQ-10 system above the cac did not maintain a constant value contrary to that in the SDS/PDADMAC system but increased quite a lot, Cb should not be regarded as [SDS] - cac above the cac. The aggregation number in the SDS/PQ-10 system increased almost linearly with increasing total concentration of SDS, while that in the SDS/PDADMAC system reached a plateau. With increasing temperature, the aggregation number of the SDS/PDADMAC system decreased more rapidly than that of the SDS/PQ-10 system. PMID:15969141

  10. Total Acid Value Titration of Hydrotreated Biomass Fast Pyrolysis Oil: Determination of Carboxylic Acids and Phenolics with Multiple End-Point Detection

    SciTech Connect

    Christensen, E.; Alleman, T. L.; McCormick, R. L.

    2013-01-01

    Total acid value titration has long been used to estimate corrosive potential of petroleum crude oil and fuel oil products. The method commonly used for this measurement, ASTM D664, utilizes KOH in isopropanol as the titrant with potentiometric end point determination by pH sensing electrode and Ag/AgCl reference electrode with LiCl electrolyte. A natural application of the D664 method is titration of pyrolysis-derived bio-oil, which is a candidate for refinery upgrading to produce drop in fuels. Determining the total acid value of pyrolysis derived bio-oil has proven challenging and not necessarily amenable to the methodology employed for petroleum products due to the different nature of acids present. We presented an acid value titration for bio-oil products in our previous publication which also utilizes potentiometry using tetrabutylammonium hydroxide in place of KOH as the titrant and tetraethylammonium bromide in place of LiCl as the reference electrolyte to improve the detection of these types of acids. This method was shown to detect numerous end points in samples of bio-oil that were not detected by D664. These end points were attributed to carboxylic acids and phenolics based on the results of HPLC and GC-MS studies. Additional work has led to refinement of the method and it has been established that both carboxylic acids and phenolics can be determined accurately. Use of pH buffer calibration to determine half-neutralization potentials of acids in conjunction with the analysis of model compounds has allowed us to conclude that this titration method is suitable for the determination of total acid value of pyrolysis oil and can be used to differentiate and quantify weak acid species. The measurement of phenolics in bio-oil is subject to a relatively high limit of detection, which may limit the utility of titrimetric methodology for characterizing the acidic potential of pyrolysis oil and products.

  11. Modeling Precipitation and Sorption of Al, U and Co-contaminants during Titration of Acidic Sediments in Recirculation Flow-Through Experiments

    SciTech Connect

    Tang, Guoping; Luo, Wensui; Brooks, Scott C; Watson, David B; Gu, Baohua

    2013-01-01

    We conducted batch and recirculating column titration tests with contaminated acidic sediments with controlled CO2 in the headspace, and extended the geochemical model by Gu et al. (2003, GCA) to better understand and quantify the reactions governing trace metal fate in the subsurface. The sediment titration curve showed slow pH increase due to strong buffering by Al precipitation and CO2 uptake. Assuming precipitation of basaluminite at low saturation index (SI=-4), and decreasing cation exchange selectivity coefficient (kNa\\Al=0.3), the predictions are close to the observed pH and Al; and the model explains 1) the observed Ca, Mg, and Mn concentration decrease by cation exchange with sorbed Al, and 2) the decrease of U by surface complexation with Fe hydroxides at low pH, and precipitation as liebigite (Ca2UO2(CO3)3:10H2O) at pH>5.5. Without further adjustment geochemical parameters, the model describes reasonably well previous sediment and column titration tests without CO2 in the headspace, as well as the new large column test. The apparent inhibition of U and Ni decrease in the large column can be explained by formation of aqueous carbonate complexes and/or competition with carbonate for surface sites. These results indicated that ignoring labile solid phase Al would underestimate base requirement in titration of acidic aquifers.

  12. Comparative study of ZnO nanorods and thin films for chemical and biosensing applications and the development of ZnO nanorods based potentiometric strontium ion sensor

    NASA Astrophysics Data System (ADS)

    Khun, K.; Ibupoto, Z. H.; Chey, C. O.; Lu, Jun.; Nur, O.; Willander, M.

    2013-03-01

    In this study, the comparative study of ZnO nanorods and ZnO thin films were performed regarding the chemical and biosensing properties and also ZnO nanorods based strontium ion sensor is proposed. ZnO nanorods were grown on gold coated glass substrates by the hydrothermal growth method and the ZnO thin films were deposited by electro deposition technique. ZnO nanorods and thin films were characterised by field emission electron microscopy [FESEM] and X-ray diffraction [XRD] techniques and this study has shown that the grown nanostructures are highly dense, uniform and exhibited good crystal quality. Moreover, transmission electron microscopy [TEM] was used to investigate the quality of ZnO thin film and we observed that ZnO thin film was comprised of nano clusters. ZnO nanorods and thin films were functionalised with selective strontium ionophore salicylaldehyde thiosemicarbazone [ST] membrane, galactose oxidase, and lactate oxidase for the detection of strontium ion, galactose and L-lactic acid, respectively. The electrochemical response of both ZnO nanorods and thin films sensor devices was measured by using the potentiometric method. The strontium ion sensor has exhibited good characteristics with a sensitivity of 28.65 ± 0.52 mV/decade, for a wide range of concentrations from 1.00 × 10-6 to 5.00 × 10-2 M, selectivity, reproducibility, stability and fast response time of 10.00 s. The proposed strontium ion sensor was used as indicator electrode in the potentiometric titration of strontium ion versus ethylenediamine tetra acetic acid [EDTA]. This comparative study has shown that ZnO nanorods possessed better performance with high sensitivity and low limit of detection due to high surface area to volume ratio as compared to the flat surface of ZnO thin films.

  13. Developments in the Field of Conducting and Non-conducting Polymer Based Potentiometric Membrane Sensors for Ions Over the Past Decade

    PubMed Central

    Faridbod, Farnoush; Ganjali, Mohammad Reza; Dinarvand, Rassoul; Norouzi, Parviz

    2008-01-01

    Many research studies have been conducted on the use of conjugated polymers in the construction of chemical sensors including potentiometric, conductometric and amperometric sensors or biosensors over the last decade. The induction of conductivity on conjugated polymers by treating them with suitable oxidizing agents won Heeger, MacDiarmid and Shirakawa the 2000 Nobel Prize in Chemistry. Common conjugated polymers are poly(acetylene)s, poly(pyrrole)s, poly(thiophene)s, poly(terthiophene)s, poly(aniline)s, poly(fluorine)s, poly(3-alkylthiophene)s, polytetrathiafulvalenes, poly-napthalenes, poly(p-phenylene sulfide), poly(p-phenylenevinylene)s, poly(3,4-ethylene-dioxythiophene), polyparaphenylene, polyazulene, polyparaphenylene sulfide, poly-carbazole and polydiaminonaphthalene. More than 60 sensors for inorganic cations and anions with different characteristics based on conducting polymers have been reported. There have also been reports on the application of non-conducting polymers (nCPs), i.e. PVC, in the construction of potentiometric membrane sensors for determination of more than 60 inorganic cations and anions. However, the leakage of ionophores from the membranes based on these polymers leads to relatively lower life times. In this article, we try to give an overview of Solid-Contact ISE (SCISE), Single-Piece ISE (SPISE), Conducting Polymer (CP)-Based, and also non-conducting polymer PVC-based ISEs for various ions which their difference is in the way of the polymer used with selective\\ membrane. In SCISEs and SPISEs, the plasticized PVC containing the ionophore and ionic additives govern the selectivity behavior of the electrode and the conducting polymer is responsible of ion-to-electron transducer. However, in CPISEs, the conducting polymer layer is doped with a suitable ionophore which enhances the ion selectivity of the CP while its redox response has to be suppressed.

  14. Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, September 2007

    USGS Publications Warehouse

    Kinnaman, Sandra L.; Dixon, Joann F.

    2008-01-01

    This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for September 2007. Potentiometric contours are based on water-level measurements collected at 554 wells during the period September 15-27, near the end of the wet season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to ground-water withdrawals and spring flow. Potentiometric-surface highs generally correspond to topographic highs where the aquifer is recharged. Springs and areas of diffuse upward leakage naturally discharge water from the aquifer and are most prevalent along the St. Johns River. Areas of discharge are reflected by depressions in the potentiometric surface. Ground-water withdrawals locally have lowered the potentiometric surface. Ground water in the Upper Floridan aquifer generally flows from potentiometric highs to potentiometric lows in a direction perpendicular to the contours.

  15. Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, Florida, September 2008

    USGS Publications Warehouse

    Kinnaman, Sandra L.; Dixon, Joann F.

    2009-01-01

    This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for September 2008. Potentiometric contours are based on water-level measurements collected at 589 wells during the period September 15-25, near the end of the wet season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to ground-water withdrawals and spring flow. Potentiometric-surface highs generally correspond to topographic highs where the aquifer is recharged. Springs and areas of diffuse upward leakage naturally discharge water from the aquifer and are most prevalent along the St. Johns River. Areas of discharge are reflected by depressions in the potentiometric surface. Ground-water withdrawals locally have lowered the potentiometric surface. Ground water in the Upper Floridan aquifer generally flows from potentiometric highs to potentiometric lows in a direction perpendicular to the contours.

  16. An improved apparatus for intragastric titration in the conscious dog.

    PubMed

    Daly, M J; Hartley, R W; Stables, R

    1980-01-01

    An apparatus for automatic intragastric titration with on-line display of results has been described. The apparatus has been validated by titration of exogenous acid injected into the test meal in a reservoir and in vivo by assessing the secretory response of a dog with a gastric fistula to a test meal. A titration display unit provides a record of the secretory response both as a digital printout and a bar chart display. Cimetidine (2 mg kg-1h-1) significantly reduced the secretory response to a test meal.

  17. Novel titration method for surface-functionalised silica

    NASA Astrophysics Data System (ADS)

    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 NH2-, SO3H- 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.

  18. Automatic photometric titrations of calcium and magnesium in carbonate rocks

    USGS Publications Warehouse

    Shapiro, L.; Brannock, W.W.

    1955-01-01

    Rapid nonsubjective methods have been developed for the determination of calcium and magnesium in carbonate rocks. From a single solution of the sample, calcium is titrated directly, and magnesium is titrated after a rapid removal of R2O3 and precipitation of calcium as the tungstate. A concentrated and a dilute solution of disodium ethylenediamine tetraacetate are used as titrants. The concentrated solution is added almost to the end point, then the weak solution is added in an automatic titrator to determine the end point precisely.

  19. Isothermal calorimetric titrations on charge-assisted halogen bonds: role of entropy, counterions, solvent, and temperature.

    PubMed

    Walter, Sebastian M; Kniep, Florian; Rout, Laxmidhar; Schmidtchen, Franz P; Herdtweck, Eberhardt; Huber, Stefan M

    2012-05-23

    We have conducted isothermal calorimetric titrations to investigate the halogen-bond strength of cationic bidentate halogen-bond donors toward halides, using bis(iodoimidazolium) compounds as probes. These data are intended to aid the rational design of halogen-bond donors as well as the development of halogen-bond-based applications in solution. In all cases examined, the entropic contribution to the overall free energy of binding was found to be very important. The binding affinities showed little dependency on the weakly coordinating counteranions of the halogen-bond donors but became slightly stronger with higher temperatures. We also found a marked influence of different solvents on the interaction strength. The highest binding constant detected in this study was 3.3 × 10(6) M(-1).

  20. Investigation of Ligand Binding to the Multidrug Resistance Protein EmrE by Isothermal Titration Calorimetry

    PubMed Central

    Sikora, Curtis W.; Turner, Raymond J.

    2005-01-01

    Escherichia coli multidrug resistance protein E (EmrE) is an integral membrane protein spanning the inner membrane of Escherichia coli that is responsible for this organism's resistance to a variety of lipophilic cations such as quaternary ammonium compounds (QACs) and interchelating dyes. EmrE is a 12-kDa protein of four transmembrane helices considered to be functional as a multimer. It is an efflux transporter that can bind and transport cytoplasmic QACs into the periplasm using the energy of the proton gradient across the inner membrane. Isothermal titration calorimetry provides information about the stoichiometry and thermodynamic properties of protein-ligand interactions, and can be used to monitor the binding of QACs to EmrE in different membrane mimetic environments. In this study the ligand binding to EmrE solubilized in dodecyl maltoside, sodium dodecyl sulfate and reconstituted into small unilamellar vesicles is examined by isothermal titration calorimetry. The binding stoichiometry of EmrE to drug was found to be 1:1, demonstrating that oligomerization of EmrE is not necessary for binding to drug. The binding of EmrE to drug was observed with the dissociation constant (KD) in the micromolar range for each of the drugs in any of the membrane mimetic environments. Thermodynamic properties demonstrated this interaction to be enthalpy-driven with similar enthalpies of 8–12 kcal/mol for each of the drugs in any of the membrane mimetics. PMID:15501941

  1. Investigation of ligand binding to the multidrug resistance protein EmrE by isothermal titration calorimetry.

    PubMed

    Sikora, Curtis W; Turner, Raymond J

    2005-01-01

    Escherichia coli multidrug resistance protein E (EmrE) is an integral membrane protein spanning the inner membrane of Escherichia coli that is responsible for this organism's resistance to a variety of lipophilic cations such as quaternary ammonium compounds (QACs) and interchelating dyes. EmrE is a 12-kDa protein of four transmembrane helices considered to be functional as a multimer. It is an efflux transporter that can bind and transport cytoplasmic QACs into the periplasm using the energy of the proton gradient across the inner membrane. Isothermal titration calorimetry provides information about the stoichiometry and thermodynamic properties of protein-ligand interactions, and can be used to monitor the binding of QACs to EmrE in different membrane mimetic environments. In this study the ligand binding to EmrE solubilized in dodecyl maltoside, sodium dodecyl sulfate and reconstituted into small unilamellar vesicles is examined by isothermal titration calorimetry. The binding stoichiometry of EmrE to drug was found to be 1:1, demonstrating that oligomerization of EmrE is not necessary for binding to drug. The binding of EmrE to drug was observed with the dissociation constant (K(D)) in the micromolar range for each of the drugs in any of the membrane mimetic environments. Thermodynamic properties demonstrated this interaction to be enthalpy-driven with similar enthalpies of 8-12 kcal/mol for each of the drugs in any of the membrane mimetics.

  2. Influences of Probe’s Morphology for Metal Ion Detection Based on Light-Addressable Potentiometric Sensors

    PubMed Central

    Shao, Chen; Zhou, Shuang; Yin, Xuebo; Gu, Yajun; Jia, Yunfang

    2016-01-01

    The sensing mechanism of binding Hg2+ into thymine-thymine (T-T) mismatched base pairs was introduced into a light-addressable potentiometric sensor (LAPS) with anti-Hg2+ aptamer as the sensing units. Three kinds of T-rich single-strand DNA (ssDNA) chains with different spacer lengths, from 0 to 12 –CH2 groups, were designed to investigate surface charge and morphological effects on the LAPS’ output. First, by comparing the responding of LAPS modified with three kinds of ssDNA, it was found that the best performance for Hg2+ sensing was exhibited by the probe without –CH2 groups. The detection limit of Hg2+ ion was 1 ppt under the optimal condition. Second, the cooperative effects of surface charge and morphology on the output were observed by the controlled experiments. The two effects were the negative charge balanced by metal cations and the morphological changing caused by the formation of T-Hg2+-T structure. In conclusion, not only the influences of the aptamer probe’s morphology and surface charge was investigated on the platform of LAPS, but also sensing Hg2+ ions was achieved for the first time by the presented aptamer LAPS. PMID:27187412

  3. Potentiometric detection and removal of copper using porphyrins

    PubMed Central

    2013-01-01

    Background Copper is an essential trace element with a great importance in industry, environment and biological systems. The great advantage of ion-selective sensors in comparison with other proposed techniques is that they are measuring the free metal ion activity which is responsible for their toxicity. Porphyrins are known to be among the best ionophores in formulation of ion-selective sensors. Results A symmetrically substituted meso-porphyrin, namely: 5,10,15,20-tetrakis(4-allyloxyphenyl)porphyrin (TAPP) was used in the construction of a new copper selective-sensor and was also tested for the removal of copper from waste waters. The potentiometric response characteristics (slope and selectivity) of copper-selective electrodes based on TAPP in o-nitrophenyloctylether (o-NPOE), dioctyl phtalate (DOP) and dioctyl sebacate (DOS) plasticized with poly(vinyl chloride) membranes are compared. Conclusions The best results were obtained for the membrane plasticized with DOP. The sensor has linear response in the range 1x10-7 – 1x10-1 M with 28.4 ± 0.4 mV/decade near-Nernstian slope towards copper ions and presents good selectivity. Due to its chelating nature, the same porphyrin was also tested for the retention of copper from synthetic copper samples, showing a maximum adsorption capacity of 280 mg/g. PMID:23829792

  4. A potentiometric biosensor for rapid on-site disease diagnostics.

    PubMed

    Tarasov, Alexey; Gray, Darren W; Tsai, Meng-Yen; Shields, Niall; Montrose, Armelle; Creedon, Niamh; Lovera, Pierre; O'Riordan, Alan; Mooney, Mark H; Vogel, Eric M

    2016-05-15

    Quantitative point-of-care (POC) devices are the next generation for serological disease diagnosis. Whilst pathogen serology is typically performed by centralized laboratories using Enzyme-Linked ImmunoSorbent Assay (ELISA), faster on-site diagnosis would infer improved disease management and treatment decisions. Using the model pathogen Bovine Herpes Virus-1 (BHV-1) this study employs an extended-gate field-effect transistor (FET) for direct potentiometric serological diagnosis. BHV-1 is a major viral pathogen of Bovine Respiratory Disease (BRD), the leading cause of economic loss ($2 billion annually in the US only) to the cattle and dairy industry. To demonstrate the sensor capabilities as a diagnostic tool, BHV-1 viral protein gE was expressed and immobilized on the sensor surface to serve as a capture antigen for a BHV-1-specific antibody (anti-gE), produced in cattle in response to viral infection. The gE-coated immunosensor was shown to be highly sensitive and selective to anti-gE present in commercially available anti-BHV-1 antiserum and in real serum samples from cattle with results being in excellent agreement with Surface Plasmon Resonance (SPR) and ELISA. The FET sensor is significantly faster than ELISA (<10 min), a crucial factor for successful disease intervention. This sensor technology is versatile, amenable to multiplexing, easily integrated to POC devices, and has the potential to impact a wide range of human and animal diseases.

  5. Potentiometric study of antioxidant activity: development and prospects.

    PubMed

    Ivanova, A V; Gerasimova, E L; Brainina, Kh Z

    2015-01-01

    The increasing interest in the study of the antioxidant activity of different objects is caused by an unbalance between the formation of reactive oxygen species (ROS) and the performance of the antioxidant system in humans under certain conditions, which leads to oxidative stress and pathological states of the organism. This article presents a brief critical review of the methods that are used to measure integrated antioxidant activity (AOA). It is shown that the most promising methods for measuring AOA are electrochemical ones, particularly potentiometry, as it best fits the nature of the processes causing oxidative stress. The article gives the theoretical rational for requirements that an oxidizer of antioxidants (AO) should meet. The work presents the thermodynamic grounds for the use of an earlier proposed mediator system, kinetics of chemical reactions between AO and the mediator system. In order to confirm reliability and accuracy of the results, numerous correlation studies were conducted, aiming to compare the data obtained with the use the proposed method and independent analytical methods. The article presents the results of the potentiometric study of AOA for a variety of objects, including individual antioxidant → nutritional supplements → food → blood and blood fractions.

  6. A potentiometric biosensor for rapid on-site disease diagnostics.

    PubMed

    Tarasov, Alexey; Gray, Darren W; Tsai, Meng-Yen; Shields, Niall; Montrose, Armelle; Creedon, Niamh; Lovera, Pierre; O'Riordan, Alan; Mooney, Mark H; Vogel, Eric M

    2016-05-15

    Quantitative point-of-care (POC) devices are the next generation for serological disease diagnosis. Whilst pathogen serology is typically performed by centralized laboratories using Enzyme-Linked ImmunoSorbent Assay (ELISA), faster on-site diagnosis would infer improved disease management and treatment decisions. Using the model pathogen Bovine Herpes Virus-1 (BHV-1) this study employs an extended-gate field-effect transistor (FET) for direct potentiometric serological diagnosis. BHV-1 is a major viral pathogen of Bovine Respiratory Disease (BRD), the leading cause of economic loss ($2 billion annually in the US only) to the cattle and dairy industry. To demonstrate the sensor capabilities as a diagnostic tool, BHV-1 viral protein gE was expressed and immobilized on the sensor surface to serve as a capture antigen for a BHV-1-specific antibody (anti-gE), produced in cattle in response to viral infection. The gE-coated immunosensor was shown to be highly sensitive and selective to anti-gE present in commercially available anti-BHV-1 antiserum and in real serum samples from cattle with results being in excellent agreement with Surface Plasmon Resonance (SPR) and ELISA. The FET sensor is significantly faster than ELISA (<10 min), a crucial factor for successful disease intervention. This sensor technology is versatile, amenable to multiplexing, easily integrated to POC devices, and has the potential to impact a wide range of human and animal diseases. PMID:26765531

  7. New potentiometric sensors based on selective recognition sites for determination of ephedrine in some pharmaceuticals and biological fluids.

    PubMed

    Hassan, Saad S M; Kamel, Ayman H; Abd El-Naby, Heba

    2013-01-15

    New cost-effective potentiometric membrane sensors with cylindrical configuration responsive to ephedrine are described. The sensors setup is, based on the use of triacetyl-β-cyclodextrin [(triacetyl-β-CD)] as a neutral ionophore embedded in a plasticized poly (vinyl chloride) (PVC) matrix (sensor I) and carboxylated poly(vinyl chloride) [(PVC-COOH)] as a simultaneous plastic matrix and ion exchanger (sensor II). Both sensors showed significant enhancement of response towards ephedrinium cation (EPD(+)) over a concentration range of 3.0 × 10(-5)-8.0 × 10(-3) mol L(-1) at pH 4-9 and 3-8 with low detection limits of 5.7 × 10(-6) and 6.2 × 10(-6) mol L(-1) for sensors (I) and (II), respectively. The sensors displayed near-Nernstian cationic slope of 57.0 and 55.6 mV decade(-1) for EPD(+) and the effects of lipophilic salts and various foreign common ions were examined. The sensors were also satisfactorily used as tubular detectors in a double channel flow injection system. The intrinsic characteristics of the detectors in a low dispersion manifold under hydrodynamic mode of operation were determined and compared with data obtained under batch mode of operation. Validation of the method revealed good performance characteristics including long life span, good selectivity for EPD(+) over a wide variety of other organic compounds, long term stability, high reproducibility, fast response, low detection limit, wide measurement range, acceptable accuracy and precision. Applications of the sensors to the determination of EPD(+) in pharmaceutical formulations and spiked biological fluid samples were carried out and compared with standard techniques. Notably, the sensors introduced offer several advantages over many of those previously described that are amenable to quality control/quality assurance assessment of the homogeneity, stability and purity of ephedrine drug tablets.

  8. Modeling the acid-base properties of bacterial surfaces: A combined spectroscopic and potentiometric study of the gram-positive bacterium Bacillus subtilis.

    PubMed

    Leone, Laura; Ferri, Diego; Manfredi, Carla; Persson, Per; Shchukarev, Andrei; Sjöberg, Staffan; Loring, John

    2007-09-15

    In this study, macroscopic and spectroscopic data were combined to develop a surface complexation model that describes the acid-base properties of Bacillus subtilis. The bacteria were freeze-dried and then resuspended in 0.1 M NaCl ionic medium. Macroscopic measurements included potentiometric acid-base titrations and electrophoretic mobility measurements. In addition, ATR-FTIR spectra of wet pastes from suspensions of Bacillus subtilis at different pH values were collected. The least-squares program MAGPIE was used to generate a surface complexation model that takes into account the presence of three acid-base sites on the surface: tripple bond COOH, tripple bond NH+, and tripple bond PO-, which were identified previously by XPS measurements. Both potentiometric titration data and ATR-FTIR spectra were used quantitatively, and electrostatic effects at the charged bacterial surface were accounted for using the constant capacitance model. The model was calculated using two different approaches: in the first one XPS data were used to constrain the ratio of the total concentrations of all three surface sites. The capacitance of the double layer, the total buffer capacity, and the deprotonation constants of the tripple bond NH+, tripple bond POH, and tripple bond COOH species were determined in the fit. A second approach is presented in which the ratio determined by XPS of the total concentrations of tripple bond NH+ to tripple bond PO- sites is relaxed. The total concentration of tripple bond PO- sites was determined in the fit, while the deprotonation constant for tripple bond POH was manually varied until the minimization led to a model which predicted an isoelectric point that resulted in consistency with electrophoretic mobility data. The model explains well the buffering capacity of Bacillus subtilis suspensions in a wide pH range (between pH=3 and pH=9) which is of considerable environmental interest. In particular, a similar quantitative use of the IR data

  9. A Titration Technique for Demonstrating a Magma Replenishment Model.

    ERIC Educational Resources Information Center

    Hodder, A. P. W.

    1983-01-01

    Conductiometric titrations can be used to simulate subduction-setting volcanism. Suggestions are made as to the use of this technique in teaching volcanic mechanisms and geochemical indications of tectonic settings. (JN)

  10. THE TITRATION OF YELLOW FEVER VIRUS IN STEGOMYIA MOSQUITOES

    PubMed Central

    Davis, Nelson C.; Frobisher, Martin; Lloyd, Wray

    1933-01-01

    Titrations were made of yellow fever virus in stegomyia mosquitoes, using rhesus monkeys as test animals. It was found that: (a) The average mosquito immediately after engorging on highly infectious blood contained between 1 and 2 million lethal doses of virus. The titer of freshly ingested blood was as high as 1 billion lethal doses of virus per cubic centimeter. (b) During the fortnight succeeding a meal on infectious blood there occurred a reduction of titratable virus to not more than 1 per cent of that present in the freshly fed insects. (c) The titer was somewhat higher at later periods. This rise in titer signified possibly not a multiplication, but merely an increase of extracellular virus and of that easily freed by grinding to a titratable form. (d) At no later stage did the quantity of titratable virus equal that demonstrable in freshly fed insects. PMID:19870190

  11. Microscope Titration and Extraction of DNA from Liver.

    ERIC Educational Resources Information Center

    Mayo, Lois T.; And Others

    1993-01-01

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

  12. Automatic Titrators in the Analytical and Physical Chemistry Laboratories

    NASA Astrophysics Data System (ADS)

    Williams, Kathryn R.

    1998-09-01

    In 1995 the University of Florida received an NSF-ILI grant to purchase six automatic titrators, which have now been successfully integrated into the analytical and physical chemistry teaching laboratories. After they have mastered fundamental techniques, students in the introductory analytical laboratory gain experience with automated analyses in three experiments: the iodimetric analysis of ascorbic acid, the determination of polymer molecular weight, and the analysis of chloride by ion selective electrode. The titrators are also used in the instrumental analysis laboratory for Karl Fischer titrations and the coulometric analysis of EDTA. A physical chemistry experiment, the kinetics of methyl acetate hydrolysis, has also been modified for use with the titrators Instructor write-ups for all experiments may be obtained via JCE Online.

  13. Potentiometric map of the Winona-Tallahatta Aquifer in northwestern Mississippi, fall 1979

    USGS Publications Warehouse

    Wasson, B.E.

    1980-01-01

    The potentiometric map of the Winona-Tallahatta aquifer is one of a series of maps, prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources , Bureau of Land and Water Resources, delineating the potentiometric surfaces of the major aquifers in Mississippi. In the outcrop area of the Winona-Tallahatta aquifer the potentiometric surface is strongly affected by recharge from precipitation, by topography, and by drainage of the aquifer by streams. The potentiometric surface slopes downward generally to the west away from the area of outcrop and is strongly affected by recharge from precipitation, by topography, and by drainage of the aquifer by streams. The potentiometric surface slopes downward generally to the west away from the area of outcrop and is strongly affected by pumpage from wells in Leflore, Sunflower , and Bolivar Counties, Historically, water levels in or near the outcrop of the Winona-Tallahatta have shown little or no long-term changes, but the heavy withdrawals in the confined part of the aquifer have caused long-term water-level declines of 1 to 2 feet per year. (USGS)

  14. Highly sensitive covalently functionalized light-addressable potentiometric sensor for determination of biomarker.

    PubMed

    Liang, Jintao; Guan, Mingyuan; Huang, Guoyin; Qiu, Hengming; Chen, Zhengcheng; Li, Guiyin; Huang, Yong

    2016-06-01

    A biomarker is related to the biological status of a living organism and shows great promise for the early prediction of a related disease. Herein we presented a novel structured light-addressable potentiometric sensor (LAPS) for the determination of a model biomarker, human immunoglobulin G (hIgG). In this system, the goat anti-human immunoglobulin G antibody was used as recognition element and covalently immobilized on the surface of light-addressable potentiometric sensor chip to capture human immunoglobulin G. Due to the light addressable capability of light-addressable potentiometric sensor, human immunoglobulin G dissolved in the supporting electrolyte solution can be detected by monitoring the potential shifts of the sensor. In order to produce a stable photocurrent, the laser diode controlled by field-programmable gate array was used as the light emitter to drive the light-addressable potentiometric sensor. A linear correlation between the potential shift response and the concentration of human immunoglobulin G was achieved and the corresponding regression equation was ΔV (V)=0.00714ChIgG (μg/mL)-0.0147 with a correlation coefficient of 0.9968 over a range 0-150 μg/mL. Moreover, the light-addressable potentiometric sensor system also showed acceptable stability and reproducibility. All the results demonstrated that the system was more applicable to detection of disease biomarkers with simple operation, multiple-sample format and might hold great promise in various environmental, food, and clinical applications.

  15. Intrinsic thermodynamics of 4-substituted-2,3,5,6-tetrafluorobenzenesulfonamide binding to carbonic anhydrases by isothermal titration calorimetry.

    PubMed

    Zubrienė, Asta; Smirnovienė, Joana; Smirnov, Alexey; Morkūnaitė, Vaida; Michailovienė, Vilma; Jachno, Jelena; Juozapaitienė, Vaida; Norvaišas, Povilas; Manakova, Elena; Gražulis, Saulius; Matulis, Daumantas

    2015-10-01

    Para substituted tetrafluorobenzenesulfonamides bind to carbonic anhydrases (CAs) extremely tightly and exhibit some of the strongest known protein-small ligand interactions, reaching an intrinsic affinity of 2 pM as determined by displacement isothermal titration calorimetry (ITC). The enthalpy and entropy of binding to five CA isoforms were measured by ITC in two buffers of different protonation enthalpies. The pKa values of compound sulfonamide groups were measured potentiometrically and spectrophotometrically, and enthalpies of protonation were measured by ITC in order to evaluate the proton linkage contributions to the observed binding thermodynamics. Intrinsic means the affinity of a sulfonamide anion for the Zn bound water form of CAs. Fluorination of the benzene ring significantly enhanced the observed affinities as it increased the fraction of deprotonated ligand while having little impact on intrinsic affinities. Intrinsic enthalpy contributions to the binding affinity were dominant over entropy and were more exothermic for CA I than for other CA isoforms. Thermodynamic measurements together with the X-ray crystallographic structures of protein-ligand complexes enabled analysis of structure-activity relationships in this enzyme ligand system.

  16. Geochemical modeling of reactions and partitioning of trace metals and radionuclides during titration of contaminated acidic sediments

    SciTech Connect

    Zhang, Fan; Parker, Jack C.; Brooks, Scott C; Watson, David B; Jardine, Philip M; Gu, Baohua

    2008-01-01

    This study investigated sorption of uranium and technetium onto aluminum and iron hydroxides during titration of a contaminated groundwater using both Na hydroxide and carbonate as titrants. The contaminated groundwater has a low pH of 3.8 and high concentrations of NO3-, SO42-, Al, Ca, Mg, Mn, trace metals such as Ni and Co, and radionuclides such as U and Tc. During titration, most Al and Fe were precipitated out at pH above ~4.5. U as well as Tc was found to be removed from aqueous phase at pH below ~5.5, but to some extent released at higher pH values. An earlier geochemical equilibrium reaction path model that considered aqueous complexation and precipitation/dissolution reactions predicted mineral precipitation and adequately described concentration variations of Al, Fe and some other metal cations, but failed to predict sulfate, U and Tc concentrations during titration. Previous studies have shown that Fe- and Al-oxyhydroxides strongly sorb dissolved sulfate, U and Tc species. Therefore, an anion exchange model was developed for the sorption of sulfate, U and Tc onto Al and Fe hydroxides. With the additional consideration of the anion exchange reactions, concentration profiles of sulfate, U and Tc were more accurately predicted. Results of this study indicate that consideration of complex reactions such as sorption/desorption on mixed mineral phases, in addition to hydrolysis and precipitation, could improve the prediction of various contaminants during pre- and post-groundwater treatment practices.

  17. Functionalized β-cyclodextrin based potentiometric sensor for naproxen determination.

    PubMed

    Lenik, Joanna; Łyszczek, Renata

    2016-04-01

    Potentiometric sensors based on neutral β-cyclodextrins: (2-hydroxypropyl)-β-cyclodextrin, heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, heptakis(2,3,6-tri-O-benzoyl)-β-cyclodextrin and anionic β-cyclodextrin: (2-hydroxy-3-N,N,N-trimethylamino)propyl-β-cyclodextrin chloride for naproxen are described. Inclusion complexes of naproxen with the above-mentioned cyclodextrins were studied using IR spectroscopy. The electrode surface was made from PVC membranes doped with the appropriate β-cyclodextrin as ionophores and quaternary ammonium chlorides as positive charge additives that were dispersed in plasticizers. The optimum membrane contains heptakis(2,3,6-tri-O-benzoyl)-β-cyclodextrin, o-nitrophenyloctyl ether and tetraoctyl ammonium chloride as a lipophilic salt. The electrode is characterized by a Nernstian response slope of -59.0 ± 0.5 mV decade(-1) over the linear range of 5.0 × 10(-5)-1.0 × 10(-2) mol L(-1) and the detection limit 1.0 × 10(-5) mol L(-1), as well as the response time 10s. It can be used in the pH range 6.2-8.5 for 10 months without any considerable deterioration. Incorporation of β-cyclodextrins improved the electrode selectivity towards naproxen ions from several inorganic and organic interferents and some common drug excipients due to concovalent interactions (host molecule-guest molecule). The notable advantages of the naproxen-selective electrode include its high sensitivity, high selectivity, cost-effectiveness as well as accurate and comfortable application in drug analysis and milk samples. PMID:26838835

  18. Real-time potentiometric detection of bacteria in complex samples.

    PubMed

    Zelada-Guillén, Gustavo A; Bhosale, Suryakant V; Riu, Jordi; Rius, F Xavier

    2010-11-15

    Detecting and identifying pathogen bacteria is essential to ensure quality at all stages of the food chain and to diagnose and control microbial infections. Traditional detection methods, including those based on cell culturing, are tedious and time-consuming, and their further application in real samples generally implies more complex pretreatment steps. Even though state-of-the-art techniques for detecting microorganisms enable the quantification of very low concentrations of bacteria, to date it has been difficult to obtain successful results in real samples in a simple, reliable, and rapid manner. In this Article, we demonstrate that the label-free detection and identification of living bacteria in real samples can be carried out in a couple of minutes and in a direct, simple, and selective way at concentration levels as low as 6 colony forming units/mL (CFU) in complex matrices such as milk or 26 CFU/mL in apple juice where the pretreatment step of samples is extremely easy. We chose Escherichia coli ( E. coli ) CECT 675 cells as a model organism as a nonpathogenic surrogate for pathogenic E. coli O157:H7 to test the effectiveness of a potentiometric aptamer-based biosensor. This biosensor uses single-walled carbon nanotubes (SWCNT) as excellent ion-to-electron transducers and covalently immobilized aptamers as biorecognition elements. The selective aptamer-target interaction significantly changes the electrical potential, thus allowing for both interspecies and interstrain selectivity and enabling the direct detection of the target. This technique is therefore a powerful tool for the immediate identification and detection of microorganisms. We demonstrate the highly selective detection of living bacteria with an immediate linear response of up to 10(4) CFU/mL. The biosensor can be easily built and used, is regenerated without difficulty, and can be used at least five times with no loss in the minimum amount of detected bacteria.

  19. Potentiometric surface of the Ozark aquifer in northern Arkansas, 2010

    USGS Publications Warehouse

    Czarnecki, John B.; Pugh, Aaron L.; Blackstock, Joshua M.

    2014-01-01

    The Ozark aquifer in northern Arkansas is composed of dolomite, limestone, sandstone, and shale of Late Cambrian to Middle Devonian age and ranges in thickness from approximately 1,100 feet to more than 4,000 feet. Hydrologically, the aquifer is complex, characterized by discrete and discontinuous flow components with large variations in permeability. The potentiometric-surface map, based on 56 well and 5 spring water-level measurements made in 2010 in Arkansas and Missouri, has a maximum water-level altitude measurement of 1,174 feet in Carroll County and a minimum water-level altitude measurement of 120 feet in Randolph County. Regionally, the flow within the aquifer is to the south and southeast in the eastern and central part of the study area and to the west, northwest, and north in the western part of the study area. Water-level altitudes changed 0.5 feet or less in 31 out of 56 wells measured between 2007 and 2010. Despite rapidly increasing population within the study area, the increase appears to have minimal effect on groundwater levels, although the effect may have been minimized by the development and use of surface-water distribution infrastructure, suggesting that most of the incoming populations are fulfilling their water needs from surface-water sources. The conversion of some users from groundwater to surface water may be allowing water levels in some wells to recover (rise) or decline at a slower rate in some areas such as in Benton, Carroll, and Washington Counties.

  20. Potentiometric map of the Gordo Aquifer in northeastern Mississippi, September, October, and November 1978

    USGS Publications Warehouse

    Wasson, B.E.

    1979-01-01

    This potentiometric map of the Gordo aquifer in northeastern Mississippi is the second in a series of maps, prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources, Bureau of Land and Water Resources, delineating the potentiometric surfaces of the major aquifers in Mississippi. The potentiometric surface of the Gordo aquifer slopes generally to the west away from the outcrop area and it is depressed generally by large ground-water withdrawals in the Tupelo and Columbus areas. Historically, water levels in or near the outcrop of the Gordo aquifer have shown little or no long-term changes. Heavy withdrawals from the downdip area have caused long-term water-level declines of 1 to 2 feet per year in much of the confined part of the aquifer. Water-level decline in one observation well in Tupelo has averaged about 5 feet per year since 1966. (USGS)

  1. Potentiometric Surface of the Upper Patapsco Aquifer in Southern Maryland, September 2001

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2002-01-01

    This report presents a map showing the potentiometric surface of the Upper Patapsco aquifer in the Patapsco Formation of Cretaceous age in Southern Maryland during September 2001. The map is based on water-level measurements in 49 wells. The potentiometric surface was highest at 118 feet above sea level near the northern boundary and outcrop area of the aquifer in northern Anne Arundel County. From this area, the potentiometric surface declined to the southeast toward large well fields in the Annapolis area, and from all directions toward a cone of depression located southwest of Waldorf. The ground-water level declined to 26 feet below sea level in the Annapolis area, and the lowest water level was 132 feet below sea level southwest of Waldorf.

  2. Potentiometric surface of the upper Patapsco aquifer in southern Maryland, September 1999

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2001-01-01

    This report presents a map showing the potentiometric surface of the Upper Patapsco aquifer in the Patapsco Formation of Cretaceous age in Southern Maryland during September 1999. The map is based on water-level measurements in 49 wells. The potentiometric surface was 119 feet above sea level near the northern boundary and outcrop area of the aquifer in a topographically high area of Anne Arundel County, and 55 feet above sea level in a similar setting in Prince Georges County. From these high areas, the potentiometric surface declined to the southeast toward large well fields in the Annapolis area, and from all directions toward a cone of depression southwest of Waldorf. Ground-water levels declined to 20 feet below sea level in the Annapolis area, and 131 feet below sea level southwest of Waldorf.

  3. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 1995

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Mack, Frederick K.

    1996-01-01

    A map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Cretaceous age in southern Maryland during September 1995 was prepared from water-level measurements in 92 wells. The potentiometric surface was highest near the northwestern boundaryand outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties. Regionally, the potentiometric surface sloped gently downward towards the southeast and the local gradients were directed toward the centers of three cones of depression that have developed in response to pumping. These cones were centeredaround well fields in the Annapolis, Waldorf, and Chalk Point areas. Ground-water levels were as low as 63 feet below sea level in the Waldorf area, more than 50 feet below sea level at Chalk Point, and almost 20 feet below sea level near Annapolis.

  4. Potentiometric surface of the Magothy Aquifer in southern Maryland during September 1988

    USGS Publications Warehouse

    Mack, Frederick K.; Andreasen, David C.; Curtin, Stephen E.; Wheeler, Judith C.

    1990-01-01

    A map showing the potentiometric surface of the Magothy aquifer in southern Maryland during the fall of 1988 was prepared from water-level measurements in 83 observation wells. The potentiometric surface was highest near the northwest boundary and outcrop area of the aquifer in topographically high locations of Anne Arundel and Prince Georges Counties. The hydraulic gradient in the study area was generally southeastward or toward the centers of three cones of depression that have developed in response to pumping stresses. These cones formed around well fields in the Annapolis, Waldorf, and Chalk Point areas. The potentiometric surface of the Magothy aquifer was more than 40 ft below sea level in parts of the Waldorf and Chalk Point areas. (USGS)

  5. Potentiometric surface of the Magothy Aquifer in southern Maryland, September 1991

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, D.C.; Mack, Frederick K.

    1993-01-01

    A map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Cretaceous age in southern Maryland during September 1991 was prepared from water levels measured in 89 wells. The potentiometric surface was highest near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties. Regionally, the potentiometric surface sloped gently downward toward the southeast, and the local gradients were directed toward the centers of 3 cones of depression that have developed in response to pumping. These cones were centered around well fields in the Annapolis, Waldorf, and Chalk Point areas. Groundwater levels were more than 50 feet below sea level in the Waldorf area, nearly 50 feet below sea level at Chalk Point, and greater than 10 feet below sea level near Annapolis.

  6. Potentiometric surface of the Magothy Aquifer in southern Maryland during the fall of 1987

    USGS Publications Warehouse

    Mack, Frederick K.; Andreasen, David C.; Curtin, Stephen E.; Wheeler, Judith C.

    1989-01-01

    A map showing the potentiometric surface of the Magothy aquifer in the Cretaceous Magothy Formation in southern Maryland during the fall of 1987 was prepared by using water level measurements in 85 observation wells. The potentiometric surface was highest near the northwestern boundary and outcrop area of the aquifer in topographically high locations of Anne Arundel and Prince Georges Counties. The hydraulic gradient in the study area was generally southeastward or toward the centers of three cones of depression which have developed in response to pumping stresses. These cones formed around well fields in the Annapolis, Waldorf, and Chalk Point areas. The potentiometric surface of the Magothy aquifer was more than 40 ft below sea level in parts of the Waldorf and Chalk Point areas. (USGS)

  7. Potentiometric surface of the Magothy Aquifer in southern Maryland, September 1994

    USGS Publications Warehouse

    Curtin, Stephen E.; Mack, Frederick K.; Andreasen, David C.

    1995-01-01

    A map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Cretaceous age in southern Maryland during September 1994 was prepared from water levels measured in 85 wells. The potentiometric surface was highest near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties. Regionally, the potentiometric surface sloped gently downward toward the southeast, and the local gradients were directed toward the centers of three cones of depression that have developed in response to pumping. These cones were centered around well fields in the Annapolis, Waldorf, and Chalk Point areas. Ground-water levels were as low as 60 feet below sea level in the Waldorf area, more than 45 feet below sea level at Chalk Point, and almost 15 feet below sea level near Annapolis.

  8. Potentiometric surface of the upper Patapsco Aquifer in southern Maryland, September 1994

    USGS Publications Warehouse

    Curtin, Stephen E.; Mack, Frederick K.; Andreasen, David C.

    1995-01-01

    A map showing the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1994 was prepared from water levels measured in 43 wells. The potentiometric surface was at least 70 feet above sea level near the northwestern boundary and outcrop area of the aquifer in a topographically high area of Anne Arundel County, and nearly 60 feet above sea level in a similar setting in Prince Georges County. From these high areas, the potentiometric surface declined to the south and southeast toward large well fields in the Annapolis and Waldorf areas and at the Chalk Point powerplant. Ground-water levels reached nearly 30 feet below sea level in the Annapolis area, nearly 110 feet below sea level southwest of Waldorf, and more than 25 feet below sea level at the Chalk Point powerplant.

  9. Potentiometric measurement of glucose concentration with an immobilized glucose oxidase/catalase electrode.

    PubMed

    Wingard, L B; Liu, C C; Wolfson, S K; Yao, S J; Drash, A L

    1982-01-01

    A series of enzyme electrodes for measurement of glucose have been constructed. The electrodes contain glucose oxidase immobilized on platinum, either with or without co-immobilization of catalase. When placed in buffered glucose, the enzyme electrodes show a potentiometric response to glucose with respect to a Ag/AgCl reference electrode. This response is reproducible in the physiologic range of glucose concentrations. The immobilization technique, some of the environmental variables such as oxygen concentration and pH, and several compounds that might interfere with the selectivity of the enzyme electrodes for glucose have received preliminary study. This direct potentiometric approach is undergoing further evaluation to determine the basic electrochemical mechanism responsible for the potentiometric signal and whether it can be adapted for continuous in vivo monitoring of the glucose concentration in body fluids. PMID:7172983

  10. Potentiometric map of the lower Wilcox aquifer in Mississippi, fall 1982

    USGS Publications Warehouse

    Darden, Daphne

    1986-01-01

    This potentiometric map is the second map of the lower Wilcox aquifer in a series of maps prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources, Bureau of Land and Water Resources, delineating the potentiometric surface of the major aquifers in Mississippi. The potentiometric surface of the lower Wilcox aquifer slopes generally to the west away from the outcrop area and it is marked by a large groundwater cone of depression in the area of Tallahatchie, Quitman, and Panola Counties. Water levels in or near the outcrop of the lower Wilcox aquifer show little longterm change. Heavy withdrawals in the downdip area have caused water level declines of about 1 to 2 feet per year since 1979 in much of the confined part of the aquifer. These water level declines in the area of Tallahatchie, Quitman, and Panola Counties have resulted in a wider cone of depression since 1979. (USGS)

  11. Potentiometric surface of the Floridan Aquifer, Southwest Florida Water Management District, May 1980

    USGS Publications Warehouse

    Yobbi, D.K.; Woodham, W.M.; Schiner, George R.

    1980-01-01

    A May 1980 potentiometric-surface map of the Southwest Florida Water Management District depicts the annual low water-level period. Potentiometric levels decreased 5 to 36 feet between September 1979 and May 1980, in the citrus and farming sections of southern Hillsborough, southwestern Polk, northwestern DeSoto , Hardee, and Manatee Counties. Water levels in these areas are widely affected by pumping for irrigation and have the greatest range in fluctuations. Water-level decreases ranged from 0 to 8 feet in coastal, northern, and southern areas of the Water Management District. Generally, potentiometric levels were lower than previous May levels except in the northernmost and southernmost counties where water levels were 1 to 5 feet higher. (USGS)

  12. Prediction of uranium and technetium sorption during titration of contaminated acidic groundwater

    SciTech Connect

    Zhang, Fan; Parker, Jack C.; Watson, David B; Jardine, Philip M; Gu, Baohua

    2010-01-01

    This study investigates uranium and technetium sorption onto aluminum and iron hydroxides during titration of acidic groundwater. The contaminated groundwater exhibits oxic conditions with high concentrations of NO{sub 3}{sup -}, SO{sub 4}{sup 2-}, U, Tc, and various metal cations. More than 90% of U and Tc was removed from the aqueous phase as Al and Fe precipitated above pH 5.5, but was partially resolublized at higher pH values. An equilibrium hydrolysis and precipitation reaction model adequately described variations in aqueous concentrations of metal cations. An anion exchange reaction model was incorporated to simulate sulfate, U and Tc sorption onto variably charged (pH-dependent) Al and Fe hydroxides. Modeling results indicate that competitive sorption/desorption on mixed mineral phases needs to be considered to adequately predict U and Tc mobility. The model could be useful for future studies of the speciation of U, Tc and co-existing ions during pre- and post-groundwater treatment practices.

  13. Cesium cation affinities and basicities

    NASA Astrophysics Data System (ADS)

    Gal, Jean-François; Maria, Pierre-Charles; Massi, Lionel; Mayeux, Charly; Burk, Peeter; Tammiku-Taul, Jaana

    2007-11-01

    This review focuses on the quantitative data related to cesium cation interaction with neutral or negatively charged ligands. The techniques used for measuring the cesium cation affinity (enthalpies, CCA), and cesium cation basicities (Gibbs free energies, CCB) are briefly described. The quantum chemical calculations methods that were specifically designed for the determination of cesium cation adduct structures and the energetic aspects of the interaction are discussed. The experimental results, obtained essentially from mass spectrometry techniques, and complemented by thermochemical data, are tabulated and commented. In particular, the correlations between cesium cation affinities and lithium cation affinities for the various kinds of ligands (rare gases, polyatomic neutral molecules, among them aromatic compounds and negative ions) serve as a basis for the interpretation of the diverse electrostatic modes of interaction. A brief account of some recent analytical applications of ion/molecule reactions with Cs+, as well as other cationization approaches by Cs+, is given.

  14. Potentiometric surface of the Sparta and Memphis aquifers in eastern Arkansas, April through July 1993

    USGS Publications Warehouse

    Westerfield, Paul W.

    1995-01-01

    A water-level map of the Sparta and Memphis aquifers for 1993 is presented in this map report. The Sparta-Memphis aquifer, consisting of sands of Eocene age, is present in much of southern and eastern Arkansas. The potentiometric surface map and long-term hydrographs illustrate the effects of large withdrawals for industrial and public supply and, to a lesser extent, agricultural use, on water levels in the aquifer. Three cones of depression, centered in Columbia, Jefferson, and Union Counties, occur in the potentiometric surface.

  15. Potentiometric surface of the Magothy aquifer in southern Maryland, September 1999

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2001-01-01

    This report presents a map showing the change in the potentiometric surface of the Lower Patapsco aquifer in the Lower Patapsco Formation of Cretaceous age in Southern Maryland for September 1990 and September 1999. The map, based on water?level measurements in 52 wells, shows that the change of the potentiometric surface during the 9- year period ranged from a rise of 13 feet at Indian Head and 6 feet near the outcrop area in Glen Burnie, to declines of 34 feet at Arnold, 30 feet at Waldorf, and 24 feet at Morgantown.

  16. Construction of a potentiometric glutamate biosensor for determination of glutamate in some real samples.

    PubMed

    Y Lmaz, Demet; Karaku, Emine

    2011-12-01

    The potentiometric glutamate biosensor based on ammonium-selective poly(vinylchloride) (PVC) membrane electrode was constructed by chemically immobilizing glutamate oxidase. Ammonium ions produced after an enzymatic reaction were determined potentiometrically. We determined the optimum working conditions of the biosensor such as buffer concentration, buffer pH, lifetime, response time, linear working range, kinetic constants (K(m) and V(max)) of glutamate oxidase enzyme used for biosensor construction values, and other response characteristics. Additionally, glutamate assay in some real samples such as chicken bullion, healthy human serum, and commercial multipower amino acid mixture were also successfully carried out. The results showed good agreement with previously reported values.

  17. Potentiometric Electronic Tongues for Foodstuff and Biosample Recognition—An Overview

    PubMed Central

    Ciosek, Patrycja; Wróblewski, Wojciech

    2011-01-01

    Potentiometric sensors are attractive tools for the fabrication of various electronic tongues that can be used in wide area of applications, ranging from foodstuff recognition to environmental monitoring and medical diagnostics. Their main advantages are the ability to modify their selectivity (including cross-sensitivity effects) and the possibility of miniaturization using appropriate construction methods for the transducer part (e.g., with the use of solid-state technology). In this overview various examples of the design, performance, and applications of potentiometric electronic tongues are presented. The results summarize recent research in the field conducted in the Department of Microbioanalytics, Warsaw University of Technology (WUT). PMID:22163870

  18. Potentiometric surface of the Floridan Aquifer, Southwest Florida Water Management District and adjacent areas, September 1978

    USGS Publications Warehouse

    Wolansky, R.M.; Mills, L.R.; Woodham, W.M.; Laughlin, C.P.

    1978-01-01

    A September 1978 potentiometric-surface map depicts the annual high water-level period of the Floridan aquifer in the Southwest Florida Management District. Potentiometric levels increased 10 to 25 feet between May 1978 and September 1978, in the citrus and farming sections of southern Hillsborough, northern Hardee, southwestern Polk and Manatee Counties. These areas are widely affected by pumping for irrigation and have the greatest fluctuations in water-levels between the low and high water-level periods. Water-level rises in coastal, northern and southern areas of the Water Management District ranged from 0 to 10 feet. (Woodard-USGS)

  19. Potentiometric surface of Floridan aquifer, Southwest Florida Water Management District and adjacent areas, September 1977

    USGS Publications Warehouse

    Ryder, P.D.; Mills, L.R.; Laughlin, C.P.

    1978-01-01

    A potentiometric-surface map of the Southwest Florida Water Management District depicts the annual high water-level period. Potentiometric levels increased 15 to 30 feet between May 1977 and September 1977 in the citrus and farming sections of southeastern Hillsborough, northern Hardee, and southwestern Polk Counties. These areas are widely affected by pumpage for irrigation and have the greatest range in water-level fluctuations between the low and high water-level periods. Water-level rises in coastal, northern, and southern areas of the Water Management District ranged from 0 to 15 feet. (Woodard-USGS)

  20. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2001

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2002-01-01

    This report presents a map showing the change in the potentiometric surface of the Aquia aquifer in the Aquia Formation of Paleocene age in Southern Maryland for September 1982 and September 2001. The map, based on water level measurements in 58 wells, shows that the potentiometric surface during the 19-year period declined from zero in the northernmost part of the study area, which is the outcrop of the aquifer, to 120 feet at Lexington Park. Lexington Park is near the southeasternmost part of the study area and approaches the downdip boundary of the aquifer.

  1. Complexometric titrations: new reagents and concepts to overcome old limitations.

    PubMed

    Zhai, Jingying; Bakker, Eric

    2016-07-21

    Chelators and end point indicators are the most important parts of complexometric titrations. The most widely used universal chelator ethylenediamine tetraacetic acid (EDTA) and its derivatives can strongly coordinate with different metal ions. Their limited selectivity often requires the use of masking agents, and the multiple pKa values of the chelators necessitate a careful adjustment of pH during the procedure. Real world requirements for pH independent, selective and sensitive chelators and indicators call for a new design of these reagents. New concepts and structures of chelators and indicators have indeed recently emerged. We present here recent developments on chelators and indicators for complexometric titrations. Many of these advances were made possible only recently by moving the titration from a homogeneous to a heterogeneous phase using a new class of chelators and indicators based on highly selective ionophores embedded in ion-selective nanosphere emulsions. In view of achieving titrations in situ by complete instrumental control, thin layer electrochemistry has recently been shown to be an attractive concept that replaces the traditional cumbersome titration protocol with a direct reagent free sensing tool. PMID:27272695

  2. Complexometric titrations: new reagents and concepts to overcome old limitations.

    PubMed

    Zhai, Jingying; Bakker, Eric

    2016-07-21

    Chelators and end point indicators are the most important parts of complexometric titrations. The most widely used universal chelator ethylenediamine tetraacetic acid (EDTA) and its derivatives can strongly coordinate with different metal ions. Their limited selectivity often requires the use of masking agents, and the multiple pKa values of the chelators necessitate a careful adjustment of pH during the procedure. Real world requirements for pH independent, selective and sensitive chelators and indicators call for a new design of these reagents. New concepts and structures of chelators and indicators have indeed recently emerged. We present here recent developments on chelators and indicators for complexometric titrations. Many of these advances were made possible only recently by moving the titration from a homogeneous to a heterogeneous phase using a new class of chelators and indicators based on highly selective ionophores embedded in ion-selective nanosphere emulsions. In view of achieving titrations in situ by complete instrumental control, thin layer electrochemistry has recently been shown to be an attractive concept that replaces the traditional cumbersome titration protocol with a direct reagent free sensing tool.

  3. A mercury(II) selective sensor based on N,N'-bis(salicylaldehyde)-phenylenediamine as neutral carrier for potentiometric analysis in water samples.

    PubMed

    Abu-Shawish, Hazem M

    2009-08-15

    Mercuric ions in water samples were determined by a new modified carbon paste electrode based on N,N'-bis(salicylaldehyde)-phenylenediamine (salophen) as a chemical modifier. The construction, performance, and applications of mercury carbon paste electrode are described. The electrode displays a linear log[Hg(2+)] versus EMF response over a wide concentration range of 3.2 x 10(-7) to 3.2 x 10(-4) with Nernstian slope of 58.8+/-0.3 mV/decade with limit of detection 1.5 x 10(-7) over the pH range 3.8-7.8; the presence of the complex Hg(OH)(+) ion explains the slope of the response curve. The proposed sensor shows a reasonable discrimination ability towards Hg(II) in comparison to some alkali, alkaline earth transition and heavy metal ions. The modified electrode was applied as indicator electrode in potentiometric titration and successfully used to determine mercury(II) in water samples with satisfactory results.

  4. Acidity constants in methanol/water mixtures of polycarboxylic acids used in drug salt preparations. Potentiometric determination of aqueous pKa values of quetiapine formulated as hemifumarate.

    PubMed

    Garrido, Gemma; Ràfols, Clara; Bosch, Elisabeth

    2006-05-01

    The acidic dissociation constants in a number of methanol/water mixtures of mono and polycarboxylic acids commonly used in the preparation of drug salts were determined. These solvent mixtures are usually used to determine the pKa of drugs of low aqueous solubility. However, when these drugs are prepared in salt form, the acid-base equilibria of both the basic drug and the counter-anion are involved in the potentiometric titration curves. In these instances, the inclusion of the pKa of acids as constant values in the curve fitting provides easy computation of the drug pKa without the need of any previous step to get the free base. As an application example, the aqueous pKa values of the quetiapine formulated as hemifumarate (Seroquel) were estimated by extrapolation from the experimental pKa in several methanol/water mixtures, which were then calculated according to the suitable constants of fumaric acid. The estimated aqueous pKa values of quetiapine are compared with those directly obtained in aqueous solution by potentiometry and by capillary electrophoresis.

  5. Map showing how the potentiometric surface of the Magothy Aquifer of August 1980 differed from the potentiometric surface of September 1977, in southern Maryland

    USGS Publications Warehouse

    Mack, Frederick K.; Wheeler, J.C.; Curtin, Stephen E.

    1982-01-01

    The map is based on the differences between two sets of water-level measurements made in 65 observation wells. One set was made in 1977, a relatively dry year, and the other set was made in 1980, another relatively dry year. The map shows that the potentiometric surface was higher in 1980, by as much as 9 feet, than it was in 1977, in a band a few miles wide near the outcrop and subcrop areas of the aquifer in northern Prince Georges County and central Anne Arundel County. In the remainder of the map area, the 1980 potentiometric surface was lower than it had been in 1977, with declines as great as 20 feet measured in well fields at Waldorf and Chalk Point. The network of observation wells was developed and is operated and maintained as part of the cooperative program between the U.S. Geological Survey and agencies of the Maryland Department of Natural Resources. (USGS)

  6. Potentiometric measurement of polymer-membrane electrodes based on lanthanum

    NASA Astrophysics Data System (ADS)

    Saefurohman, Asep; Buchari, Noviandri, Indra; Syoni

    2014-03-01

    Quantitative analysis of rare earth elements which are considered as the standard method that has a high accuracy, and detection limits achieved by the order of ppm is inductively coupled plasma atomic emission spectroscopy (ICPAES). But these tools are expensive and valuable analysis of the high cost of implementation. In this study be made and characterized selective electrode for the determination of rare earth ions is potentiometric. Membrane manufacturing techniques studied is based on immersion (liquid impregnated membrane) in PTFE 0.5 pore size. As ionophores to be used tri butyl phosphate (TBP) and bis(2-etylhexyl) hydrogen phosphate. There is no report previously that TBP used as ionophore in polymeric membrane based lanthanum. Some parameters that affect the performance of membrane electrode such as membrane composition, membrane thickness, and types of membrane materials studied in this research. Manufacturing of Ion Selective Electrodes (ISE) Lanthanum (La) by means of impregnation La membrane in TBP in kerosene solution has been done and showed performance for ISE-La. FTIR spectrum results for PTFE 0.5 pore size which impregnated in TBP and PTFE blank showed difference of spectra in the top 1257 cm-1, 1031 cm-1 and 794.7 cm-1 for P=O stretching and stretching POC from group -OP =O. The result showed shift wave number for P =O stretching of the cluster (-OP=O) in PTFE-TBP mixture that is at the peak of 1230 cm-1 indicated that no interaction bond between hydroxyl group of molecules with molecular clusters fosforil of TBP or R3P = O. The membrane had stable responses in pH range between 1 and 9. Good responses were obtained using 10-3 M La(III) internal solution, which produced relatively high potential. ISE-La showed relatively good performances. The electrode had a response time of 29±4.5 second and could be use for 50 days. The linear range was between 10-5 and 10-1 M.

  7. Potentiometric measurement of polymer-membrane electrodes based on lanthanum

    SciTech Connect

    Saefurohman, Asep Buchari, Noviandri, Indra; Syoni

    2014-03-24

    Quantitative analysis of rare earth elements which are considered as the standard method that has a high accuracy, and detection limits achieved by the order of ppm is inductively coupled plasma atomic emission spectroscopy (ICPAES). But these tools are expensive and valuable analysis of the high cost of implementation. In this study be made and characterized selective electrode for the determination of rare earth ions is potentiometric. Membrane manufacturing techniques studied is based on immersion (liquid impregnated membrane) in PTFE 0.5 pore size. As ionophores to be used tri butyl phosphate (TBP) and bis(2-etylhexyl) hydrogen phosphate. There is no report previously that TBP used as ionophore in polymeric membrane based lanthanum. Some parameters that affect the performance of membrane electrode such as membrane composition, membrane thickness, and types of membrane materials studied in this research. Manufacturing of Ion Selective Electrodes (ISE) Lanthanum (La) by means of impregnation La membrane in TBP in kerosene solution has been done and showed performance for ISE-La. FTIR spectrum results for PTFE 0.5 pore size which impregnated in TBP and PTFE blank showed difference of spectra in the top 1257 cm{sup −1}, 1031 cm{sup −1} and 794.7 cm{sup −1} for P=O stretching and stretching POC from group −OP =O. The result showed shift wave number for P =O stretching of the cluster (−OP=O) in PTFE-TBP mixture that is at the peak of 1230 cm{sup −1} indicated that no interaction bond between hydroxyl group of molecules with molecular clusters fosforil of TBP or R{sub 3}P = O. The membrane had stable responses in pH range between 1 and 9. Good responses were obtained using 10{sup −3} M La(III) internal solution, which produced relatively high potential. ISE-La showed relatively good performances. The electrode had a response time of 29±4.5 second and could be use for 50 days. The linear range was between 10{sup −5} and 10{sup −1} M.

  8. Determination of sulphite in wine by coulometric titration.

    PubMed

    Lowinsohn, D; Bertotti, M

    2001-09-01

    A method for the determination of both free and bound S(IV) in white wine samples by coulometric titration with electrogenerated iodine is described, the S(IV) speciation being performed by extracting SO2 from samples acidified wiith hydrochloric acid. Titrations of samples treated with NaOH led to the total S(IV) concentration, the results being in agreement with the ones obtained by the distillation procedure as well as by using the classical Monier-Williams method. An average recovery of 97% was obtained for samples spiked with S(IV) in the range 0.4-1.2 mM, which demonstrated the validity of the proposed procedure. The repeatability was 1.3% and the limit of detection was estimated as 0.01 mM. Results from direct titrations of wine added to the electrochemical cell are reported, which give indications of the stability of adducts towards the reaction with iodine.

  9. Differential titration of bases in glacial acetic acid.

    PubMed

    Castellano, T; Medwick, T; Shinkai, J H; Bailey, L

    1981-01-01

    A study of bases in acetic acid and their differential titration was carried out. The overall basicity constants for 20 bases were measured in acetic acid, and the differential titration of five binary mixtures of variable delta pKb values in acetic acid was followed using a glass electrode-modified calomel electrode system. Agreement with literature values was good. A leveling diagram was constructed that indicated that bases stronger than aqueous pKb 10 are leveled to an acetous pKb 5.69, whereas weaker bases are not leveled but instead exhibit their own intrinsic basicity, with the acetous pKb to aqueous pKb values being linearly related (slope 1.18, correlation coefficient 0.962). A minimum acetous delta pKb of four units is required for the satisfactory differential titration of two bases in acetic acid.

  10. Cationic cellulose nanofibers from waste pulp residues and their nitrate, fluoride, sulphate and phosphate adsorption properties.

    PubMed

    Sehaqui, Houssine; Mautner, Andreas; Perez de Larraya, Uxua; Pfenninger, Numa; Tingaut, Philippe; Zimmermann, Tanja

    2016-01-01

    Cationic cellulose nanofibers (CNF) having 3 different contents of positively charged quaternary ammonium groups have been prepared from waste pulp residues according to a water-based modification method involving first the etherification of the pulp with glycidyltrimethylammonium chloride followed by mechanical disintegration. The cationic nanofibers obtained were observed by scanning electron microscopy and the extent of the reaction was evaluated by conductometric titration, ζ-potential measurements, and thermogravimetric analyses. The cationic CNF had a maximum cationic charge content of 1.2mmolg(-1) and positive ζ-potential at various pH values. Sorption of negatively charged contaminants (fluoride, nitrate, phosphate and sulphate ions) and their selectivity onto cationic CNF have been evaluated. Maximum sorption of ∼0.6mmolg(-1) of these ions by CNF was achieved and selectivity adsorption studies showed that cationic CNF are more selective toward multivalent ions (PO4(3-) and SO4(2-)) than monovalent ions (F(-) and NO3(-)). In addition, we demonstrated that cationic CNF can be manufactured into permeable membranes capable of dynamic nitrate adsorption by utilizing a simple paper-making process.

  11. Cationic cellulose nanofibers from waste pulp residues and their nitrate, fluoride, sulphate and phosphate adsorption properties.

    PubMed

    Sehaqui, Houssine; Mautner, Andreas; Perez de Larraya, Uxua; Pfenninger, Numa; Tingaut, Philippe; Zimmermann, Tanja

    2016-01-01

    Cationic cellulose nanofibers (CNF) having 3 different contents of positively charged quaternary ammonium groups have been prepared from waste pulp residues according to a water-based modification method involving first the etherification of the pulp with glycidyltrimethylammonium chloride followed by mechanical disintegration. The cationic nanofibers obtained were observed by scanning electron microscopy and the extent of the reaction was evaluated by conductometric titration, ζ-potential measurements, and thermogravimetric analyses. The cationic CNF had a maximum cationic charge content of 1.2mmolg(-1) and positive ζ-potential at various pH values. Sorption of negatively charged contaminants (fluoride, nitrate, phosphate and sulphate ions) and their selectivity onto cationic CNF have been evaluated. Maximum sorption of ∼0.6mmolg(-1) of these ions by CNF was achieved and selectivity adsorption studies showed that cationic CNF are more selective toward multivalent ions (PO4(3-) and SO4(2-)) than monovalent ions (F(-) and NO3(-)). In addition, we demonstrated that cationic CNF can be manufactured into permeable membranes capable of dynamic nitrate adsorption by utilizing a simple paper-making process. PMID:26453885

  12. Error assessment in recombinant baculovirus titration: evaluation of different methods.

    PubMed

    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.

  13. An estimated potentiometric surface of the Death Valley region, Nevada and California, developed using geographic information system and automated interpolation techniques

    SciTech Connect

    D`Agnese, F.A.; Faunt, C.C.; Turner, A.K.

    1998-07-01

    An estimated potentiometric surface was constructed for the Death Valley region, Nevada and California, from numerous, disparate data sets. The potentiometric surface was required for conceptualization of the ground-water flow system and for construction of a numerical model to aid in the regional characterization for the Yucca Mountain repository. Because accurate, manual extrapolation of potentiometric levels over large distances is difficult, a geographic-information-system method was developed to incorporate available data and apply hydrogeologic rules during contour construction. Altitudes of lakes, springs, and wetlands, interpreted as areas where the potentiometric surface intercepts the land surface, were combined with water levels from well data. Because interpreted ground-water recharge and discharge areas commonly coincide with groundwater basin boundaries, these areas also were used to constrain a gridding algorithm and to appropriately place local maxima and minima in the potentiometric-surface map. The resulting initial potentiometric surface was examined to define areas where the algorithm incorrectly extrapolated the potentiometric surface above the land surface. A map of low-permeability rocks overlaid on the potentiometric surface also indicated areas that required editing based on hydrogeologic reasoning. An interactive editor was used to adjust generated contours to better represent the natural water table conditions, such as large hydraulic gradients and troughs, or ``vees``. The resulting estimated potentiometric-surface map agreed well with previously constructed maps. Potentiometric-surface characteristics including potentiometric-surface mounds and depressions, surface troughs, and large hydraulic gradients were described.

  14. Accuracy of the endpoint assay for virus titration.

    PubMed

    Nielsen, L K; Smyth, G K; Greenfield, P F

    1992-01-01

    The statistics of estimators used with the endpoint assay for virus titration were investigated. For a standard assay with 10 wells/dilution, the graphical estimator traditionally used was found to produce estimates with significant positive bias and a relatively low accuracy. Furthermore, the graphical estimator was found to be inconsistent. A superior estimator based on the maximum likelihood principle was developed. The results are discussed in relation to the choice between the endpoint titration assay and the plaque assay, and an alternative two-stage assay is presented.

  15. Analyzing a kinetic titration series using affinity biosensors.

    PubMed

    Karlsson, Robert; Katsamba, Phinikoula S; Nordin, Helena; Pol, Ewa; Myszka, David G

    2006-02-01

    The classical method of measuring binding constants with affinity-based biosensors involves testing several analyte concentrations over the same ligand surface and regenerating the surface between binding cycles. Here we describe an alternative approach to collecting kinetic binding data, which we call "kinetic titration." This method involves sequentially injecting an analyte concentration series without any regeneration steps. Through a combination of simulation and experimentation, we show that this method can be as robust as the classical method of analysis. In addition, kinetic titrations can be more efficient than the conventional data collection method and allow us to fully characterize analyte binding to ligand surfaces that are difficult to regenerate.

  16. Map showing the potentiometric surface of the Magothy Aquifer in southern Maryland, September 1982

    USGS Publications Warehouse

    Mack, Frederick K.; Wheeler, Judith C.; Curtin, Stephen E.

    1982-01-01

    A map was prepared that shows the potentiometric surface of the Magothy aquifer in southern Maryland in September 1982. The map is based on measurements from a network of 83 observation wells. The highest levels of the potentiometric surface, 57 and 58 feet above sea level, were measured near the outcrop-subcrop of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties. The potentiometric surface slopes to the southeast to about sea level along much of the western shore of the Chesapeake Bay. Three distinct and extensive cones of depression have developed in the potentiometric surface around the well fields of the Annapolis area, Waldorf area, and Chalk Point. Several square miles of each cone are below sea level, and in some areas at Chalk Point and Waldorf, the cone is more than 50 feet below sea level. The network of wells was developed as part of the cooperative program between the U.S. Geological Survey, the Maryland Geological Survey, and the Maryland Energy Administration. (USGS)

  17. Potentiometric pH Measurements of Acidity Are Approximations, Some More Useful than Others

    ERIC Educational Resources Information Center

    de Levie, Robert

    2010-01-01

    A recent article by McCarty and Vitz "demonstrating that it is not true that pH = -log[H+]" is examined critically. Then, the focus shifts to underlying problems with the IUPAC definition of pH. It is shown how the potentiometric method can provide "estimates" of both the IUPAC-defined hydrogen activity "and" the hydrogen ion concentration, using…

  18. Lead in Hair and in Red Wine by Potentiometric Stripping Analysis: The University Students' Design.

    ERIC Educational Resources Information Center

    Josephsen, Jens

    1985-01-01

    A new program for training upper secondary school chemistry teachers (SE 537 693) depends heavily on student project work. A project in which lead in hair and in red wine was examined by potentiometric stripping analysis is described and evaluated. (JN)

  19. Detection of Catechol by Potentiometric-Flow Injection Analysis in the Presence of Interferents

    ERIC Educational Resources Information Center

    Lunsford, Suzanne K.; Widera, Justyna; Zhang, Hong

    2007-01-01

    This article describes an undergraduate analytical chemistry experiment developed to teach instrumental lab skills while incorporating common interferents encountered in the real-world analysis of catechol. The lab technique incorporates potentiometric-flow injection analysis on a dibenzo-18-crown-6 dual platinum electrode to detect catechol in…

  20. BIOSENSOR FOR DIRECT DETERMINATION OF ORGANOPHOSPHATE NERVE AGENTS. 1. POTENTIOMETRIC ENZYME ELECTRODE. (R823663)

    EPA Science Inventory

    A potentiometric enzyme electrode for the direct measurement of organophosphate (OP)
    nerve agents was developed. The basic element of this enzyme electrode was a pH electrode
    modified with an immobilized organophosphorus hydrolase (OPH) layer formed by cross-linking
    OPH ...

  1. Design and Evaluation of Potentiometric Principles for Bladder Volume Monitoring: A Preliminary Study

    PubMed Central

    Chen, Shih-Ching; Hsieh, Tsung-Hsun; Fan, Wen-Jia; Lai, Chien-Hung; Chen, Chun-Lung; Wei, Wei-Feng; Peng, Chih-Wei

    2015-01-01

    Recent advances in microelectronics and wireless transmission technology have led to the development of various implantable sensors for real-time monitoring of bladder conditions. Although various sensing approaches for monitoring bladder conditions were reported, most such sensors have remained at the laboratory stage due to the existence of vital drawbacks. In the present study, we explored a new concept for monitoring the bladder capacity on the basis of potentiometric principles. A prototype of a potentiometer module was designed and fabricated and integrated with a commercial wireless transmission module and power unit. A series of in vitro pig bladder experiments was conducted to determine the best design parameters for implementing the prototype potentiometric device and to prove its feasibility. We successfully implemented the potentiometric module in a pig bladder model in vitro, and the error of the accuracy of bladder volume detection was <±3%. Although the proposed potentiometric device was built using a commercial wireless module, the design principles and animal experience gathered from this research can serve as a basis for developing new implantable bladder sensors in the future. PMID:26039421

  2. Potentiometric surface of the Upper Floridan aquifer, west-central Florida, September 2010

    USGS Publications Warehouse

    Ortiz, A.G.

    2011-01-01

    This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the approximate annual low and high water-level conditions, respectively. This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2010. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when groundwater levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 53.17 inches for west-central Florida (from October 2009 through September 2010) was 0.41 inches above the historical cumulative average of 52.76 inches (Southwest Florida Water Management District, 2010). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District.

  3. Potentiometric surface in the Central Oklahoma (Garber-Wellington) aquifer, Oklahoma, 2009

    USGS Publications Warehouse

    Mashburn, Shana L.; Magers, Jessica

    2011-01-01

    A study of the hydrogeology of the Central Oklahoma aquifer was started in 2008 to provide the Oklahoma Water Resources Board (OWRB) hydrogeologic data and a groundwater flow model that can be used as a tool to help manage the aquifer. The 1973 Oklahoma water law requires the OWRB to do hydrologic investigations of Oklahoma's aquifers (termed 'groundwater basins') and to determine amounts of water that may be withdrawn by permitted water users. 'Maximum annual yield' is a term used by OWRB to describe the total amount of water that can be withdrawn from a specific aquifer in any year while allowing a minimum 20-year life of the basin (Oklahoma Water Resources Board, 2010). Currently (2010), the maximum annual yield has not been determined for the Central Oklahoma aquifer. Until the maximum annual yield determination is made, water users are issued a temporary permit by the OWRB for 2 acre-feet/acre per year. The objective of the study, in cooperation with the Oklahoma Water Resources Board, was to study the hydrogeology of the Central Oklahoma aquifer to provide information that will enable the OWRB to determine the maximum annual yield of the aquifer based on different proposed management plans. Groundwater flow models are typically used by the OWRB as a tool to help determine the maximum annual yield. This report presents the potentiometric surface of the Central Oklahoma aquifer based on water-level data collected in 2009 as part of the current (2010) hydrologic study. The U.S. Geological Survey (USGS) Hydrologic Investigations Atlas HA-724 by Christenson and others (1992) presents the 1986-87 potentiometric-surface map. This 1986-87 potentiometric-surface map was made as part of the USGS National Water-Quality Assessment pilot project for the Central Oklahoma aquifer that examined the geochemical and hydrogeological processes operating in the aquifer. An attempt was made to obtain water-level measurements for the 2009 potentiometric-surface map from the wells

  4. Cation-induced stabilization of the engineered cation-binding loop in cytochrome c peroxidase (CcP).

    PubMed

    Bhaskar, B; Bonagura, Christopher A; Li, Huiying; Poulos, Thomas L

    2002-02-26

    We have previously shown that the K(+) site found in the proximal heme pocket of ascorbate peroxidase (APX) could be successfully engineered into the closely homologous cytochrome c peroxidase (CcP) [Bonagura et al., (1996) Biochemistry 35, 6107-6115; Bonagura et al. (1999) Biochemistry 38, 5538-5545]. In addition, specificity could be switched to binding Ca(2+) as found in other peroxidases [Bonagura et al. (1999) J. Biol. Chem. 274, 37827-37833]. The introduction of a proximal cation-binding site also promotes conversion of the Trp191 containing cation-binding loop from a "closed" to an "open" conformer. In the present study we have changed a crucial hinge residue of the cation-binding loop, Asn195, to Pro which stabilizes the loop, albeit, only in the presence of bound K(+). The crystal structure of this mutant, N195PK2, has been refined to 1.9 A. As predicted, introduction of this crucial hinge residue stabilizes the cation-binding loop in the presence of the bound K(+). As in earlier work, the characteristic EPR signal of Trp191 cation radical becomes progressively weaker with increasing [K(+)] and the lifetime of the Trp191 radical also has been considerably shortened in this mutant. This mutant CcP exhibits reduced enzyme activity, which could be titrated to lower levels with increasing [K(+)] when horse heart cytochrome c is the substrate. However, with yeast cytochrome c as the substrate, the mutant was as active as wild-type at low ionic strength, but 40-fold lower at high ionic strength. We attribute this difference to a change in the rate-limiting step as a function of ionic strength when yeast cytochrome c is the substrate. PMID:11851415

  5. Complexation Effect on Redox Potential of Iron(III)-Iron(II) Couple: A Simple Potentiometric Experiment

    ERIC Educational Resources Information Center

    Rizvi, Masood Ahmad; Syed, Raashid Maqsood; Khan, Badruddin

    2011-01-01

    A titration curve with multiple inflection points results when a mixture of two or more reducing agents with sufficiently different reduction potentials are titrated. In this experiment iron(II) complexes are combined into a mixture of reducing agents and are oxidized to the corresponding iron(III) complexes. As all of the complexes involve the…

  6. Toxicity of cationic lipids and cationic polymers in gene delivery.

    PubMed

    Lv, Hongtao; Zhang, Shubiao; Wang, Bing; Cui, Shaohui; Yan, Jie

    2006-08-10

    Gene therapy, as a promising therapeutics to treat genetic or acquired diseases, has achieved exciting development in the past two decades. Appropriate gene vectors can be crucial for gene transfer. Cationic lipids and polymers, the most important non-viral vectors, have many advantages over viral ones as non-immunogenic, easy to produce and not oncogenic. They hold the promise to replace viral vectors to be used in clinic. However, the toxicity is still an obstacle to the application of non-viral vectors to gene therapy. For overcoming the problem, many new cationic compounds have been developed. This article provides a review with respect to toxicity of cationic lipids and polymers in gene delivery. We evaluate the structural features of cationic compounds and summarize the relationship of toxicity and structure and hope to provide available suggestions on the development of these cationic compounds.

  7. Potentiometric surface of the Upper Floridan aquifer in the Suwannee River Water Management District, Florida, May 2005

    USGS Publications Warehouse

    Verdi, Richard Jay; Sepulveda, A. Alejandro

    2006-01-01

    Introduction: This map depicts the potentiometric surface of the Upper Floridan aquifer in the Suwannee River Water Management District (SRWMD) during May 2005. Potentiometric contours are based on water-level measurements taken at more than 400 observation wells during the period of May 1-31, 2005. A potentiometric surface is defined as an areal representation of the levels to which water would rise in tightly cased wells open to an aquifer (Fetter, 1988). Since these water-level measurements from the Upper Floridan aquifer were taken over a 31-day period, they do not represent a 'snapshot' of the conditions at a specific date and time.

  8. Potentiometric surface of the lower Cape Fear Aquifer in the central coastal plain of North Carolina, December 1986

    USGS Publications Warehouse

    Winner, M.D.; Lyke, William L.; Brockman, Allen R.

    1989-01-01

    Water level measurements were made in four wells open to the lower Cape Fear aquifer at the end of 1986 to determine the configuration of its potentiometric surface over an area of approximately 4,100 sq mi. Because of the scarcity of data, five earlier measurements were also used to help estimate the position of the potentiometric contours. These were one-time measurements in temporary observation wells. A broad cone of depression has formed in the area between Kinston and New Bern where the potentiometric surface is below sea level and seems likely related to large groundwater withdrawals from the aquifers overlying the lower Cape Fear in that area.

  9. Revised potentiometric-surface map, Yucca Mountain and vicinity, Nevada; Water-resources investigations report 93-4000

    SciTech Connect

    Ervin, E.M.; Luckey, R.R.; Burkhardt, D.J.

    1994-05-01

    This report presents a revised potentiometric-surface map based mainly on the 1988 average water levels at Yucca Mountain and the nearby vicinity extending from Crater Flat to Jackass Flats. Discussion includes an explanation of the revised potentiometric-surface map, an examination of yearly trends in the water levels, and adjustments for temperature and density effects in the deeper wells. Report scope focuses on the potentiometric surface of the uppermost saturated zone in the Tertiary volcanic rocks at Yucca Mountain. Some information, related to the underlying Paleozoic carbonate aquifer, pertinent to the volcanic flow system, is presented.

  10. Characterisation of iron binding ligands in seawater by reverse titration.

    PubMed

    Hawkes, Jeffrey A; Gledhill, Martha; Connelly, Douglas P; Achterberg, Eric P

    2013-03-01

    Here we demonstrate the use of reverse titration - competitive ligand exchange-adsorptive cathodic stripping voltammetry (RT-CLE-ACSV) for the analysis of iron (Fe) binding ligands in seawater. In contrast to the forward titration, which examines excess ligands in solution, RT-CLE-ACSV examines the existing Fe-ligand complexes by increasing the concentration of added (electroactive) ligand (1-nitroso-2-naphthol) and analysis of the proportion of Fe bound to the added ligand. The data manipulation allows the accurate characterisation of ligands at equal or lower concentrations than Fe in seawater, and disregards electrochemically inert dissolved Fe such as some colloidal phases. The method is thus superior to the forward titration in environments with high Fe and low ligand concentrations or high concentrations of inert Fe. We validated the technique using the siderophore ligand ferrioxamine B, and observed a stability constant [Formula: see text] of 0.74-4.37×10(21) mol(-1), in agreement with previous results. We also successfully analysed samples from coastal waters and a deep ocean hydrothermal plume. Samples from these environments could not be analysed with confidence using the forward titration, highlighting the effectiveness of the RT-CLE-ACSV technique in waters with high concentrations of inert Fe.

  11. Coulometric titration of ruthenium and iridium by the generated hydroquinone

    SciTech Connect

    Organeysan, L.S.; Butakova, N.A.

    1986-05-10

    This paper studies the electrogeneration of hydroquinone from solutions of quinone on platinum and glass-carbon electrodes in HC1 and H/sub 2/SO/sub 4/ media of different concentrations, to select the optimal conditions for the coulometric titration of Ru(IV) and Ir(IV).

  12. A General Simulator for Acid-Base Titrations

    NASA Astrophysics Data System (ADS)

    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.

  13. Analysis of the purity of cetrimide by titrations.

    PubMed

    Rasmussen, Claus D; Nielsen, Hans B; Andersen, Jens E T

    2006-01-01

    The purity of cetrimide, trimethyl tetradecyl ammonium bromide (TTAB), which is an important preservative of many cosmetic and pharmaceutical products, was determined by three independent methods of titration. Traditionally, cetrimide was analysed by an assay method of the European Pharmacopoeia, which showed consistently a low purity of cetrimide with associated large standard deviations, however. A systematic 3% bias of the European Pharmacopoeia assay method was identified by comparing the result with results of two alternative methods of titration that exhibited high precision and high accuracy. Titration by perchloric acid showed a 99.69% +/- 0.05% purity of cetrimide, and titration by silver nitrate showed a 99.85% +/- 0.05% purity, while the traditional assay method predicted a purity of only 97.1% +/- 0.4%. It was found that the discrepancy could be identified as differences in selectivity during the extraction step of the European Pharmacopoeia assay method. The distribution coefficients between chloroform and water of cetrimide and the corresponding iodide species (TTAI) were thus determined as 2150 +/- 50 M(-1) and 68000 +/- 4000 M(-1), respectively.

  14. Determination of Acidity Constants by Gradient Flow-Injection Titration

    ERIC Educational Resources Information Center

    Conceicao, Antonio C. L.; Minas da Piedade, Manuel E.

    2006-01-01

    A three-hour laboratory experiment, designed for an advanced undergraduate course in instrumental analysis that illustrates the application of the gradient chamber flow-injection titration (GCFIT) method with spectrophotometric detection to determine acidity constants is presented. The procedure involves the use of an acid-base indicator to obtain…

  15. Isothermal Titration Calorimetry Can Provide Critical Thinking Opportunities

    ERIC Educational Resources Information Center

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

    2016-01-01

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

  16. Chemical force titrations of functionalized Si(111) surfaces.

    PubMed

    Mengistu, Tadesse Z; Goel, Vishya; Horton, J Hugh; Morin, Sylvie

    2006-06-01

    Chemical force titrations-plots of the adhesive force between an atomic force microscope tip and sample as a function of pH-were acquired on alkyl monolayer-derivatized Si(111) surfaces. Gold-coated AFM tips modified with thioalkanoic acid self-assembled monolayers (SAM) were employed. Alkyl monolayer-derivatized Si(111) surfaces terminated with methyl, carboxyl, and amine groups were produced via hydrosilylation reactions between 1-alkene reagents and H-terminated silicon. The functionalized surfaces were characterized using standard surface science techniques (AFM, FTIR, and XPS). Titration of the methyl-terminated surface using the modified (carboxyl-terminated) atomic force microscope tip resulted in a small pH-independent hydrophobic interaction. Titration of the amine-terminated surface using the same tip resulted in the determination of a surface pKa of 5.8 for the amine from the pH value from the maximum in the force titration curve. A pK(1/2) of 4.3 was determined for the carboxyl-terminated Si(111) in a similar way. These results will be discussed in relation to the modified Si(111) surface chemistry and organic layer structure, as well as with respect to existing results on Au surfaces modified with SAMs bearing the same functional groups.

  17. Asphalt compatibility testing using the automated Heithaus titration test

    SciTech Connect

    Pauli, A.T.

    1996-12-31

    The Heithaus titration test or variations of the test have been used for over 35 years to predict compatibilities of blends of asphalts from different crude sources. Asphalt compatibility is determined from three calculated parameters that measure the state of peptization of an asphalt or asphalt blend. The parameter p{sub a} is a measure of the peptizability of the asphaltenes. The parameter p{sub a} is a measure of the peptizing power of the maltenes, and the parameter P, derived from p{sub a} and p{sub o} values, is a measure of the overall state of peptization of the asphalt or asphalt blend. In Heithaus original procedure, samples of asphalt were dissolved in toluene and titrated with n-heptane in order to initiate flocculation. The onset of flocculation was detected either by photography or by spotting a filter paper with a small amount of the titrated solution. Recently, an {open_quotes}automated{close_quotes} procedure, after Hotier and Robin, has been developed for use with asphalt. In the automated method UV-visible spectrophotometric detection measures the onset of flocculation as a peak with the percent transmittance plotted as a function of the volume of titrating solvent added to a solution of asphalt. The automated procedure has proven to be less operator dependent and much faster than the original Heithaus procedure. Results from the automated procedure show the data to be consistent with results from the original, {open_quotes}classical{close_quotes} Heithaus procedure.

  18. Using Spreadsheets to Produce Acid-Base Titration Curves.

    ERIC Educational Resources Information Center

    Cawley, Martin James; Parkinson, John

    1995-01-01

    Describes two spreadsheets for producing acid-base titration curves, one uses relatively simple cell formulae that can be written into the spreadsheet by inexperienced students and the second uses more complex formulae that are best written by the teacher. (JRH)

  19. A Low-Cost Device for Automatic Photometric Titrations

    NASA Astrophysics Data System (ADS)

    Rocha, Fábio R. P.; Reis, Boaventura F.

    2000-02-01

    Electronics is an important topic in chemistry courses. However, the introduction of basic concepts is often difficult and the lab instruments are frequently seen as "black boxes". To address this problem, we propose the construction of a simple, low-cost (about $150 U.S.) automatic photometric titrator employing a light-emitting diode (LED) and a phototransistor. The electronic circuit can be assembled by the students themselves. The device was employed to implement a common procedure in chemical labs, making feasible the introduction of concepts related to electronics in undergraduate chemistry courses. The titrator is able to work automatically, since a feedback system permits stopping the addition of titrant solution when the end-point is achieved. With this demonstration, it can be stressed that automatic procedures can be implemented without expensive instruments. Additionally, a classical procedure becomes more attractive to the students and its importance to chemical analysis can be emphasized. The feasibility of the titrator was demonstrated by acid-base titrations of HCl solutions with NaOH in the presence of phenolphthalein and by iodimetric determination of ascorbic acid in vitamin C tablets and lemon juice. Precise results (0.7% relative standard deviation, n = 10) in agreement at the 95% confidence level with those attained by a conventional procedure were obtained.

  20. Surface cationized cellulose nanofibrils for the production of contact active antimicrobial surfaces.

    PubMed

    Saini, Seema; Yücel Falco, Çiğdem; Belgacem, Mohamed Naceur; Bras, Julien

    2016-01-01

    In the last decade, a new fiber pretreatment has been proposed to make easy cellulose fibrillation into microfibrils. In this context, different surface cationized MFC was prepared by optimizing the experimental parameters for cellulose fibers pretreatment before fibrillation. All MFCs were characterized by conductometric titration to establish degree of substitution, field emission gun scanning electron microscopy (FEG-SEM), atomic force microscopy (AFM) and optical microscopy assessed the effect of pretreatment on the morphology of the ensuing MFCs. Antibacterial activities of neat and cationized MFC samples were investigated against Gram positive bacteria (Bacillus subtilis, Staphylococcus aureus) and Gram negative bacteria (Escherichia coli). The CATMFC sample at DS greater than 0.18 displayed promising results with antibacterial properties without any leaching of quaternary ammonium into the environment. This work proved the potential of cationic MFCs with specific DS for contact active antimicrobial surface applications in active food packaging, medical packaging or in health and cosmetic field. PMID:26453874

  1. Cation-Induced Hydration Effects Cause Lower Critical Solution Temperature Behavior in Protein Solutions.

    PubMed

    Matsarskaia, Olga; Braun, Michal K; Roosen-Runge, Felix; Wolf, Marcell; Zhang, Fajun; Roth, Roland; Schreiber, Frank

    2016-08-11

    The phase behavior of protein solutions is important for numerous phenomena in biology and soft matter. We report a lower critical solution temperature (LCST) phase behavior of aqueous solutions of a globular protein induced by multivalent metal ions around physiological temperatures. The LCST behavior manifests itself via a liquid-liquid phase separation of the protein-salt solution upon heating. Isothermal titration calorimetry and zeta-potential measurements indicate that here cation-protein binding is an endothermic, entropy-driven process. We offer a mechanistic explanation of the LCST. First, cations bind to protein surface groups driven by entropy changes of hydration water. Second, the bound cations bridge to other protein molecules, inducing an entropy-driven attraction causing the LCST. Our findings have general implications for condensation, LCST, and hydration behavior of (bio)polymer solutions as well as the understanding of biological effects of (heavy) metal ions and their hydration. PMID:27414502

  2. [Effect of calcium cations on acid-base properties and free radical oxidation of dopamine and pyrocatechol].

    PubMed

    Lebedev, A V; Ivanova, M V; Timoshin, A A; Ruuge, E K

    2008-01-01

    Ca2+-induced increase in the rate of pyrocatechol and dopamine oxidation by dioxygen and Ca2+-dependent acid-base properties of the catechols were studied by potentiometric titration, UV/Vis-spectrophotometry, EPR-spectroscopy, and by measurement of oxygen consumption. The effect of Ca2+ on the chain reactions of oxidation can be explained by additional deprotonation (decrease in pKai) of the catechols that accelerates one electron transport to dioxygen and formation of calcium semiquinonate, undergoing further oxidation. The described Ca2+-dependent redox-conversion of ortho-phenols proposes that an additional function of calcium in the cell can be its involvement in free radical oxidoreductive reactions at pH > pKai.

  3. Redox titrations of carbon monoxide dehydrogenase from Clostridium thermoaceticum.

    PubMed

    Shin, W; Stafford, P R; Lindahl, P A

    1992-07-01

    Redox titrations of carbon monoxide dehydrogenase (CODH) from Clostridium thermoaceticum were performed using the reductant CO and the oxidant thionin. Titrations were followed at 420 nm, a wavelength sensitive to redox changes of the iron-sulfur clusters in the enzyme. When CODH was oxidized by just enough thionin to maximize A420, two molecules of CO per mole of CODH dimer (4 equiv/mol) reduced the enzyme fully. Likewise, 4 equiv/mol of thionin oxidized the fully-reduced enzyme to the point where A420 maximized. The four n = 1 redox sites which titrated in this region were designated group I sites. They include at least two iron-sulfur clusters, [Fe/S]A and [Fe/S]B, and two other sites, A' and B'. The [Fe4S4]2+/1+ cluster in CODH is included in this group. [Fe/S]B and B' have reduction potentials (at pH 8) below -480 mV vs NHE; [Fe/S]A and A' have reduction potentials above that value. The reduction potential of either [Fe/S]B or B' is near to the CO/CO2 couple at pH 8 (-622 mV). When CODH was oxidized by more than enough thionin to maximize A420, some of the excess thionin oxidized the so-called group II redox sites. These sites have reduction potentials more positive than group I and do not exhibit changes at 420 nm when titrated. Titration of group II sites required 1-2 equiv/mol. EPR of reduced group II sites exhibited the gav = 1.82 signal. When these sites were oxidized, the only signal present had g values at 2.075, 2.036, and 1.983.(ABSTRACT TRUNCATED AT 250 WORDS)

  4. [Titration of Ebola and Marburg viruses by plaque formation under semi liquid agar].

    PubMed

    Ustinova, E N; Shestopalov, A M; Bakulina, L F; Chepurnov, A A

    2003-01-01

    The method of titration of Ebola and Marburg viruses using plaque formation under semifluid agar cover is considered. Advantages of this method over conventional method of titration of these viruses with the use of hard agar cover are discussed.

  5. Colloid Titration--A Rapid Method for the Determination of Charged Colloid.

    ERIC Educational Resources Information Center

    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)

  6. Nile blue and brilliant cresyl blue as redox indicators in iron(II) titrations.

    PubMed

    Sriramam, K

    1975-01-01

    Nile Blue and Brilliant Cresyl Blue, two compounds related to diaminophenoxazine, have been studied as indicators in titrations of iron(II) with cerium(IV)(in hydrochloric, sulphuric and perchloric acid media), dichromate, vanadate and permanganate. They are particularly suited for titrations in a fairly concentrated sulphuric acid medium and for titrations with dilute solutions. A probable indicator mechanism is suggested.

  7. The Acid-Base Titration of a Very Weak Acid: Boric Acid

    ERIC Educational Resources Information Center

    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…

  8. Scopolamine Effects Under a Titrating-Delayed-Nonmatching-to-Position Procedure

    ERIC Educational Resources Information Center

    Porritt, M.; Poling, A.

    2008-01-01

    In a study of working memory, the performance of rats under titrating-delayed-nonmatching- to-position (TDNMTP) procedures was examined. Overall accuracy and the number of trials completed were inversely related to titration value, whereas the highest delay attained was directly related to titration value. When given intraperitoneally,…

  9. The Cation-π Interaction

    PubMed Central

    DOUGHERTY, DENNIS A.

    2014-01-01

    CONSPECTUS The chemistry community now recognizes the cation-π interaction as a major force for molecular recognition, joining the hydrophobic effect, the hydrogen bond, and the ion pair in determining macromolecular structure and drug-receptor interactions. This Account provides the author’s perspective on the intellectual origins and fundamental nature of the cation-π interaction. Early studies on cyclophanes established that water-soluble, cationic molecules would forgo aqueous solvation to enter a hydrophobic cavity if that cavity was lined with π systems. Important gas phase studies established the fundamental nature of the cation-π interaction. The strength of the cation-π interaction – Li+ binds to benzene with 38 kcal/mol of binding energy; NH4+ with 19 kcal/mol– distinguishes it from the weaker polar-π interactions observed in the benzene dimer or water-benzene complexes. In addition to the substantial intrinsic strength of the cation-π interaction in gas phase studies, the cation-π interaction remains energetically significant in aqueous media and under biological conditions. Many studies have shown that cation-π interactions can enhance binding energies by 2 – 5 kcal/mol, making them competitive with hydrogen bonds and ion pairs in drug-receptor and protein-protein interactions. As with other noncovalent interactions involving aromatic systems, the cation-π interaction includes a substantial electrostatic component. The six (four) Cδ−–Hδ+ bond dipoles of a molecule like benzene (ethylene) combine to produce a region of negative electrostatic potential on the face of the π system. Simple electrostatics facilitate a natural attraction of cations to the surface. The trend for (gas phase) binding energies is Li+>Na+>K+>Rb+: as the ion gets larger the charge is dispersed over a larger sphere and binding interactions weaken, a classical electrostatic effect. On other hand, polarizability does not define these interactions. Cyclohexane

  10. Nano- and microsized zeolites as a perspective material for potentiometric biosensors creation.

    PubMed

    Soldatkin, Oleksandr O; Shelyakina, Margaryta K; Arkhypova, Valentyna N; Soy, Esin; Kirdeciler, Salih Kaan; Ozansoy Kasap, Berna; Lagarde, Florence; Jaffrezic-Renault, Nicole; Akata Kurç, Burcu; Soldatkin, Alexei P; Dzyadevych, Sergei V

    2015-01-01

    A number of potentiometric biosensors based on coimmobilization of enzymes with different types of zeolite on pH-ion-sensitive field-effect transistor (ISFET) have been developed. Their working characteristics have been determined and compared. It was shown that clinoptilolite and zeolite Beta polymorph A (BEA) are more promising for creating biosensors than zeolite A. Changing the concentration of zeolite BEA in membranes, it is possible to extend the biosensor linear measurement range. The two-layer method of deposition of the enzyme with clinoptilolite was found to provide a significant increase in the biosensor sensitivity to substrates, whereas thermal modification of the zeolite BEA crystals can improve analytical characteristics of potentiometric biosensors for detection of toxic substances. These results show that it is possible to regulate the ISFET characteristics for different enzyme-based biosensors by tailoring the electrode surfaces via different zeolites. This makes zeolites strong candidates for integration into biosensors as ISFET modifiers.

  11. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 69 wells. The highest measured water level was 85 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south. Local gradients were directed toward the center of a cone of depression in the Waldorf area that developed in response to pumping. Measured ground-water levels were as low as 90 feet below sea level in the Waldorf area.

  12. Potentiometric Surface of the Aquia Aquifer in southern Maryland, September 1995

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Mack, Frederick K.

    1997-01-01

    A map showing the potentiometric surface of the Aquia aquifer in the Aquia Formation of Paleocene age in southern Maryland during September 1995 was prepared from water-level measurements in 80 wells. The potentiometric surface was above sea level near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties, and was below sea level in the remainder of the study area. The hydraulic gradient was directed southeastward toward an extensive cone of depression around well fields at Lexington Park and Solomons Island. Ground-water levels were more than 70 feet below sea level in a 60-square-mile area surrounding the deepest part of the cone of depression and 126 feet below sea level in one well near the center of the cone.

  13. Potentiometric Surface of the Aquia Aquifer in Southern Maryland, September 2001

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2002-01-01

    This report presents a map showing the potentiometric surface of the Aquia aquifer in the Aquia Formation of Paleocene age in Southern Maryland during September 2001. The map is based on water-level measurements in 76 wells. The potentiometric surface was highest at 40 feet above sea level near the northern boundary and outcrop area of the aquifer in the central part of Anne Arundel County, and was below sea level in the remainder of the study area. The hydraulic gradient was directed southeastward toward an extensive cone of depression around well fields at Lexington Park and Solomons Island. A cone of depression formed in northern Calvert County due to pumpage at Chesapeake Beach and North Beach. The water level has declined to 44 feet below sea level in this area. The lowest measurement was 160 feet below sea level at the center of a cone of depression at Lexington Park.

  14. Potentiometric surface of the Aquia Aquifer in southern Maryland, September 1994

    USGS Publications Warehouse

    Curtin, Stephen E.; Mack, Frederick K.; Andreasen, David C.

    1995-01-01

    A map showing the potentiometric surface of the Aquia aquifer in the Aquia aquifer in the Aquia Formation of Paleocene age in southern Maryland during September 1994 was prepared from water levels measured in 74 wells. The potentiometric surface was above sea level near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties, and was below sea level in the remainder of the study area. The hydraulic gradient was directed southeastward toward an extensive cone of depression around well fields at Lexington Park and Solomons Island. Ground-water levels were more than 70 feet below sea level in a 60-square-mile area surrounding the deepest part of the cone of depression and 131 feet below sea level in one well near the center of the cone.

  15. Potentiometric surfaces of the Mississippi River Valley alluvial aquifer in eastern Arkansas, spring 1972 and 1980

    USGS Publications Warehouse

    Ackerman, D.J.

    1989-01-01

    Maps that show contours of the altitude of water levels for wells completed in the Mississippi River Valley alluvial aquifer in eastern Arkansas were prepared using water-level measurements made in the spring of 1972-1980. Hydrographs for selected wells are included to show trends and lack of trends in water-level changes. The aquifer consists of gravel and sand in flood-plain and terrace deposits of Quaternary age. The aquifer supplies much of the water used for irrigation and aquaculture in eastern Arkansas. A large depression in the potentiometric surface caused by pumping for irrigation and aquaculture occurs in Arkansas, Lonoke, and Prairie Counties. A smaller depression in the potentiometric surface occurs north of Brinkley. Significant water-level declines occurred during the period 1972-80 in several counties west of Crowleys Ridge. (USGS)

  16. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2009

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2010-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Late Cretaceous age in Southern Maryland during September 2009. The map is based on water-level measurements in 66 wells. The highest measured water level was 85 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south. Local hydraulic gradients were directed toward the center of a cone of depression in the Waldorf area that developed in response to pumping. Measured groundwater levels were as low as 71 feet below sea level in the Waldorf area. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  17. Potentiometric Surface of the Upper Patapsco Aquifer in Southern Maryland, September 2002

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2003-01-01

    This report presents a map showing the potentiometric surface of the Upper Patapsco aquifer in the Patapsco Formation of Lower Cretaceous age in Southern Maryland during September 2002. The map is based on water-level measurements in 50 wells. The highest measured water level was 117 feet above sea level near the northern boundary and outcrop area of the aquifer in northern Anne Arundel County. From this area, the potentiometric surface declined to the southeast toward large well fields in Arnold and Annapolis, and from all directions toward a cone of depression located southwest of Waldorf. The measured ground-water level declined to 36 feet below sea level in Arnold, and to 23 feet below sea level in Annapolis. The lowest water level measured was 136 feet below sea level southwest of Waldorf.

  18. Potentiometric surface of the Aquia Aquifer in southern Maryland, September 1991

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, D.C.; Mack, Frederick K.

    1993-01-01

    A map showing the potentiometric surface of the Aquia aquifer in the Aquia Formation of Paleocene age in southern Maryland during September 1991 was prepared from water levels measured in 82 wells. The potentiometric surface was above sea level near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel and Prince Georges Counties, and was below sea level in the remainder of the study area. The hydraulic gradient was directed southeastward toward an extensive cone of depression around well fields at Lexington Park and Solomons Island. Groundwater levels were more than 60 feet below sea level in a 60-sq-mi area surrounding the deepest part of the cone of depression and 117 feet below sea level in one well near the center of the cone.

  19. Map showing the potentiometric surface of the Magothy Aquifer in southern Maryland, August 1980

    USGS Publications Warehouse

    Mack, Frederick K.; Wheeler, Judith C.; Curtin, Stephen E.

    1981-01-01

    This map is based on measurements made in a network of 77 observation wells. Highest levels of the potentiometric surface, 61 to 64 feet above sea level, were near the outcrop or subcrop of the aquifer in topographically high areas of Anne Arundel and northern Prince Georges Counties. The potentiometric surface slopes toward centers of pumpage near Annapolis, in northern Charles County, and southern Prince Georges County. Two separate , distinct, and extensive cones of depression have developed in the surface around the well fields of Waldorf, in northern Charles County, and the Chalk Point power plant, in southern Prince Georges County. The cone of depression in the Annapolis area has coalesced with a more shallow cone that includes the Broadneck Peninsula. The network of wells was developed and is operated and maintained as part of the cooperative program between the U.S. Geological Survey and agencies of the Maryland Department of Natural Resources. (USGS)

  20. Potentiometric Surface of the Magothy Aquifer in Southern Maryland, September 2002

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2003-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Upper Cretaceous age in Southern Maryland during September 2002. The map is based on water-level measurements in 79 wells. The highest measured water level was 83 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south and east. Local gradients were directed toward the centers of two cones of depression that developed in response to pumping. These cones of depression were centered around well fields in the Waldorf area and at the Chalk Point power plant. Measured ground-water levels were as low as 81 feet below sea level in the Waldorf area and 75 feet below sea level at Chalk Point.

  1. Potentiometric Surface of the Patuxent Aquifer in Southern Maryland, September 2009

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2010-01-01

    This report presents a map showing the potentiometric surface of the Patuxent aquifer in the Patuxent Formation of Early Cretaceous age in Southern Maryland during September 2009. The map is based on water-level measurements in 42 wells. The highest measured water level was 169 feet above sea level in the outcrop area of the aquifer in northern Prince George's County. From this area, the potentiometric surface declined south towards well fields at Glen Burnie, Bryans Road, the Morgantown power plant, and the Chalk Point power plant. The measured groundwater levels were 78 feet below sea level at Glen Burnie, 56 feet below sea level at Bryans Road, 29 feet below sea level at the Morgantown power plant, and 28 feet below sea level at the Chalk Point power plant. The map also shows well yield in gallons per day for 2008 at wells or well fields.

  2. Potentiometric Surface of the Patuxent Aquifer in Southern Maryland, September 2007

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Staley, Andrew W.

    2009-01-01

    This report presents a map showing the potentiometric surface of the Patuxent aquifer in the Patuxent Formation of Early Cretaceous age in Southern Maryland during September 2007. The map is based on water-level measurements in 41 wells. The highest measured water level was 165 feet above sea level near the northwestern boundary and in the outcrop area of the aquifer in northern Prince George's County. From this area, the potentiometric surface declined south towards well fields at Glen Burnie, Bryans Road, the Morgantown power plant, and the Chalk Point power plant. The measured ground-water levels were 81 feet below sea level at Glen Burnie, 47 feet below sea level southwest of Bryans Road, 27 feet below sea level at the Morgantown power plant, and 24 feet below sea level at the Chalk Point power plant.

  3. Potentiometric Surface of the Upper Patapsco Aquifer in Southern Maryland, September 1995

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Mack, Frederick K.

    1996-01-01

    A map showing the potentiometric surface of the upper Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1995 was prepared from water-level measurements in 42 wells. The potentiometric surface was nearly 120 feet above sea level near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel County, and 55 feet above sea level in a similar setting in Prince Georges County. From these high areas, the potentiometic surface declined to the south and southeast toward large well fields in the Annapolis and Waldorf areas and at the Chalk Point powerplant. Ground-water levels reached nearly 30 feet below sea level in the Annapolis area, 113 feet below sea level southwest of Waldorf, and more than 30 feet below sea level at the Chalk Point powerplant.

  4. Potentiometric surface map of the Magothy aquifer in southern Maryland, September, 2003

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2005-01-01

    This report presents a map showing the potentiometric surface of the Magothy aquifer in the Magothy Formation of Upper Cretaceous age in Southern Maryland during September 2002. The map is based on water-level measurements in 79 wells. The highest measured water level was 83 feet above sea level near the northern boundary and outcrop area of the aquifer in the north-central part of Anne Arundel County. The potentiometric surface declined towards the south and east. Local gradients were directed toward the centers of two cones of depression that developed in response to pumping. These cones of depression were centered around well fields in the Waldorf area and at the Chalk Point power plant. Measured ground-water levels were as low as 81 feet below sea level in the Waldorf area and 75 feet below sea level at Chalk Point.

  5. Potentiometric Determination of CO2 Concentration in the Gaseous Phase: Applications in Different Laboratory Activities

    NASA Astrophysics Data System (ADS)

    Cortón, Eduardo; Kocmur, Santiago; Haim, Liliana; Galagovsky, Lydia

    2000-09-01

    Four simple experiments are described, in two laboratory sessions of 3 hours each. They provide high school students of a combined science course with the opportunity to review and integrate many topics while participating in a hands-on activity that resembles real industrial problems. The first lab comprises the calibration of a CO2 potentiometric detector with gas mixtures. The CO2 and CO2-free air required for the gaseous samples are produced in the lab by an inexpensive and simple apparatus. In the second lab, the CO2 potentiometric device is used to measure CO2uptake and release during different metabolic processes. The variation of CO2 production will be also estimated while changing the air/fuel proportion in a Bunsen burner.

  6. Potentiometric map of the Meridian-Upper Wilcox Aquifer in Mississippi, fall 1983

    USGS Publications Warehouse

    Darden, Daphne

    1986-01-01

    The Meridian-upper Wilcox aquifer consists of the Meridian Sand member of the Tallahatta Formation and the uppermost sand beds of the Wilcox Group. Thickness of the aquifer ranges from 50 ft to 500 ft. Precipitation recharges the Meridian-upper Wilcox in the outcrop area, which extends from Benton County, MS, in the north to Clarke County, MS, in the south. The potentiometric map is based on water level measurements made in about 170 wells in the Meridian-upper Wilcox aquifer in October 1983, and on the approximate altitudes of water surfaces in some major streams. The contours show altitudes at which water levels would have stood in tightly cased unpumped wells. This map, the second in the series for the Meridian-upper Wilcox aquifer, updates a map that delineated the potentiometric surface of the aquifer in 1979. (Lantz-PTT)

  7. Potentiometric surface of the Floridan Aquifer, Southwest Florida Water Management District, May 1981

    USGS Publications Warehouse

    Yobbi, D.K.; Woodham, W.M.; Schiner, George R.

    1981-01-01

    A May 1981 potentiometric-surface map of the Southwest Florida Water Management District depicts the annual low water-level period. Potentiometric levels decreased 10 to 45 feet between September 1980 and May 1981 in the citrus and farming sections of southern Hillsborough, northern Hardee, southwestern Polk, northwestern DeSoto, and Manatee Counties. Water levels in these areas are widely affected by pumping for irrigation and have the greatest range in fluctuations. Water-level decreases ranged from 0 to 1 feet in coastal, northern, and southern areas of the Water Management District. Water levels in all of the approximate 700 wells measured in May 1981 are lower than May 1980 because of the virtual absence of rainfall in April and May. (USGS)

  8. Computer-assisted Gran titration procedure for strong acid determination

    SciTech Connect

    Phillips, M.F.; Gaffney, J.S.; Goodrich, R.W.; Tanner, R.L.

    1984-10-01

    An automated method for determining, by coulometric titration, small amounts of strong acid in the presence of weak acids is given. Essentially, a pH meter and a coulometer are coupled with a Tektronix 4052 mini-computer, and a two-step computer program then directs the titration and calculates the equivalence point by the method of Gran. A comparison of precision and accuracy of results for test solutions by manual and automated data reduction methods is presented. The method is being used successfully to analyze for the H/sup +/ content in ambient aerosol samples from aerometric field experiments, and can be used for cloud and rainwater samples as well. 3 references, 1 figure, 1 table.

  9. Titration of vaccinia virus by intravenous injection of chick embryos.

    PubMed

    KAPLAN, C

    1960-01-01

    The final test of a smallpox vaccine is its capacity to prevent the disease from developing in inoculated individuals. This capacity, however, cannot be measured directly, so that other methods of assessing the efficacy of vaccine have had to be developed. A laboratory method-pock counting on the chorio-allantoic membrane of chick embryos-has recently been shown to provide a reasonably reliable estimate of the number of infective units in a given vaccine. In this paper, the author compares this pock-counting method with another method-titration by intravenous injection of chick embryos. He concludes that, although the reproducibility of titrations by intravenous injection compares very favourably with that obtained by chorio-allantoic inoculation, the former method would not be advantageous for the assay of vaccines, since it is very time-consuming and since differences in virulence might obscure comparisons between the efficacy of vaccines.

  10. High-throughput titration of luciferase-expressing recombinant viruses.

    PubMed

    Garcia, Vanessa; Krishnan, Ramya; Davis, Colin; Batenchuk, Cory; Le Boeuf, Fabrice; Abdelbary, Hesham; Diallo, Jean-Simon

    2014-01-01

    Standard plaque assays to determine infectious viral titers can be time consuming, are not amenable to a high volume of samples, and cannot be done with viruses that do not form plaques. As an alternative to plaque assays, we have developed a high-throughput titration method that allows for the simultaneous titration of a high volume of samples in a single day. This approach involves infection of the samples with a Firefly luciferase tagged virus, transfer of the infected samples onto an appropriate permissive cell line, subsequent addition of luciferin, reading of plates in order to obtain luminescence readings, and finally the conversion from luminescence to viral titers. The assessment of cytotoxicity using a metabolic viability dye can be easily incorporated in the workflow in parallel and provide valuable information in the context of a drug screen. This technique provides a reliable, high-throughput method to determine viral titers as an alternative to a standard plaque assay.

  11. Applications of isothermal titration calorimetry in protein science.

    PubMed

    Liang, Yi

    2008-07-01

    During the past decade, isothermal titration calorimetry (ITC) has developed from a specialist method for understanding molecular interactions and other biological processes within cells to a more robust, widely used method. Nowadays, ITC is used to investigate all types of protein interactions, including protein-protein interactions, protein-DNA/RNA interactions, protein-small molecule interactions and enzyme kinetics; it provides a direct route to the complete thermodynamic characterization of protein interactions. This review concentrates on the new applications of ITC in protein folding and misfolding, its traditional application in protein interactions, and an overview of what can be achieved in the field of protein science using this method and what developments are likely to occur in the near future. Also, this review discusses some new developments of ITC method in protein science, such as the reverse titration of ITC and the displacement method of ITC.

  12. [The use of tapioca as coverage in viral titration].

    PubMed

    Post, P R; de Carvalho, R; Brito, E C; Galler, R

    1992-01-01

    Virus titration is an important step required on viral vaccines quality control. "Plaque assay", which employs several types of overlay media, is usually used on viral titrations. In this paper we describe the use of Tapioca as an overlay media. Firstly, the toxicity of Tapioca was tested on Vero cells inoculated or not with the Yellow Fever virus (YF) 17DD vaccine strain. Secondly, different batches of the 17DD virus using the Tapioca and Karaya gum as the overlay on Vero cells were tested when higher titres were obtained using Tapioca. Tapioca was also shown to be a suitable overlay to be used in thermostability and plaque reduction neutralization tests. Other systems could benefit from the use of Tapioca as an overlay, since it was possible to titer Measles virus in Vero cells. Tapioca is a cheap Brazilian product, is locally available, easy to use, and reliable. Its use is suggested.

  13. SBR on-line monitoring by set-point titration.

    PubMed

    Fiocchi, N; Ficara, E; Canziani, R; Luccarini, L; Ciappelloni, F; Ratini, P; Pirani, M; Mariani, S

    2006-01-01

    The applicability of set-point titration for monitoring biological processes has been widely demonstrated in the literature. Based on published and on-going experiences, some operating procedures have been specifically developed to be applied to SBRs, so that real-time information about the process and/or the influent can be obtained. This, in turn, would allow plant operators to select the most appropriate actions properly and timely. Five operating modes are described for the monitoring of (1) influent toxicity, (2) influent N-content, (3) nitrification capacity, (4) end of the nitrification reaction, and (5) nitrate effluent concentration, and are currently tested on the on-line titrator TITAAN (TITrimetric Automated ANalyser) which is in operation on a pilot scale SBR. PMID:16722107

  14. Rational Catalyst Design of Titanium-Silica Materials Aided by Site-Specific Titration Tools

    NASA Astrophysics Data System (ADS)

    Eaton, Todd Robert

    Silica-supported titanium materials are widely used for thermocatalytic applications such as hydroxylation of alkanes and aromatics, oxidation of alcohols and ethers, ammoximation of carbonyls, and sulfoxidations, while Ti-based materials are widely studied for photocatalytic applications such as photo-oxidation of organic substrates and photo-reduction of CO 2. However, the underlying phenomena of how to synthesize, identify, and control the active structures in these materials is not well understood because of the narrow scope of previous work. Studies of titanium-based catalysts typically focus on materials where the metal is present as either highly-dispersed Ti cations or in bulk crystalline TiO2 form, neglecting the numerous and potentially useful intermediate structures. Furthermore, these works typically focus on a single synthesis technique and rely upon bulk characterization techniques to understand the materials. Here rigorous titanium-silica synthesis-structure-function relationships are established by examining several different synthetic method and utilizing characterization techniques that enable an atomic-level understanding of the materials. The materials studied span the range from isolated Ti cations to clustered TiOx domains, polymeric TiO x domains, anatase-like 2D TiO2 domains, and 3D crystalline TiO2. Tools to quantify accessible TiO x and tetrahedral Ti sites are developed, utilizing the selective titration of titanium with phenylphosphonic acid (PPA). Catalytic properties are probed with the photocatalytic oxidation of benzyl alcohol and the thermocatalytic epoxidation of cis-cyclooctene with H2O2 . PPA titration data indicate that the rate of benzyl alcohol photo-oxidation is independent of titanium coordination, while the rate of alkene epoxidation with H2O2 is proportional to the number of tetrahedral titanium sites on the catalyst. PPA titration data also enables the estimation of TiO2 particle size and reveals an important distinction

  15. pH titration monitored by quantum cascade laser-based vibrational circular dichroism.

    PubMed

    Rüther, Anja; Pfeifer, Marcel; Lórenz-Fonfría, Víctor A; Lüdeke, Steffen

    2014-04-10

    Vibrational circular dichroism (VCD) spectra of aqueous solutions of proline were recorded in the course of titrations from basic to acidic pH using a spectrometer equipped with a quantum cascade laser (QCL) as an infrared light source in the spectral range from 1320 to 1220 cm(-1). The pH-dependent spectra were analyzed by singular value decomposition and global fitting of a two-pK Henderson-Hasselbalch model. The analysis delivered relative fractions of the three different protonation species. Their agreement with the relative fractions obtained from performing the same analysis on pH-dependent Fourier transform infrared (FT-IR) and QCL-IR spectra validates the quantitative results from QCL-VCD. Global fitting of the pH-dependent VCD spectra of L-proline allowed for extraction of pure spectra corresponding to anionic, zwitterionic, and cationic L-proline. From a static experiment, only pure spectra of the zwitterion would be accessible in a straightforward way. A comparison to VCD spectra calculated for all three species led to assignment of vibrational modes that are characteristic for the respective protonation states. The study demonstrates the applicability of QCL-VCD both for quantitative evaluation and for qualitative interpretation of dynamic processes in aqueous solutions.

  16. pH titration monitored by quantum cascade laser-based vibrational circular dichroism.

    PubMed

    Rüther, Anja; Pfeifer, Marcel; Lórenz-Fonfría, Víctor A; Lüdeke, Steffen

    2014-04-10

    Vibrational circular dichroism (VCD) spectra of aqueous solutions of proline were recorded in the course of titrations from basic to acidic pH using a spectrometer equipped with a quantum cascade laser (QCL) as an infrared light source in the spectral range from 1320 to 1220 cm(-1). The pH-dependent spectra were analyzed by singular value decomposition and global fitting of a two-pK Henderson-Hasselbalch model. The analysis delivered relative fractions of the three different protonation species. Their agreement with the relative fractions obtained from performing the same analysis on pH-dependent Fourier transform infrared (FT-IR) and QCL-IR spectra validates the quantitative results from QCL-VCD. Global fitting of the pH-dependent VCD spectra of L-proline allowed for extraction of pure spectra corresponding to anionic, zwitterionic, and cationic L-proline. From a static experiment, only pure spectra of the zwitterion would be accessible in a straightforward way. A comparison to VCD spectra calculated for all three species led to assignment of vibrational modes that are characteristic for the respective protonation states. The study demonstrates the applicability of QCL-VCD both for quantitative evaluation and for qualitative interpretation of dynamic processes in aqueous solutions. PMID:24655319

  17. Diarylferrocene tweezers for cation binding.

    PubMed

    Lima, Carlos F R A C; Fernandes, Ana M; Melo, André; Gonçalves, Luís M; Silva, Artur M S; Santos, Luís M N B F

    2015-10-01

    The host-guest chemistry of ferrocene derivatives was explored by a combined experimental and theoretical study. Several 1-arylferrocenes and 1,1'-diarylferrocenes were synthesized by the Suzuki-Miyaura cross-coupling reaction. The ability of these compounds to bind small cations in the gas phase was investigated experimentally by electrospray ionization mass spectrometry (ESI-MS). The results evidenced a noticeable ability of all 1,1'-diarylferrocenes studied to bind cations, while the same was not observed for the corresponding 1-arylferrocenes nor ferrocene. The 1,1'-diarylferrocenecation relative interaction energies were evaluated by ESI-MS and quantum chemical calculations and showed that cation binding in these systems follows electrostatic trends. It was found that, due to their unique molecular shape and smooth torsional potentials, 1,1'-diarylferrocenes can act as molecular tweezers of small-sized cations in the gas phase. PMID:26309143

  18. Selective detection and enumeration of fecal coliforms in water by potentiometric measurement of lipoic acid reduction.

    PubMed

    Jouenne, T; Junter, G A; Charriere, G

    1985-11-01

    Water samples of various origins were inoculated into a specific coliform-selective lactose broth provided with lipoic (thioctic) acid, and the time evolution of the redox potential of the cultures was monitored during incubation at 41 degrees C by use of gold versus reference electrodes. Positive potential-time responses, i.e., 100-mV potential shifts recorded within 20 h of inoculation, were related to the initial number of fecal coliforms in the broth determined by control enumeration techniques, and the organisms responsible were isolated and identified by conventional procedures. A total of 30 samples of wastewater, 38 of surface water, 553 of groundwater, and 110 of drinking water were tested successively. A total of 240 natural water samples, including 172 groundwater samples, and 1 drinking water sample were found to be positive in the potentiometric test. The majority (i.e., 92.5%) of the relevant potentiometric detection times were shorter than 15 h, and 96% of these could be attributed to Escherichia coli. Fifteen hours corresponded to the limit for detecting 1 E. coli cell per 100 ml of water. About 78% of the potentiometric responses occurring after 15 h were induced by fecal coliforms other than E. coli (Enterobacter cloacae, Klebsiella pneumoniae, and Citrobacter freundii). Calibration curves relating detection times shorter than 15 h to fecal coliform (i.e., E. coli) concentrations were constructed for the natural water samples tested. There were minor variations in the average growth rate of the organisms in the relation to the contamination level of the water tested. The number of false-positive samples in the potentiometric test was equivalent to that of false-negative samples (groundwater or drinking water).

  19. Impact of Residual Inducer on Titratable Expression Systems

    PubMed Central

    Afroz, Taliman; Luo, Michelle L.; Beisel, Chase L.

    2015-01-01

    Inducible expression systems are widely employed for the titratable control of gene expression, yet molecules inadvertently present in the growth medium or synthesized by the host cells can alter the response profile of some of these systems. Here, we explored the quantitative impact of these residual inducers on the apparent response properties of inducible systems. Using a simple mathematical model, we found that the presence of residual inducer shrinks the apparent dynamic range and causes the apparent Hill coefficient to converge to one. We also found that activating systems were more sensitive than repressing systems to the presence of residual inducer and the response parameters were most heavily dependent on the original Hill coefficient. Experimental interrogation of common titratable systems based on an L-arabinose inducible promoter or a thiamine pyrophosphate-repressing riboswitch in Escherichia coli confirmed the predicted trends. We finally found that residual inducer had a distinct effect on “all-or-none” systems, which exhibited increased sensitivity to the added inducer until becoming fully induced. Our findings indicate that residual inducer or repressor alters the quantitative response properties of titratable systems, impacting their utility for scientific discovery and pathway engineering. PMID:26348036

  20. Lab on paper: iodometric titration on a printed card.

    PubMed

    Myers, Nicholas M; Kernisan, Emalee N; Lieberman, Marya

    2015-04-01

    A paper test card has been engineered to perform an iodometric titration, an application that requires storage and mixing on demand of several mutually incompatible reagents. The titration is activated when a user applies a test solution to the test card: the dried reagents are reconstituted and combined through a surface-tension-enabled mixing (STEM) mechanism. The device quantifies 0.8-15 ppm of iodine atoms from iodate in aqueous solutions. This is useful, for example, to quantify iodine levels in fortified salt. A blinded internal laboratory validation established the accuracy as 1.4 ppm I and the precision as 0.9 ppm I when the test card was read by newly trained users. Using computer software to process images, the accuracy and precision both improved to 0.9 ppm I. The paper card can also detect substandard β lactam antibiotics using an iodometric back-titration. When used to quantify amoxicillin, good distinction is achieved between solutions that differ by 0.15 mg/mL over a working range of 0-0.9 mg/mL. The test card was designed to meet the World Health Organization ASSURED criteria for use in low resource settings, where laboratory-based analytical procedures are often not available.

  1. New methods to titrate EIAV-based lentiviral vectors.

    PubMed

    Martin-Rendon, Enca; White, Linda J; Olsen, Anna; Mitrophanous, Kyriacos A; Mazarakis, Nicholas D

    2002-05-01

    Ideally, gene transfer vectors used in clinical protocols should only express the gene of interest. So far most vectors have contained marker genes to aid their titration. We have used quantitative real-time PCR to titrate equine infectious anemia virus (EIAV) vectors for gene therapy applications. Viral RNA was isolated from vector preparations and analyzed in a one-step RT-PCR reaction in which reverse transcription and amplification were combined in one tube. The PCR assay of vector stocks was quantitative and linear over four orders of magnitude. In tandem, the integration efficiency of these vectors has also been determined by real-time PCR, measuring the number of vector genomes in the target cells. We have found that these methods permit reliable and sensitive titration of lentiviral vectors independent from the expression of a transgene. They also allow us to determine the integration efficiency of different vector genomes. This technology has proved very useful, especially in the absence of marker genes and where vectors express multiple genes.

  2. Suspension culture titration: A simple method for measuring baculovirus titers.

    PubMed

    Matindoost, Leila; Chan, Leslie C L; Qi, Ying Mei; Nielsen, Lars K; Reid, Steven

    2012-08-01

    The baculovirus-insect cell expression system is an important technology for the production of recombinant proteins and baculovirus-based biopesticides. Budded virus titration is critical when scaling up baculovirus production processes in suspension cultures, to ensure reproducible infections, especially when a low multiplicity of infection (MOI) is applied. In this study, a simple suspension culture titration (SCT) assay was developed that involves accurate measurements of the initial cell densities (ICDs) and peak cell densities (PCDs) of an infected culture, from which the MOI and hence the virus inoculum infectious titer can be estimated, using the established Power-Nielsen baculovirus infection model. The SCT assay was assessed in parallel with two adherent culture-based assays (MTT and AlamarBlue) for the Heliothine baculovirus HaSNPV, and was shown to be more objective, time-efficient and reproducible. The model predicted a linear correlation between log(PCD/ICD) and log(MOI), hence an alternative model-independent SCT assay was also developed, which relies on a well-replicated standard curve relating suspension culture-derived PCD/ICD ratios with plaque or endpoint assay-derived MOIs. Standard curves with excellent linearity were generated for HaSNPV and the industrially significant rAcMNPV, demonstrating the feasibility of this simple titration approach, especially in terms of its applicability to a wide range of virus infection kinetics.

  3. Impact of Residual Inducer on Titratable Expression Systems.

    PubMed

    Afroz, Taliman; Luo, Michelle L; Beisel, Chase L

    2015-01-01

    Inducible expression systems are widely employed for the titratable control of gene expression, yet molecules inadvertently present in the growth medium or synthesized by the host cells can alter the response profile of some of these systems. Here, we explored the quantitative impact of these residual inducers on the apparent response properties of inducible systems. Using a simple mathematical model, we found that the presence of residual inducer shrinks the apparent dynamic range and causes the apparent Hill coefficient to converge to one. We also found that activating systems were more sensitive than repressing systems to the presence of residual inducer and the response parameters were most heavily dependent on the original Hill coefficient. Experimental interrogation of common titratable systems based on an L-arabinose inducible promoter or a thiamine pyrophosphate-repressing riboswitch in Escherichia coli confirmed the predicted trends. We finally found that residual inducer had a distinct effect on "all-or-none" systems, which exhibited increased sensitivity to the added inducer until becoming fully induced. Our findings indicate that residual inducer or repressor alters the quantitative response properties of titratable systems, impacting their utility for scientific discovery and pathway engineering. PMID:26348036

  4. Potentiometric, spectrophotometric and density functional study of the interaction of N-hydroxyacetamide with oxovanadium(IV): the influence of ligand to the V(IV)/V(V) oxi-reduction reaction.

    PubMed

    da Silva Santos, José Mauro; Carvalho, Sandra; Paniago, Eucler B; Duarte, Hélio A

    2003-05-01

    The interaction of N-hydroxyacetamide (acetohydroxamic acid, HL) with V(IV) in aqueous solution has been investigated using potentiometric and spectrophotometric experiments. Density functional method (DFT) has been used aiming to understand the ligand chelation at a molecular level. Stability constants have been estimated for species with the metal/ligand ratios 1:1 and 1:2 from spectrophotometric and potentiometric measurements. The stability of these V(IV) species toward oxidation has been investigated. Experiments carried out in an oxygen atmosphere led to the displacement of the titration curves with respect to the one obtained under inert atmosphere. Spectrophotometric evidence of the V(IV)/V(V) oxidation in the presence of N-hydroxyacetamide is presented. It has been shown that V(IV)/V(V) oxidation in the presence of N-hydroxyacetamide by the oxygen can be simulated using the standard programs for simulating the equilibrium in a multiligand/multimetal system. In this approach, the oxygen is considered a ligand and the log beta estimated from the standard oxidation potential. The structure and respective tautomers of the species have been optimized from DFT calculations. Geometrical and thermodynamical properties have been estimated for the most stable complexes. The VOL-->VOL(2) equilibrium constant has been theoretically estimated with a less than 1.5 logarithmic unit of error with respect to the experimental estimate. The oxidation process has also been investigated and it is adequately described by the equation: 4[VOL(2)]+2H(2)O+O(2)-->4[VO(OH)L(2)]. The calculated value of DeltaG for this reaction is about -46.2 kcal mol(-1), in excellent agreement with the experimental estimates.

  5. Epidermal tattoo potentiometric sodium sensors with wireless signal transduction for continuous non-invasive sweat monitoring.

    PubMed

    Bandodkar, Amay J; Molinnus, Denise; Mirza, Omar; Guinovart, Tomás; Windmiller, Joshua R; Valdés-Ramírez, Gabriela; Andrade, Francisco J; Schöning, Michael J; Wang, Joseph

    2014-04-15

    This article describes the fabrication, characterization and application of an epidermal temporary-transfer tattoo-based potentiometric sensor, coupled with a miniaturized wearable wireless transceiver, for real-time monitoring of sodium in the human perspiration. Sodium excreted during perspiration is an excellent marker for electrolyte imbalance and provides valuable information regarding an individual's physical and mental wellbeing. The realization of the new skin-worn non-invasive tattoo-like sensing device has been realized by amalgamating several state-of-the-art thick film, laser printing, solid-state potentiometry, fluidics and wireless technologies. The resulting tattoo-based potentiometric sodium sensor displays a rapid near-Nernstian response with negligible carryover effects, and good resiliency against various mechanical deformations experienced by the human epidermis. On-body testing of the tattoo sensor coupled to a wireless transceiver during exercise activity demonstrated its ability to continuously monitor sweat sodium dynamics. The real-time sweat sodium concentration was transmitted wirelessly via a body-worn transceiver from the sodium tattoo sensor to a notebook while the subjects perspired on a stationary cycle. The favorable analytical performance along with the wearable nature of the wireless transceiver makes the new epidermal potentiometric sensing system attractive for continuous monitoring the sodium dynamics in human perspiration during diverse activities relevant to the healthcare, fitness, military, healthcare and skin-care domains.

  6. Simulated changes in potentiometric levels resulting from groundwater development for phosphate mines, west-central Florida

    USGS Publications Warehouse

    Wilson, W.E.; Gerhart, J.M.

    1979-01-01

    A digital model of two-dimensional groundwater flow was used to predict changes in the potentiometric surface of the Floridan aquifer resulting from groundwater development for proposed and existing phosphate mines during 1976-2000. The modeled area covers 15,379 km2 in west-central Florida. In 1975, groundwater withdrawn from the Floridan aquifer for irrigation, phosphate mines, other industries and municipal supplies averaged about 28,500 l/s. Withdrawals for phosphate mines are expected to shift from Polk County to adjacent counties to the south and west, and to decline from about 7,620 l/s in 1975 to about 7,060 l/s in 2000. The model was calibrated under steady-state and transient conditions. Input parameters included aquifer transmissivity and storage coefficient; thickness, vertical hydraulic conductivity, and storage coefficient of the upper confining bed; altitudes of the water table and potentiometric surface; and groundwater withdrawals. Simulation of November 1976 to October 2000, using projected combined pumping rates for existing and proposed phosphate mines, resulted in a rise in the potentiometric surface of about 6 m in Polk County, and a decline of about 4 m in parts of Manatee and Hardee counties. ?? 1979.

  7. Potentiometric detection of chemical vapors using molecularly imprinted polymers as receptors

    NASA Astrophysics Data System (ADS)

    Liang, Rongning; Chen, Lusi; Qin, Wei

    2015-07-01

    Ion-selective electrode (ISE) based potentiometric gas sensors have shown to be promising analytical tools for detection of chemical vapors. However, such sensors are only capable of detecting those vapors which can be converted into ionic species in solution. This paper describes for the first time a polymer membrane ISE based potentiometric sensing system for sensitive and selective determination of neutral vapors in the gas phase. A molecularly imprinted polymer (MIP) is incorporated into the ISE membrane and used as the receptor for selective adsorption of the analyte vapor from the gas phase into the sensing membrane phase. An indicator ion with a structure similar to that of the vapor molecule is employed to indicate the change in the MIP binding sites in the membrane induced by the molecular recognition of the vapor. The toluene vapor is used as a model and benzoic acid is chosen as its indicator. Coupled to an apparatus manifold for preparation of vapor samples, the proposed ISE can be utilized to determine volatile toluene in the gas phase and allows potentiometric detection down to parts per million levels. This work demonstrates the possibility of developing a general sensing principle for detection of neutral vapors using ISEs.

  8. Potentiometric Surface of the Lower Patapsco Aquifer in Southern Maryland, September 2001

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Wheeler, Judith C.

    2002-01-01

    This report presents a map showing the potentiometric surface of the Lower Patapsco aquifer in the Patapsco Formation of Cretaceous age in Southern Maryland during September 2001. The map is based on water-level measurements in 65 wells. The potentiometric surface was as high as 110 feet above sea level near the northwestern boundary and outcrop area of the aquifer in northern Anne Arundel County. From this area, the potentiometric surface declined towards large well fields at Severndale, Arnold, and Annapolis. The ground-water levels declined to 78 feet below sea level at Severndale, 38 feet below sea level at Arnold, and 31 feet below sea level a few miles west of Annapolis. There was also a cone of depression covering a large area in Charles County that includes Waldorf, LaPlata, Indian Head, and the Morgantown power plant. The ground-water levels were as low as 173 feet below sea level at Waldorf, 126 feet below sea level at LaPlata, 112 feet below sea level at Indian Head, and 92 feet below sea level at the Morgantown power plant.

  9. Potentiometric surface of the lower Patapsco Aquifer in southern Maryland, September 1994

    USGS Publications Warehouse

    Curtin, Stephen E.; Mack, Frederick K.; Andreasen, David C.

    1995-01-01

    A map showing the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1994 was prepared from water levels measured in 56 wells. The potentiometric surface was at least 104 feet above sea level near the northwestern boundary and outcrop area of the aquifer in a topographically high area of Prince Georges County, and at least 89 feet above sea level in a similar setting in Anne Arundel County. From these high areas, the potentiometric surface declined to the south and southeast toward large well fields at Crofton, Severndle, Arnold, Annapolis, Waldorf, La Plata, Indian Head, and Morgantown. The ground-water levels reached 20 feet below sea level at Crofton, 80 feet below sea level at Severndale, 25 feet below sea level at Arnold, more than 10 feet below sea level near Annapolis, more than 130 feet below sea level in the Waldorf area, more than 100 feet below sea level at La Plata an Indian Head, an nearly 80 feet below sea level at the Morgantown powerplant.

  10. Potentiometric Surface of the Lower Patapsco Aquifer in Southern Maryland, September 1995

    USGS Publications Warehouse

    Curtin, Stephen E.; Andreasen, David C.; Mack, Frederick K.

    1996-01-01

    A map showing the potentiometric surface of the lower Patapsco aquifer in the Patapsco Formation of Cretaceous age in southern Maryland during September 1995 was prepared from water-level measurements in 69 wells. The potentiometric surface was 87 feet above sea level near the northwestern boundary and outcrop area of the aquifer in topographically high areas of Anne Arundel County. From this high area, the potentiometric surface declined to the south and southeast toward large well fields at Crofton, Severndale, Arnold, Annapolis, Waldorf, LaPlata, Indian Head, and Morgantown. The ground-water levels reached 18 feet below sea level at Crofton, 62 feet below sea level at Severndale, 26 feet below sea level at Arnold, more than 20 feet below sea level near Annapolis, 160 feet below sea level in the Waldorf area, nearly 100 feet below sea level at LaPlata, more than 110 feet below sea level at Indian Head, and 75 feet below sea level at the Morgantown powerplant.

  11. Potentiometric detection in UPLC as an easy alternative to determine cocaine in biological samples.

    PubMed

    Daems, Devin; van Nuijs, Alexander L N; Covaci, Adrian; Hamidi-Asl, Ezat; Van Camp, Guy; Nagels, Luc J

    2015-07-01

    The analytical methods which are often used for the determination of cocaine in complex biological matrices are a prescreening immunoassay and confirmation by chromatography combined with mass spectrometry. We suggest an ultra-high-pressure liquid chromatography combined with a potentiometric detector, as a fast and practical method to detect and quantify cocaine in biological samples. An adsorption/desorption model was used to investigate the usefulness of the potentiometric detector to determine cocaine in complex matrices. Detection limits of 6.3 ng mL(-1) were obtained in plasma and urine, which is below the maximum residue limit (MRL) of 25 ng mL(-1). A set of seven plasma samples and 10 urine samples were classified identically by both methods as exceeding the MRL or being inferior to it. The results obtained with the UPLC/potentiometric detection method were compared with the results obtained with the UPLC/MS method for samples spiked with varying cocaine concentrations. The intraclass correlation coefficient was 0.997 for serum (n =7) and 0.977 for urine (n =8). As liquid chromatography is an established technique, and as potentiometry is very simple and cost-effective in terms of equipment, we believe that this method is potentially easy, inexpensive, fast and reliable.

  12. Potentiometric detection of chemical vapors using molecularly imprinted polymers as receptors

    PubMed Central

    Liang, Rongning; Chen, Lusi; Qin, Wei

    2015-01-01

    Ion-selective electrode (ISE) based potentiometric gas sensors have shown to be promising analytical tools for detection of chemical vapors. However, such sensors are only capable of detecting those vapors which can be converted into ionic species in solution. This paper describes for the first time a polymer membrane ISE based potentiometric sensing system for sensitive and selective determination of neutral vapors in the gas phase. A molecularly imprinted polymer (MIP) is incorporated into the ISE membrane and used as the receptor for selective adsorption of the analyte vapor from the gas phase into the sensing membrane phase. An indicator ion with a structure similar to that of the vapor molecule is employed to indicate the change in the MIP binding sites in the membrane induced by the molecular recognition of the vapor. The toluene vapor is used as a model and benzoic acid is chosen as its indicator. Coupled to an apparatus manifold for preparation of vapor samples, the proposed ISE can be utilized to determine volatile toluene in the gas phase and allows potentiometric detection down to parts per million levels. This work demonstrates the possibility of developing a general sensing principle for detection of neutral vapors using ISEs. PMID:26215887

  13. Potentiometric map of the Paleozoic aquifer in northeastern Mississippi, November and December 1982

    USGS Publications Warehouse

    Darden, Daphne

    1984-01-01

    This potentiometric map is the second map of the Gordo aquifer in a series of maps prepared by the U.S. Geological Survey in cooperation with the Mississippi Department of Natural Resources , Bureau of Land and Water Resources, delineating the potentiometric surfaces of the major aquifers in Mississippi. The potentiometric surface of the Gordo aquifer slopes generally to the west away from the outcrop area and it is marked by large ground-water cones of depression in the Tupelo and Columbus areas. Water levels in or near the outcrop of the Gordo aquifer show little long-term change. Heavy withdrawals in the downdip area have caused water-level declines of about 2 feet per year since 1978 in much of the confined part of the aquifer. The water-level decline in the Tupelo area has averaged about 5 feet per year since 1966; however, there has been water-level rise at the center of the cone of depression as a result of a change in the distribution of pumping. (USGS)

  14. Potentiometric determination of pantoprazole using an ion-selective sensor based on polypyrrole doped films.

    PubMed

    Noronha, Bárbara V; Bindewald, Eduardo H; de Oliveira, Michelle C; Papi, Maurício A P; Bergamini, Márcio F; Marcolino-Jr, Luiz H

    2014-10-01

    The present work reports for the first time the use of polypyrrole (PPy) doped film for development of a potentiometric disposable sensor for determination of pantoprazole (PTZ), a drug used for ulcer treatment. Selective potentiometric response has been found by using a membrane of PPy doped with PTZ anions prepared under galvanostatic conditions at graphite pencil electrode (GPEM/PPy-PTZ) surface. Potentiometric response has been influenced for conditions adopted in polymerization and measurement step. After optimization of experimental (e.g. pH and time of conditioning) and instrumental parameters (e.g. current density and electrical charge) a linear analytical curve from 1.0 × 10(-5) to 1.1 × 10(-2) mol L(-1) with a slope of calibration of the 57.6 mV dec(-1) and limit of detection (LOD) of 6.9 × 10(-6) mol L(-1) was obtained. The determination of the PTZ content in pharmaceutical samples using the proposed methodology and official method recommended by Brazilian Pharmacopeia are in agreement at the 95% confidence level and within an acceptable range of error. PMID:25175244

  15. Potentiometric determination of pantoprazole using an ion-selective sensor based on polypyrrole doped films.

    PubMed

    Noronha, Bárbara V; Bindewald, Eduardo H; de Oliveira, Michelle C; Papi, Maurício A P; Bergamini, Márcio F; Marcolino-Jr, Luiz H

    2014-10-01

    The present work reports for the first time the use of polypyrrole (PPy) doped film for development of a potentiometric disposable sensor for determination of pantoprazole (PTZ), a drug used for ulcer treatment. Selective potentiometric response has been found by using a membrane of PPy doped with PTZ anions prepared under galvanostatic conditions at graphite pencil electrode (GPEM/PPy-PTZ) surface. Potentiometric response has been influenced for conditions adopted in polymerization and measurement step. After optimization of experimental (e.g. pH and time of conditioning) and instrumental parameters (e.g. current density and electrical charge) a linear analytical curve from 1.0 × 10(-5) to 1.1 × 10(-2) mol L(-1) with a slope of calibration of the 57.6 mV dec(-1) and limit of detection (LOD) of 6.9 × 10(-6) mol L(-1) was obtained. The determination of the PTZ content in pharmaceutical samples using the proposed methodology and official method recommended by Brazilian Pharmacopeia are in agreement at the 95% confidence level and within an acceptable range of error.

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

    PubMed

    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.

  17. Potentiometric Surface of the Upper Floridan Aquifer in the St. Johns River Water Management District and Vicinity, May 2008

    USGS Publications Warehouse

    Kinnaman, Sandra L.; Dixon, Joann F.

    2008-01-01

    This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 2008. Potentiometric contours are based on water-level measurements collected at 567 wells during the period May 6-May 27, near the end of the dry season. Some contours are inferred from previous potentiometric-surface maps with larger well networks. The potentiometric surface of the carbonate Upper Floridan aquifer responds mainly to rainfall, and more locally, to ground-water withdrawals and spring flow. Potentiometric-surface highs generally correspond to topographic highs where the aquifer is recharged. Springs and areas of diffuse upward leakage naturally discharge water from the aquifer and are most prevalent along the St. Johns River. Areas of discharge are reflected by depressions in the potentiometric surface. Ground-water withdrawals locally have lowered the potentiometric surface. Ground water in the Upper Floridan aquifer generally flows from potentiometric highs to potentiometric lows in a direction perpendicular to the contours. Measured values of the potentiometric surface ranged from 7 feet below NGVD29 near Fernandina Beach, Florida, to 124 feet above NGVD29 in Polk County, Florida. The average water level of the network in May 2008 was about 1 foot lower than the average in September 2007 following below-average rainfall during the dry season of 2007-08. Seasonal differences in network average water levels generally range from 4 to 6 feet. For 457 wells with previous measurements, May 2008 levels ranged from about 19 feet below to about 11 feet above September 2007 water levels. The average water level of the network in May 2008 was about 1 foot higher than the average in May 2007. For 544 wells with previous measurements, May 2008 levels ranged from about 8 feet below to about 13 feet above May 2007 water levels. Long-term hydrographs of ground-water levels for continuous and periodic wells are available

  18. Kinetic and chemical mechanisms for the effects of univalent cations on the spectral properties of aromatic amine dehydrogenase.

    PubMed Central

    Zhu, Z; Davidson, V L

    1998-01-01

    Univalent cations and pH influence the UV-visible absorption spectrum of the tryptophan tryptophylquinone (TTQ) enzyme, aromatic amine dehydrogenase (AADH). Little spectral perturbation was observed when pH was varied in the absence of univalent cations. The addition of alkali metal univalent cations (K+, Na+, Li+, Rb+ or Cs+) to oxidized AADH caused significant changes in its absorption spectrum. The apparent Kd for each cation, determined from titrations of the spectral perturbation, decreased with increasing pH. Transient kinetic studies involving rapid mixing of AADH with cations and pH jump revealed that the rate of the cation-induced spectral changes initially decreased with increasing cation concentration to a minimum value, then increased with increasing cation concentration. A kinetic model was developed to fit these data, determine the true pH-independent Kd values for K+ and Na+, and explain the pH-dependence of the apparent Kd. A chemical reaction mechanism, based on the kinetic data, is presented in which the metallic univalent cation facilitates the chemical modification of the TTQ prosthetic group to form an hydroxide adduct which gives rise to the spectral change. Addition of NH4(+)/NH3 to AADH caused changes in the absorption spectrum which were very different form those caused by addition of the metallic univalent cations. The kinetics of the reaction induced by addition of NH4+/NH3 were also different, being simple saturation kinetics. Another reaction mechanism is proposed for the NH4+/NH3-induced spectral change that involves nucleophilic addition of the unprotonated NH3 to TTQ. The general relevance of these data and models to the physiological reactions of TTQ-dependent enzymes and to the roles of univalent cations in modulating enzyme activity are discussed. PMID:9405291

  19. Evidence for Cation-Controlled Excited-State Localization in a Ruthenium Polypyridyl Compound.

    PubMed

    Beauvilliers, Evan E; Meyer, Gerald J

    2016-08-01

    The visible absorption and photoluminescence (PL) properties of the four neutral ruthenium diimine compounds [Ru(bpy)2(dcb)] (B2B), [Ru(dtb)2(dcb)] (D2B), [Ru(bpy)2(dcbq)] (B2Q), and [Ru(dtb)2(dcbq)] (D2Q), where bpy is 2,2'-bipyridine, dcb is 4,4'-(CO2(-))2-bpy, dtb is 4,4'-(tert-butyl)2-bpy, and dcbq is 4,4'-(CO2(-))2-2,2'-biquinoline, are reported in the presence of Lewis acidic cations present in fluid solutions at room temperature. In methanol solutions, the measured spectra were insensitive to the presence of these cations, while in acetonitrile a significant red shift in the PL spectra (≤1400 cm(-1)) was observed consistent with stabilization of the metal-to-ligand charge transfer (MLCT) excited state through Lewis acid-base adduct formation. No significant spectral changes were observed in control experiments with the tetrabutylammonium cation. Titration data with Li(+), Na(+), Mg(2+), Ca(2+), Zn(2+), Al(3+), Y(3+), and La(3+) showed that the extent of stabilization saturated at high cation concentration with magnitudes that scaled roughly with the cation charge-to-size ratio. The visible absorption spectra of D2Q was particularly informative due to the presence of two well-resolved MLCT absorption bands: (1) Ru → bpy, λmax ≈ 450 nm; and (2) Ru → dcbq, λmax ≈ 540 nm. The higher-energy band blue-shifted and the lower-energy band red-shifted upon cation addition. The PL intensity and lifetime of the excited state of B2B first increased with cation addition without significant shifts in the measured spectra, behavior attributed to a cation-induced change in the localization of the emissive excited state from bpy to dcb. The importance of excited-state localization and stabilization for solar energy conversion is discussed.

  20. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, September 2006

    USGS Publications Warehouse

    Ortiz, A.G.

    2007-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing freshwater are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2006. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 46.06 inches for west-central Florida (from October 2005 through September 2006) was 6.91 inches below the historical cumulative average of 52.97 inches (Southwest Florida Water Management District, 2006). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each

  1. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, May 2007

    USGS Publications Warehouse

    Ortiz, A.G.

    2008-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in May 2007. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the dry season, when ground-water levels usually are at an annual low and withdrawals for agricultural use typically are high. The cumulative average rainfall of 41.21 inches for west-central Florida (from June 2006 through May 2007) was 11.63 inches below the historical cumulative average of 52.84 inches (Southwest Florida Water Management District, 2007). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the

  2. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, September 2007

    USGS Publications Warehouse

    Ortiz, A.G.

    2008-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2007. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 39.50 inches for west-central Florida (from October 2006 through September 2007) was 13.42 inches below the historical cumulative average of 52.92 inches (Southwest Florida Water Management District, 2007). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each

  3. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, May 2008

    USGS Publications Warehouse

    Ortiz, A.G.

    2008-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in May 2008. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the dry season, when ground-water levels usually are at an annual low and withdrawals for agricultural use typically are high. The cumulative average rainfall of 46.95 inches for west-central Florida (from June 2007 through May 2008) was 5.83 inches below the historical cumulative average of 52.78 inches (Southwest Florida Water Management District, 2008). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the

  4. Potentiometric surface of the Upper Floridan aquifer, west-central Florida, September 2005

    USGS Publications Warehouse

    Ortiz, A.G.

    2006-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing freshwater are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District (SWFWMD) and is used for major public supply, domestic use, irrigation, and brackish-water desalination in coastal communties (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2005. The potentiometric surface is an imaginary surface, connecting points of equal altitude to which water will rise in a tightly cased well that taps a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 55.19 inches for west-central Florida (from October 2004 through September 2005) was 2.00 inches above the historical cumulative average of 53.19 inches (Southwest Florida Water Management District, 2005). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to the most recent calendar year) and are updated monthly by the SWFWMD. This report, prepared by the U.S. Geological Survey (USGS) in cooperation with the SWFWMD, is part of a semiannual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the approximate annual low and high water

  5. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, September 2008

    USGS Publications Warehouse

    Ortiz, Anita G.

    2009-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in September 2008. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the wet season, when ground-water levels usually are at an annual high and withdrawals for agricultural use typically are low. The cumulative average rainfall of 50.63 inches for west-central Florida (from October 2007 through September 2008) was 2.26 inches below the historical cumulative average of 52.89 inches (Southwest Florida Water Management District, 2008). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each

  6. Potentiometric determination of trace amounts of aluminium utilizing polyvinyl chloride membrane and coated platinum sensors based on E-N'-(2-hydroxy-3-methoxybenzylidene) benzohydrazide.

    PubMed

    Tajik, Somayeh; Taher, Mohammad Ali; Sheikhshoaie, Iran

    2013-01-01

    This paper describes the construction and performance characteristics of novel polyvinyl chloride membrane (PME) and coated platinum (CPtE) aluminium (Al) ion selective electrodes based on E-N'-(2-hydroxy-3-methoxybenzylidene) benzohydrazide. The electrodes exhibited linear responses with near Nernstian slopes of 19.9 +/- 0.3 (PME) and 20.1 +/- 0.4 (CPtE) mV/decade of activity within the Al3+ ion concentration range of 3.0 x 10(-7) to 1.0 x 10(-2) M for the PME and 1.0 x 10(-7)-1.0 x 10(-2) M for the CPtE. These sensors were applicable in a pH range of 3.0 to 7.0. The LODs of the PME and CPtE were 1.7 x 10(-7) and 5.6 x 10(-8) M, respectively. They had a response time of less than 10 s and could be used practically for a period of at least 2 months without measurable divergence in results. The isothermal temperature coefficient of the PME was 1.12 x 10(-3) V/degrees C, and it can tolerate partially nonaqueous media up to 25%. The electrodes showed excellent selectivity towards Al3+ ions in the presence of a wide range of alkali, alkaline earth, and transition metals ions. They were successfully applied for the direct determination of Al3+ ions in tap water, aqueduct water, mineral water, and Al-Mg syrup and as indicator electrodes in potentiometric titration of Al ions with EDTA.

  7. Potentiometric determination of trace amounts of aluminium utilizing polyvinyl chloride membrane and coated platinum sensors based on E-N'-(2-hydroxy-3-methoxybenzylidene) benzohydrazide.

    PubMed

    Tajik, Somayeh; Taher, Mohammad Ali; Sheikhshoaie, Iran

    2013-01-01

    This paper describes the construction and performance characteristics of novel polyvinyl chloride membrane (PME) and coated platinum (CPtE) aluminium (Al) ion selective electrodes based on E-N'-(2-hydroxy-3-methoxybenzylidene) benzohydrazide. The electrodes exhibited linear responses with near Nernstian slopes of 19.9 +/- 0.3 (PME) and 20.1 +/- 0.4 (CPtE) mV/decade of activity within the Al3+ ion concentration range of 3.0 x 10(-7) to 1.0 x 10(-2) M for the PME and 1.0 x 10(-7)-1.0 x 10(-2) M for the CPtE. These sensors were applicable in a pH range of 3.0 to 7.0. The LODs of the PME and CPtE were 1.7 x 10(-7) and 5.6 x 10(-8) M, respectively. They had a response time of less than 10 s and could be used practically for a period of at least 2 months without measurable divergence in results. The isothermal temperature coefficient of the PME was 1.12 x 10(-3) V/degrees C, and it can tolerate partially nonaqueous media up to 25%. The electrodes showed excellent selectivity towards Al3+ ions in the presence of a wide range of alkali, alkaline earth, and transition metals ions. They were successfully applied for the direct determination of Al3+ ions in tap water, aqueduct water, mineral water, and Al-Mg syrup and as indicator electrodes in potentiometric titration of Al ions with EDTA. PMID:23513978

  8. Carbonic acid ionization and the stability of sodium bicarbonate and carbonate ion pairs to 200 °C - A potentiometric and spectrophotometric study

    NASA Astrophysics Data System (ADS)

    Stefánsson, Andri; Bénézeth, Pascale; Schott, Jacques

    2013-11-01

    Carbonic acid ionization and sodium bicarbonate and carbonate ion pair formation constants have been experimentally determined in dilute hydrothermal solutions to 200 °C. Two experimental approaches were applied, potentiometric acid-base titrations at 10-60 °C and spectrophotometric pH measurements using the pH indicators, 2-napthol and 4-nitrophenol, at 25-200 °C. At a given temperature, the first and second ionization constants of carbonic acid (K1, K2) and the ion pair formation constants for NaHCO(aq)(K) and NaCO3-(aq)(K) were simultaneously fitted to the data. Results of this study compare well with previously determined values of K1 and K2. The NaHCO(aq) and NaCO3-(aq) ion pair formation constants vary between 25 and 200 °C having values of logK=-0.18 to 0.58 and logK=1.01 to 2.21, respectively. These ion pairs are weak at low-temperatures but become increasingly important with increasing temperature under neutral to alkaline conditions in moderately dilute to concentrated NaCl solutions, with NaCO3-(aq) predominating over CO32-(aq) in ⩾0.1 M NaCl solution at temperatures above 100 °C. The results demonstrate that NaCl cannot be considered as an inert (non-complexing) electrolyte in aqueous carbon dioxide containing solutions at elevated temperatures.

  9. Potentiometric and spectrophotometric study of the stability of magnesium carbonate and bicarbonate ion pairs to 150 °C and aqueous inorganic carbon speciation and magnesite solubility

    NASA Astrophysics Data System (ADS)

    Stefánsson, Andri; Bénézeth, Pascale; Schott, Jacques

    2014-08-01

    The formation constants of magnesium bicarbonate and carbonate ion pairs have been experimentally determined in dilute hydrothermal solutions to 150 °C. Two experimental approaches were applied, potentiometric acid-base titrations at 10-60 °C and spectrophotometric pH measurements using two pH indicators, 2-naphthol and 4-nitrophenol, at 25 and 80-150 °C. At a given temperature, the first and second ionization constants of carbonic acid (K1, K2) and the ion pair formation constants for MgHCO3+(aq) (KMgHCO3+) and MgCO3(aq) (KMgCO3) were simultaneously fitted to the data. Results of this study compare well with previously determined values of K1 and K2. The formation constants of MgHCO3+(aq) and MgCO3(aq) ion pairs increased significantly with increasing temperature, with values of logKMgHCO3+ = 1.14 and 1.75 and of logKMgCO3 = 2.86 and 3.48 at 10 °C and 100 °C, respectively. These ion pairs are important aqueous species under neutral to alkaline conditions in moderately dilute to concentrated Mg-containing solutions, with MgCO3(aq) predominating over CO32-(aq) in solutions at pH >8. The predominance of magnesium carbonate over carbonate is dependent on the concentration of dissolved magnesium and the ratio of magnesium over carbonate. With increasing temperature and at alkaline pH, brucite solubility further reduced the magnesium concentration to levels below 1 mmol kg-1, thus limiting availability of Mg2+(aq) for magnesite precipitation.

  10. Potentiometric surface of the upper Floridan Aquifer in the St. Johns River Water Management District and vicinity, May 1995

    USGS Publications Warehouse

    Knowles, Leel; O'Reilly, A. M.; Phelps, G.G.; Bradner, L.A.

    1995-01-01

    This map depicts the potentiometric surface of the Upper Floridan aquifer in the St. Johns River Water Management District and vicinity for May 1995. The map is based on water-level measurements made at more than 900 wells and springs. Approximately 30 new wells were added to better define the potentiometric surface mainly in the northwest area of the map. Data on the map were contoured using 5-foot contour intervals in most areas. Two new wells located north of Rainbow Springs indicate a slight northward extension of the depressed area surrounding the springs. Several new wells in Bradford County indicate a slight reduction in the size of the potentiometric-surface high along the northwest edge of the county. The potentiometric surface of this karstic aquifer generally reflects land surface topography. Potentiometric-surface highs often correspond to topographic highs, which are areas of recharge to the Upper Floridan aquifer. Springs within topographic lows along with areas of more diffuse upward leakage are natural zones of discharge. Municipal, agricultural, and industrial withdrawals have lowered the potentiometric surface in some areas. The potentiometric surface ranged from 127 feet above sea level in Polk County to 84 feet below sea level in southeast Georgia near the St. Marys River. Water levels measured in May 1995 generally were about 0 to 4 feet higher than those measured in May 1994 except in St. Lucie County and near Rainbow Springs, where levels were 1 to 3 feet lower. Generally, May 1995 water levels were 0 to 5 feet lower than levels in September 1994, except near Orlando, where levels were 6 to 12 feet lower, and across the northwest corner of the map area which includes Marion, Alachua, Bradford, Baker, and Nassau Counties, north and west Duval County, and south Georgia. (USGS)

  11. Potentiometric Surface of the Upper Floridan Aquifer, West-Central Florida, May 2009

    USGS Publications Warehouse

    Ortiz, Anita G.

    2009-01-01

    The Floridan aquifer system consists of the Upper and Lower Floridan aquifers separated by the middle confining unit. The middle confining unit and the Lower Floridan aquifer in west-central Florida generally contain highly mineralized water. The water-bearing units containing fresh water are herein referred to as the Upper Floridan aquifer. The Upper Floridan aquifer is the principal source of water in the Southwest Florida Water Management District and is used for major public supply, domestic use, irrigation, and brackish water desalination in coastal communities (Southwest Florida Water Management District, 2000). This map report shows the potentiometric surface of the Upper Floridan aquifer measured in May 2009. The potentiometric surface is an imaginary surface connecting points of equal altitude to which water will rise in tightly-cased wells that tap a confined aquifer system (Lohman, 1979). This map represents water-level conditions near the end of the dry season, when ground-water levels usually are at an annual low and withdrawals for agricultural use typically are high. The cumulative average rainfall of 48.53 inches for west-central Florida (from June 2008 through May 2009) was 4.12 inches below the historical cumulative average of 52.65 inches (Southwest Florida Water Management District, 2009). Historical cumulative averages are calculated from regional rainfall summary reports (1915 to most recent complete calendar year) and are updated monthly by the Southwest Florida Water Management District. This report, prepared by the U.S. Geological Survey in cooperation with the Southwest Florida Water Management District, is part of a semi-annual series of Upper Floridan aquifer potentiometric-surface map reports for west-central Florida. Potentiometric-surface maps have been prepared for January 1964, May 1969, May 1971, May 1973, May 1974, and for each May and September since 1975. Water-level data are collected in May and September each year to show the

  12. Cationic β-cyclodextrin polymer applied to a dual cyclodextrin polyelectrolyte multilayer system.

    PubMed

    Junthip, Jatupol; Tabary, Nicolas; Leclercq, Laurent; Martel, Bernard

    2015-08-01

    A polyelectrolyte multilayer film (PEM) based on cationic and anionic β-cyclodextrin polyelectrolytes was coated onto a textile substrate for future drug delivery purposes. We firstly synthesized a novel cationic β-cyclodextrin polymer (polyEPG-CD) by crosslinking β-cyclodextrin (βCD) with epichlorohydrin (EP) under basic conditions, in the presence of glycidyltrimetrylammonium chloride (GTMAC) as cationizing group. The influence of preparation conditions has been investigated in order to preferably obtain a water soluble fraction whose charge density and molecular weights were optimal for the layer-by-layer (LbL) deposition process. The different cationic cyclodextrin polymers obtained were characterized by FTIR, NMR, colloidal titration, conductimetry, thermogravimetric analysis and size exclusion chromatography. Besides, the counterpart polyelectrolyte was a β-cyclodextrin polymer crosslinked with citric acid, polyCTR-CD, whose synthesis and characterization have been previously reported. Finally we realized the Layer by Layer (LbL) build-up of the PEM coating onto the textile support, using the dip coating method, by alternatively soaking it in cationic polyEPG-CD and anionic polyCTR-CD solutions. This multilayer self-assembly was monitored by SEM, gravimetry and OWLS in function of both polyelectrolytes concentrations and ratios. Solutions parameters such as pH, ionic strenght were also discussed.

  13. Cationic-modified cyclodextrin nanosphere/anionic polymer as flocculation/sorption systems.

    PubMed

    Xiao, Huining; Cezar, Norlito

    2005-03-15

    Simultaneous removal of dissolved and colloidal substances has been a challenging task. The cationic-modified beta-cyclodextrin nanospheres synthesized in this work, in conjunction with a water-soluble polyacrylamide-based anionic polymer, potentially provide a novel approach to address the problem. The cyclodextrin was rendered cationic using (2,3-epoxypropyl)trimethylammonium chloride as a reagent. The cationicity of the modified cyclodextrin and the reaction between cyclodextrin and the reagent were characterized by electrophoresis measurement, polyelectrolyte titration, and NMR. As a dual-component flocculation system, the cationic cyclodextrin/anionic polymer significantly induced clay flocculation, lowering the relative turbidity of the clay suspension over a wide pH range. Meanwhile, as a nanospherical absorbent, the modified cyclodextrins exhibited strong affinity toward aromatic compounds via inclusion complex formation in the hydrophobic cavities, which was monitored by UV spectroscopy. These systems facilitated the simultaneous removal of dissolved and colloidal substances, which was unachievable previously. In addition, the interaction between anionic polymers and the clay particles pretreated with cationic cyclodextrin was investigated in order to reveal the flocculation mechanism.

  14. Cationic-modified cyclodextrin nanosphere/anionic polymer as flocculation/sorption systems.

    PubMed

    Xiao, Huining; Cezar, Norlito

    2005-03-15

    Simultaneous removal of dissolved and colloidal substances has been a challenging task. The cationic-modified beta-cyclodextrin nanospheres synthesized in this work, in conjunction with a water-soluble polyacrylamide-based anionic polymer, potentially provide a novel approach to address the problem. The cyclodextrin was rendered cationic using (2,3-epoxypropyl)trimethylammonium chloride as a reagent. The cationicity of the modified cyclodextrin and the reaction between cyclodextrin and the reagent were characterized by electrophoresis measurement, polyelectrolyte titration, and NMR. As a dual-component flocculation system, the cationic cyclodextrin/anionic polymer significantly induced clay flocculation, lowering the relative turbidity of the clay suspension over a wide pH range. Meanwhile, as a nanospherical absorbent, the modified cyclodextrins exhibited strong affinity toward aromatic compounds via inclusion complex formation in the hydrophobic cavities, which was monitored by UV spectroscopy. These systems facilitated the simultaneous removal of dissolved and colloidal substances, which was unachievable previously. In addition, the interaction between anionic polymers and the clay particles pretreated with cationic cyclodextrin was investigated in order to reveal the flocculation mechanism. PMID:15721912

  15. A titration model for evaluating calcium hydroxide removal techniques

    PubMed Central

    PHILLIPS, Mark; McCLANAHAN, Scott; BOWLES, Walter

    2015-01-01

    Objective Calcium hydroxide (Ca(OH)2) 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(OH)2 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(OH)2 for 7 days, which were dissolved out and titrated to quantitate the residual Ca(OH)2 recovered from each root to produce a standard curve. Forty-eight of the remaining teeth were filled with equal amounts of Ca(OH)2 followed by gross Ca(OH)2 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(OH)2 was dissolved with glycerin and titrated to measure residual Ca(OH)2 left in the root. Results No method completely removed all residual Ca(OH)2. The addition of 30 s PUI with or without apical file use removed Ca(OH)2 significantly better than irrigation alone. Conclusions This technique allowed quantification of residual Ca(OH)2. The use of PUI (with or without apical file) resulted in significantly lower Ca(OH)2 residue compared to irrigation alone. PMID:25760272

  16. Titratable acidity of beverages influences salivary pH recovery.

    PubMed

    Tenuta, Livia Maria Andaló; Fernández, Constanza Estefany; Brandão, Ana Carolina Siqueira; Cury, Jaime Aparecido

    2015-01-01

    A low pH and a high titratable acidity of juices and cola-based beverages are relevant factors that contribute to dental erosion, but the relative importance of these properties to maintain salivary pH at demineralizing levels for long periods of time after drinking is unknown. In this crossover study conducted in vivo, orange juice, a cola-based soft drink, and a 10% sucrose solution (negative control) were tested. These drinks differ in terms of their pH (3.5 ± 0.04, 2.5 ± 0.05, and 5.9 ± 0.1, respectively) and titratable acidity (3.17 ± 0.06, 0.57 ± 0.04 and < 0.005 mmols OH- to reach pH 5.5, respectively). Eight volunteers with a normal salivary flow rate and buffering capacity kept 15 mL of each beverage in their mouth for 10 s, expectorated it, and their saliva was collected after 15, 30, 45, 60, 90, and 120 s. The salivary pH, determined using a mini pH electrode, returned to the baseline value at 30 s after expectoration of the cola-based soft drink, but only at 90 s after expectoration of the orange juice. The salivary pH increased to greater than 5.5 at 15 s after expectoration of the cola drink and at 30 s after expectoration of the orange juice. These findings suggest that the titratable acidity of a beverage influences salivary pH values after drinking acidic beverages more than the beverage pH.

  17. Electrochemical sample matrix elimination for trace-level potentiometric detection with polymeric membrane ion-selective electrodes.

    PubMed

    Chumbimuni-Torres, Karin Y; Calvo-Marzal, Percy; Wang, Joseph; Bakker, Eric

    2008-08-01

    Potentiometric sensors are today sufficiently well understood and optimized to reach ultratrace level (subnanomolar) detection limits for numerous ions. In many cases of practical relevance, however, a high electrolyte background hampers the attainable detection limits. A particularly difficult sample matrix for potentiometric detection is seawater, where the high saline concentration forms a major interfering background and reduces the activity of most trace metals by complexation. This paper describes for the first time a hyphenated system for the online electrochemically modulated preconcentration and matrix elimination of trace metals, combined with a downstream potentiometric detection with solid contact polymeric membrane ion-selective microelectrodes. Following the preconcentration at the bismuth-coated electrode, the deposited metals are oxidized and released to a medium favorable to potentiometric detection, in this case calcium nitrate. Matrix interferences arising from the saline sample medium are thus circumvented. This concept is successfully evaluated with cadmium as a model trace element and offers potentiometric detection down to low parts per billion levels in samples containing 0.5 M NaCl background electrolyte.

  18. Acid Base Titrations in Nonaqueous Solvents and Solvent Mixtures

    NASA Astrophysics Data System (ADS)

    Barcza, Lajos; Buvári-Barcza, Ágnes

    2003-07-01

    The acid base determination of different substances by nonaqueous titrations is highly preferred in pharmaceutical analyses since the method is quantitative, exact, and reproducible. The modern interpretation of the reactions in nonaqueous solvents started in the last century, but several inconsistencies and unsolved problems can be found in the literature. The acid base theories of Brønsted Lowry and Lewis as well as the so-called solvent theory are outlined first, then the promoting (and leveling) and the differentiating effects are discussed on the basis of the hydrogen-bond concept. Emphasis is put on the properties of formic acid and acetic anhydride since their importance is increasing.

  19. Complex formation of fenchone with α-cyclodextrin: NMR titrations.

    PubMed

    Nowakowski, Michał; Ejchart, Andrzej

    2014-01-01

    (13)C NMR titration studies of inclusion complexes of bicyclic terpenoid, fenchone enantiomers with α-cyclodextrin revealed their 1:2 guest-host stoichiometry. Sequential binding constants were determined indicating a strong binding cooperativity of two α-cyclodextrin to fenchone. The overall association constants were used to calculate the Gibbs free energies of diastereomeric complex formation, which might be used as a measure of chiral recognition of fenchone by α-cyclodextrin. These results were compared with corresponding data derived for camphor, which is an isomeric bicyclic terpenoid.

  20. Plaque titration and inhibition tests for bovine parvovirus.

    PubMed

    Durham, P J; Johnson, R H

    1984-08-01

    Bovine parvovirus readily produced plaques when inoculated into 60% confluent, actively growing bovine embryonic lung cells. Incorporation of DEAE-dextran, MgCl2 and DMSO in the agarose overlay medium was found to improve plaque production, especially with the latter chemical. In contrast, protamine sulphate inhibited plaque development. It was found that plaque titration and plaque inhibition tests could be conveniently carried out in 24-well cell culture plates, using an agarose overlay containing DMSO, DEAE-dextran and foetal calf serum. The procedures were highly sensitive, when compared with other established techniques.

  1. Studying the allosteric energy cycle by isothermal titration calorimetry.

    PubMed

    Martinez-Julvez, Marta; Abian, Olga; Vega, Sonia; Medina, Milagros; Velazquez-Campoy, Adrian

    2012-01-01

    Isothermal titration calorimetry (ITC) is a powerful biophysical technique which allows a complete thermodynamic characterization of protein interactions with other molecules. The possibility of dissecting the Gibbs energy of interaction into its enthalpic and entropic contributions, as well as the detailed additional information experimentally accessible on the intermolecular interactions (stoichiometry, cooperativity, heat capacity changes, and coupled equilibria), make ITC a suitable technique for studying allosteric interactions in proteins. Two experimental methodologies for the characterization of allosteric heterotropic ligand interactions by ITC are described in this chapter, illustrated with two proteins with markedly different structural and functional features: a photosynthetic electron transfer protein and a drug target viral protease.

  2. Interaction between bisphenol A and tannic Acid: Spectroscopic titration approach

    NASA Astrophysics Data System (ADS)

    Omoike, Anselm; Brandt, Benjamin

    2011-06-01

    The interaction between tannic acid (TA) and bisphenol A (BPA), an endocrine disruptor, was studied by absorption and fluorescence titration techniques. The binding constants and corresponding thermodynamic parameters at different temperatures (294, 296, 298, 300 and 303 K) were determined. The intrinsic fluorescence of BPA was strongly quenched by TA and the quenching mechanism is attributed to static quenching. The thermodynamic data revealed that the formation of TA-BPA complex was exothermic, entropic-driven, and spontaneous. Furthermore, hydrogen and van der Waals interactions seem to be the major driving forces for the formation of the nonfluorescent TA-BPA complex.

  3. Isothermal Titration Calorimetry: Assisted Crystallization of RNA-Ligand Complexes.

    PubMed

    Da Veiga, Cyrielle; Mezher, Joelle; Dumas, Philippe; Ennifar, Eric

    2016-01-01

    The success rate of nucleic acids/ligands co-crystallization can be significantly improved by performing preliminary biophysical analyses. Among suitable biophysical approaches, isothermal titration calorimetry (ITC) is certainly a method of choice. ITC can be used in a wide range of experimental conditions to monitor in real time the formation of the RNA- or DNA-ligand complex, with the advantage of providing in addition the complete binding profile of the interaction. Following the ITC experiment, the complex is ready to be concentrated for crystallization trials. This chapter describes a detailed experimental protocol for using ITC as a tool for monitoring RNA/small molecule binding, followed by co-crystallization.

  4. Interaction between bisphenol A and tannic acid: spectroscopic titration approach.

    PubMed

    Omoike, Anselm; Brandt, Benjamin

    2011-06-01

    The interaction between tannic acid (TA) and bisphenol A (BPA), an endocrine disruptor, was studied by absorption and fluorescence titration techniques. The binding constants and corresponding thermodynamic parameters at different temperatures (294, 296, 298, 300 and 303 K) were determined. The intrinsic fluorescence of BPA was strongly quenched by TA and the quenching mechanism is attributed to static quenching. The thermodynamic data revealed that the formation of TA-BPA complex was exothermic, entropic-driven, and spontaneous. Furthermore, hydrogen and van der Waals interactions seem to be the major driving forces for the formation of the nonfluorescent TA-BPA complex.

  5. Unraveling the thermodynamics and kinetics of RNA assembly: surface plasmon resonance, isothermal titration calorimetry, and circular dichroism.

    PubMed

    Hoogstraten, Charles G; Sumita, Minako; White, Neil A

    2014-01-01

    The mechanisms and driving forces of the assembly of RNA tertiary structure are a topic of much current interest. In several systems, including our own work in the docking transition of the hairpin ribozyme, intramolecular RNA tertiary folding has been converted into an intermolecular binding event, allowing the full power of contemporary biophysical techniques to be brought to bear on the analysis. We review the use of three such methods: circular dichroism to isolate the binding of multivalent cations coupled to tertiary assembly, surface plasmon resonance to determine the rates of association and dissociation, and isothermal titration calorimetry to dissect the thermodynamic contributions to RNA assembly events. We pay particular attention to practical aspects of these studies, such as careful preparation of samples with fixed free concentrations of cations in order to avoid errors due to ion depletion effects that are common in RNA systems. Examples of applications from our own work with the hairpin ribozyme are shown. Distinctions among the data handling procedures for the various techniques used and solution conditions encountered are also discussed.

  6. A microfabrication-based approach to quantitative isothermal titration calorimetry.

    PubMed

    Wang, Bin; Jia, Yuan; Lin, Qiao

    2016-04-15

    Isothermal titration calorimetry (ITC) directly measures heat evolved in a chemical reaction to determine equilibrium binding properties of biomolecular systems. Conventional ITC instruments are expensive, use complicated design and construction, and require long analysis times. Microfabricated calorimetric devices are promising, although they have yet to allow accurate, quantitative ITC measurements of biochemical reactions. This paper presents a microfabrication-based approach to integrated, quantitative ITC characterization of biomolecular interactions. The approach integrates microfabricated differential calorimetric sensors with microfluidic titration. Biomolecules and reagents are introduced at each of a series of molar ratios, mixed, and allowed to react. The reaction thermal power is differentially measured, and used to determine the thermodynamic profile of the biomolecular interactions. Implemented in a microdevice featuring thermally isolated, well-defined reaction volumes with minimized fluid evaporation as well as highly sensitive thermoelectric sensing, the approach enables accurate and quantitative ITC measurements of protein-ligand interactions under different isothermal conditions. Using the approach, we demonstrate ITC characterization of the binding of 18-Crown-6 with barium chloride, and the binding of ribonuclease A with cytidine 2'-monophosphate within reaction volumes of approximately 0.7 µL and at concentrations down to 2mM. For each binding system, the ITC measurements were completed with considerably reduced analysis times and material consumption, and yielded a complete thermodynamic profile of the molecular interaction in agreement with published data. This demonstrates the potential usefulness of our approach for biomolecular characterization in biomedical applications. PMID:26655185

  7. Determination of berkelium by the method of spectrophotometric titration

    SciTech Connect

    Frolova, L.M.; Vityutnev, V.M.; Vasil'ev, V.M.

    1987-01-01

    The method that the authors propose consists of the following: berkelium is oxidized electrochemically, spectrophotometric titration of berkelium(IV) by a solution of the reducing agent is performed, and the amount of berkelium(IV) is determined according to the volume of the titrant, and considering the degree of oxidation of berkelium(III) to berkelium(IV), the total berkelium content in the sample is also determined. In this case the necessity for preliminary determination of the molar extinction coefficient of berkelium(IV) under the experimental conditions falls away. Moreover, the radiometric method of determining the berkelium content is not used. Successful titration requires selection of a reagent which, on the one hand, would rapidly reduce berkelium(VI), but on the other hand, neither itself nor the reaction products would interfere with the measurement of the optical density of berkelium(IV). As is well known, berkelium(IV) is quantitatively and rapidly reduced by hydrogen peroxide (10, 11), hydroxylamine (11), and nitrous acid (9). After preliminary experiments, they selected hydrogen peroxide and sodium nitrite as the titrants.

  8. Titration of human coronaviruses using an immunoperoxidase assay.

    PubMed

    Lambert, Francine; Jacomy, Helene; Marceau, Gabriel; Talbot, Pierre J

    2008-01-01

    Determination of infectious viral titers is a basic and essential experimental approach for virologists. Classical plaque assays cannot be used for viruses that do not cause significant cytopathic effects, which is the case for prototype strains 229E and OC43 of human coronavirus (HCoV).Therefore, an alternative indirect immunoperoxidase assay (IPA) was developed for the detection and titration of these viruses and is described herein. Susceptible cells are inoculated with serial logarithmic dilutions of virus-containing samples in a 96-well plate format. After viral growth,viral detection by IPA yields the infectious virus titer, expressed as 'Tissue Culture Infectious Dose 50 percent' (TCID50). This represents the dilution of a virus-containing sample at which half of a series of laboratory wells contain infectious replicating virus. This technique provides are liable method for the titration of HCoV-229E and HCoV-OC43 in biological samples such as cells, tissues and fluids [corrected].

  9. Measuring the Kinetics of Molecular Association by Isothermal Titration Calorimetry.

    PubMed

    Vander Meulen, Kirk A; Horowitz, Scott; Trievel, Raymond C; Butcher, Samuel E

    2016-01-01

    The real-time power response inherent in an isothermal titration calorimetry (ITC) experiment provides an opportunity to directly analyze association kinetics, which, together with the conventional measurement of thermodynamic quantities, can provide an incredibly rich description of molecular binding in a single experiment. Here, we detail our application of this method, in which interactions occurring with relaxation times ranging from slightly below the instrument response time constant (12.5 s in this case) to as large as 600 s can be fully detailed in terms of both the thermodynamics and kinetics. In a binding titration scenario, in the most general case an injection can reveal an association rate constant (kon). Under more restrictive conditions, the instrument time constant-corrected power decay following each injection is simply an exponential decay described by a composite rate constant (kobs), from which both kon and the dissociation rate constant (koff) can be extracted. The data also support the viability of this exponential approach, for kon only, for a slightly larger set of conditions. Using a bimolecular RNA folding model and a protein-ligand interaction, we demonstrate and have internally validated this approach to experiment design, data processing, and error analysis. An updated guide to thermodynamic and kinetic regimes accessible by ITC is provided.

  10. Measuring Multivalent Binding Interactions by Isothermal Titration Calorimetry.

    PubMed

    Dam, Tarun K; Talaga, Melanie L; Fan, Ni; Brewer, Curtis F

    2016-01-01

    Multivalent glycoconjugate-protein interactions are central to many important biological processes. Isothermal titration calorimetry (ITC) can potentially reveal the molecular and thermodynamic basis of such interactions. However, calorimetric investigation of multivalency is challenging. Binding of multivalent glycoconjugates to proteins (lectins) often leads to a stoichiometry-dependent precipitation process due to noncovalent cross-linking between the reactants. Precipitation during ITC titration severely affects the quality of the baseline as well as the signals. Hence, the resulting thermodynamic data are not dependable. We have made some modifications to address this problem and successfully studied multivalent glycoconjugate binding to lectins. We have also modified the Hill plot equation to analyze high quality ITC raw data obtained from multivalent binding. As described in this chapter, ITC-driven thermodynamic parameters and Hill plot analysis of ITC raw data can provide valuable information about the molecular mechanism of multivalent lectin-glycoconjugate interactions. The methods described herein revealed (i) the importance of functional valence of multivalent glycoconjugates, (ii) that favorable entropic effects contribute to the enhanced affinities associated with multivalent binding, (iii) that with the progression of lectin binding, the microscopic affinities of the glycan epitopes of a multivalent glycoconjugate decrease (negative cooperativity), (iv) that lectin binding to multivalent glycoconjugates, especially to mucins, involves internal diffusion jumps, (bind and jump) and (v) that scaffolds of glycoconjugates influence their entropy of binding.

  11. Characterization of protein-protein interactions by isothermal titration calorimetry.

    PubMed

    Velazquez-Campoy, Adrian; Leavitt, Stephanie A; Freire, Ernesto

    2015-01-01

    The analysis of protein-protein interactions has attracted the attention of many researchers from both a fundamental point of view and a practical point of view. From a fundamental point of view, the development of an understanding of the signaling events triggered by the interaction of two or more proteins provides key information to elucidate the functioning of many cell processes. From a practical point of view, understanding protein-protein interactions at a quantitative level provides the foundation for the development of antagonists or agonists of those interactions. Isothermal Titration Calorimetry (ITC) is the only technique with the capability of measuring not only binding affinity but the enthalpic and entropic components that define affinity. Over the years, isothermal titration calorimeters have evolved in sensitivity and accuracy. Today, TA Instruments and MicroCal market instruments with the performance required to evaluate protein-protein interactions. In this methods paper, we describe general procedures to analyze heterodimeric (porcine pancreatic trypsin binding to soybean trypsin inhibitor) and homodimeric (bovine pancreatic α-chymotrypsin) protein associations by ITC.

  12. A microfabrication-based approach to quantitative isothermal titration calorimetry.

    PubMed

    Wang, Bin; Jia, Yuan; Lin, Qiao

    2016-04-15

    Isothermal titration calorimetry (ITC) directly measures heat evolved in a chemical reaction to determine equilibrium binding properties of biomolecular systems. Conventional ITC instruments are expensive, use complicated design and construction, and require long analysis times. Microfabricated calorimetric devices are promising, although they have yet to allow accurate, quantitative ITC measurements of biochemical reactions. This paper presents a microfabrication-based approach to integrated, quantitative ITC characterization of biomolecular interactions. The approach integrates microfabricated differential calorimetric sensors with microfluidic titration. Biomolecules and reagents are introduced at each of a series of molar ratios, mixed, and allowed to react. The reaction thermal power is differentially measured, and used to determine the thermodynamic profile of the biomolecular interactions. Implemented in a microdevice featuring thermally isolated, well-defined reaction volumes with minimized fluid evaporation as well as highly sensitive thermoelectric sensing, the approach enables accurate and quantitative ITC measurements of protein-ligand interactions under different isothermal conditions. Using the approach, we demonstrate ITC characterization of the binding of 18-Crown-6 with barium chloride, and the binding of ribonuclease A with cytidine 2'-monophosphate within reaction volumes of approximately 0.7 µL and at concentrations down to 2mM. For each binding system, the ITC measurements were completed with considerably reduced analysis times and material consumption, and yielded a complete thermodynamic profile of the molecular interaction in agreement with published data. This demonstrates the potential usefulness of our approach for biomolecular characterization in biomedical applications.

  13. Automatic set-point titration for monitoring nitrification in SBRs.

    PubMed

    Fiocchi, N; Ficara, E; Bonelli, S; Canziani, R; Ciappelloni, F; Mariani, S; Pirani, M; Ratini, P; Mazouni, D; Harmand, J

    2008-01-01

    Nitrification is usually the bottleneck of biological nitrogen removal processes. In SBRs systems, it is not often enough to monitor dissolved oxygen, pH and ORP to spot problems which may occur in nitrification processes. Therefore, automated supervision systems should be designed to include the possibility of monitoring the activity of nitrifying populations. Though the applicability of set-point titration for monitoring biological processes has been widely demonstrated in the literature, the possibility of an automated procedure is still at its early stage of industrial development. In this work, the use of an at-line automated titrator named TITAAN (TITrimetric Automated ANalyser) is presented. The completely automated sensor enables us to track nitrification rate trend with time in an SBR, detecting the causes leading to slower specific nitrification rates. It was also possible to perform early detection of toxic compounds in the influent by assessing their effect on the nitrifying biomass. Nitrifications rates were determined with average errors+/-10% (on 26 tests), never exceeding 20% as compared with UV-spectrophotometric determinations.

  14. Common Standards of Basal Insulin Titration in T2DM

    PubMed Central

    Arnolds, Sabine; Heise, Tim; Flacke, Frank; Sieber, Jochen

    2013-01-01

    Type 2 diabetes mellitus has become a worldwide major health problem, and the number of people affected is steadily increasing. Thus, not all patients suffering from the disease can be treated by specialized diabetes centers or outpatient clinics, but by primary care physicians. The latter, however, might have time constraints and have to deal with many kinds of diseases or with multimorbid patients, so their focus is not so much on lowering high blood glucose values. Thus, the physicians, as well as the patients themselves, are often reluctant to initiate and adjust insulin therapy, although basal insulin therapy is considered the appropriate strategy after oral antidiabetic drug failure, according to the latest international guidelines. A substantial number of clinical studies have shown that insulin initiation and optimization can be managed successfully by using titration algorithms—even in cases where patients themselves are the drivers of insulin titration. Nevertheless, tools and strategies are needed to facilitate this process in the daily life of both primary health care professionals and patients with diabetes. PMID:23759411

  15. Automatic set-point titration for monitoring nitrification in SBRs.

    PubMed

    Fiocchi, N; Ficara, E; Bonelli, S; Canziani, R; Ciappelloni, F; Mariani, S; Pirani, M; Ratini, P; Mazouni, D; Harmand, J

    2008-01-01

    Nitrification is usually the bottleneck of biological nitrogen removal processes. In SBRs systems, it is not often enough to monitor dissolved oxygen, pH and ORP to spot problems which may occur in nitrification processes. Therefore, automated supervision systems should be designed to include the possibility of monitoring the activity of nitrifying populations. Though the applicability of set-point titration for monitoring biological processes has been widely demonstrated in the literature, the possibility of an automated procedure is still at its early stage of industrial development. In this work, the use of an at-line automated titrator named TITAAN (TITrimetric Automated ANalyser) is presented. The completely automated sensor enables us to track nitrification rate trend with time in an SBR, detecting the causes leading to slower specific nitrification rates. It was also possible to perform early detection of toxic compounds in the influent by assessing their effect on the nitrifying biomass. Nitrifications rates were determined with average errors+/-10% (on 26 tests), never exceeding 20% as compared with UV-spectrophotometric determinations. PMID:18701782

  16. Precise chelatometric titrations of zinc, cadmium, and lead with molecular spectroscopy.

    PubMed

    Suzuki, Toshihiro; Tiwari, Diwakar; Hioki, Akiharu

    2007-10-01

    Spectral data during a chelatometric titration were utilized for determining an equivalence point of the titration. Three-dimensional titration data were analyzed by fitting to a theoretical equation that was derived from equilibrium equations among a metal ion, an indicator and EDTA. The equation with optimized parameters successfully explained the three-dimensional titration data. This method was applied to EDTA titration systems of zinc, cadmium and lead with xylenol orange (XO) as an indicator. These systems were analyzed while taking the formation of 1:1 and 2:1 metal-indicator complexes into account. By this method, an accurate equivalence point was determined as well as stability constants and molar absorption spectra of metal-indicator complexes in each titration system. Moreover, the comparability among the concentrations of the metal standard solutions prepared from pure metals (Zn, Pb, and Cd) was also confirmed by the proposed evaluation method.

  17. New potentiometric and spectrophotometric methods for the determination of dextromethorphan in pharmaceutical preparations.

    PubMed

    Elmosallamy, Mohamed A F; Amin, Alaa S

    2014-01-01

    New, simple and convenient potentiometric and spectrophotometric methods are described for the determination of dextromethorphan hydrobromide (DXM) in pharmaceutical preparations. The potentiometric technique is based on developing a potentiometric sensor incorporating the dextromethorphan tetrakis(p-chlorophenyl)borate ion-pair complex as an electroactive species in a plasticized PVC matrix membrane with o-nitophenyl octyl ether or dioctyl phthalate. The sensor shows a rapid near Nernstian response of over 1 × 10(-5) - 1 × 10(-2) mol L(-1) dextromethorphan in the pH range of 3.0 - 9.0. The detection limit is 2 × 10(-6) mol L(-1) DXM and the response time is instantaneous (2 s). The proposed spectrophotometric technique involves the reaction of DXM with eriochrom black T (EBT) to form an ion-associate complex. Solvent extraction is used to improve the selectivity of the method. The optimal extraction and reaction conditions have been studied, and the analytical characteristics of the method have been obtained. Linearity is obeyed in the range of 7.37 - 73.7 × 10(-5) mol L(-1) DXM, and the detection limit of the method is 1.29 × 10(-5) mol L(-1). The relative standard deviation (RSD) and relative error for six replicate measurements of 3.685 × 10(-4) mol L(-1) are 0.672 and 0.855%, respectively. The interference effect of some excepients has also been tested. The drug contents in pharmaceutical preparations were successfully determined by the proposed methods by applying the standard-addition technique.

  18. Fusion of Potentiometric & Voltammetric Electronic Tongue for Classification of Black Tea Taste based on Theaflavins (TF) Content

    NASA Astrophysics Data System (ADS)

    Bhattacharyya, Nabarun; Legin, Andrey; Papieva, Irina; Sarkar, Subrata; Kirsanov, Dmitry; Kartsova, Anna; Ghosh, Arunangshu; Bandyopadhyay, Rajib

    2011-09-01

    Black tea is an extensively consumed beverage worldwide with an expanding market. The final quality of black tea depends upon number of chemical compounds present in the tea. Out of these compounds, theaflavins (TF), which is responsible for astringency in black tea, plays an important role in determining the final taste of the finished black tea. The present paper reports our effort to correlate the theaflavins contents with the voltammetric and potentiometric electronic tongue (e-tongue) data. Noble metal-based electrode array has been used for collecting data though voltammetric electronic tongue where as liquid filled membrane based electrodes have been used for potentiometric electronic tongue. Black tea samples with tea taster score and biochemical results have been collected from Tea Research Association, Tocklai, India for the analysis purpose. In this paper, voltammetric and potentiometric e-tongue responses are combined to demonstrate improvement of cluster formation among tea samples with different ranges of TF values.

  19. Potentiometric surface of the Floridan Aquifer, St. Johns River Water Management District and vicinity, Florida, May 1981

    USGS Publications Warehouse

    Schiner, George R.; Hayes, Eugene C.

    1981-01-01

    This map presents the potentiometric surface of the Floridan aquifer in the St. Johns River Water Management District and vicinity for May 1981. The Floridan aquifer is the principal source of potable water in the area. Water-level measurements were made in approximately 1,000 wells and at several springs. The potentiometric surface is shown mostly by 5-foot contour intervals. In the Fernandina Beach area 20 and 40-foot intervals are used to show a deep cone of depression. The potentiometric surface ranged from 122 feet above NGVD (National Geodetic Vertical Datum of 1929) in Polk County to 125 feet below NGVD in Nassau County. Water levels were at record lows in many counties due to lack of rainfall. Declines were as much as 10 feet and commonly 5 feet from the May 1980 levels. (USGS)

  20. Potentiometric surface of the upper Cape Fear Aquifer in the central coastal plain of North Carolina, December 1986

    USGS Publications Warehouse

    Winner, M.D.; Lyke, William L.; Brockman, Allen R.

    1989-01-01

    Water-level measurements were made in 84 wells open to the upper Cape Fear aquifer at the end of 1986 to determine the configuration of its potentiometric surface over an area of approximately 5,500 sq mi. The major feature of the potentiometric surface is the development of a large, almost circular cone of depression as a result of the merging of a number of smaller cones. The center of the large cone lies along an axis between Greenville and Kinston. The potentiometric surface in the upper Cape Fear is nearly 100 ft below sea level at Greenville; it is more than 100 ft above sea level south of the Neuse River near Colorado.